CN101764253B - Secondary aluminum battery and preparation method thereof - Google Patents
Secondary aluminum battery and preparation method thereof Download PDFInfo
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- CN101764253B CN101764253B CN2009102345176A CN200910234517A CN101764253B CN 101764253 B CN101764253 B CN 101764253B CN 2009102345176 A CN2009102345176 A CN 2009102345176A CN 200910234517 A CN200910234517 A CN 200910234517A CN 101764253 B CN101764253 B CN 101764253B
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- 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
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Abstract
The invention discloses a secondary aluminum battery and a preparation method thereof. The material of the positive electrode of the battery is organic polysulfide, the material of the negative electrode is aluminum or aluminum alloy, and the electrolyte is halogen aluminic acid ionic liquid; and the organic polysulfide is polysulfide carbine, thereby solving the problems that the elementary active substance is bad in conductivity and the frame is collapsed due to the dissolving of the reducing product. The electrolyte used is non-aqueous ionic liquid so that no oxide film, corrosive product or colloidal secondary product can be produced on the surface of the aluminum negative electrode so as to reduce the capacity loss of the negative electrode; the oxidation reduction reaction of the aluminum electrode in the electrolyte is reversible; and the battery is rechargeable. The preparation method for the secondary aluminum battery comprises the following steps: (1) preparing positive active material paste; (2) coating the positive active material paste on a foam nickel base, baking the paste and rolling the base into a positive plate; (3) rolling the positive plate, glass fiber non-woven membrane and the negative electrode made by taking any one of aluminum powder, aluminum foil and aluminum alloy as the negative active material into a battery core and arranging the battery core in a nickel-plated steel shell; then adding organic electrolyte in the steel shell; and sealing the steel shell to make the AA-type cylindrical secondary aluminum battery. The invention further discloses a preparation method for the positive material polysulfide carbyne of the battery.
Description
Technical field
The present invention relates to a kind of secondary aluminium cell and preparation method thereof.
Background technology
Littler, gentlier and more high performance electronic and communication apparatus, electric automobile, and the developing rapidly of new powers such as wind power generation, photovoltaic generation, to the battery performance of supporting power supply increasingly high requirement has been proposed.Commercial at present lead acid accumulator, nickel-cadmium cell, Ni-MH battery and lithium ion battery can not satisfy these requirements.Press for the exploitation have the energy height, the electrokinetic cell and the energy-storage battery of characteristics such as cost is low, the life-span is long, environmental protection, battery material aboundresources, reusable edible.With aluminum metal or aluminium alloy is that negative pole and sulfenyl material are that the secondary aluminium-sulfur battery of positive pole then is the most attractive battery system that meets these demands.
Aluminium is a kind of high-energy carrier.The aluminium electrode potential is-2.35V (vs SHE) that theoretical energy density is 2980mAh/g, is only second to lithium (3870mAh/g); And its volume energy density is 8050mAh/cm3, is 4 times of lithium, is higher than other all metal materials.In addition, the light weight of aluminium, cheap and aboundresources, pollution-free, reliability is high, safe in utilization, be desirable cell negative electrode material.
Though the theoretical energy density of aluminium-air cell can reach 8100Wh/Kg, actual energy density has only 350Wh/kg.This is because a lot of problems that the aluminium electrode can produce in aqueous electrolyte: very strong affinity is arranged between (1) aluminium alloy and the oxygen; In the air and the aqueous solution; The surface generates the fine and close passive oxidation film of one deck; 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 when also causing discharge simultaneously.(2) aluminium is typical amphoteric metal, and activity is higher, is prone to and acid, alkali effect, oxide-film is destroyed, and in a single day oxide-film is destroyed and will be corroded rapidly, makes the utilance of electrode low, and wet poor storage performance.(3) aluminium is bigger from corrosion in alkaline solution, and serious evolving hydrogen reaction takes place easy and medium, has reduced the utilance of electrode, influences the operate as normal of battery.(4) in the 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 the aluminium anodes polarization, make the aluminum cell mis-behave.(5) need heat-exchange system to get rid of dissolving and the corrosion of aluminium in alkaline solution and produce a large amount of heat.
In addition, because the reduction potential of aluminium is more negative than hydrogen, can not be at aqueous solution electrodeposition aluminium.Therefore, using the reduction of can't charging of the aluminum cell of aqueous electrolyte, can only be primary cell.
Sulphur has the theoretical energy density of 1675mAhg, is the highest positive electrode of known energy density.No matter be elemental sulfur directly as electrode, or sulfur-based compound, compare with traditional positive electrode that all there is great advantage several aspects once: (1) theoretical specific capacity is big; (2) the occurring in nature reserves are abundant, obtain easily, and are cheap; (3) safety non-toxic, environmental pollution is little; (4) synthesis technique is simple, can synthesize with multiple material.So sulphur is as a kind of desirable cell positive material, but cooperate the aluminium-sulfur battery of the cheap and aboundresources of constructed price, pollution-free, safe in utilization, high-energy-density with the aluminium negative pole.
Licht equals the nineties in 20th century exploitation a kind of high specific energy alkaline aqueous solution of the novel S of containing aluminium-sulfur battery (US Pat:5431881,4828492,5648183) that at normal temperatures can repid discharge.This battery is anode with the aluminium alloy, is negative electrode with the polysulfide that is dissolved in the alkaline electrolyte.But because the imperfection of aluminium anodes polarization and electrolyte system, the aluminium-sulfur battery of developing in the reality has only the battery OCP of 1.3V and the energy density of 110Wh/kg.(Investigation?of?a?novel?aqueous?aluminum/sulfur?battery.Journal?of?Power?Sources，1993，3(45)：311-323)
Sulphur is as the positive electrode of lithium metal/sulphur battery, for example US 3532543,3907591,4469761, Rauh, et al, J.Electrochem.Soc., 1979; 126 (4), 523-527, Yamin, et al, J Electrochem.Soc.; 1988,135 (5), 1045-1048, Peled, etal; J.of Power Source, 1989,26,269-271.The polysulfide that lithium/sulphur battery forms when discharge is soluble in the electrolyte; Produce self-discharge and stop up barrier film; In charging process, be easy to form passivation layer, be difficult to carry out ion and electron transfer, thereby cause the specific capacity decline and the cycle life of battery very poor on the positive active material surface.
Yet this positive electrode still has many shortcomings, the practicability of restriction lithium/sulphur battery: the one, and the electrical insulating property of elemental sulfur causes the utilance of active matter low; The 2nd, sulphur during discharge-sulfide linkage fracture, the micromolecule sulfide of generation is dissolved in electrolyte, generates the unordered sulphur of irreversible reaction; Cause self-discharge of battery, the viscosity of electrolyte is increased, ions diffusion is obstructed; And the distribution of active matter in electrode alters a great deal; Repeatedly after the circulation agglomeration possibly take place, cause capacity to decay rapidly, the cycle performance of battery is descended very soon.
Summary of the invention
Technical problem to be solved by this invention provides a kind of shortcoming that overcomes prior art, and a kind of secondary aluminium cell that contains non-aqueous solution electrolysis plastidome is provided.
Technical scheme is:
A kind of secondary aluminium cell; Comprise anode, negative pole, electrolyte, barrier film, collector, battery case and lead-in wire; The material of anode is the organic polysulfide compound, and the material of said GND is an aluminum or aluminum alloy, and said electrolyte is halogen aluminic acid ionic liquid.
Said organic polysulfide compound is a carbyne polysulfide; Said organic polysulfide compound can be many sulfo-s cyclopentadiene or many sulfo-s naphthalene or many sulfo-s aniline or many sulfo-s pyridine or many sulfo-s pyrroles or many sulfo-s thiophene or many thio-furans.
Said halogen aluminic acid ionic liquid is an aluminum halide with any is formed in quaternary ammonium salt Huo quaternary alkylphosphonium salt or the season sulfosalt; Halogen aluminic acid ionic liquid can be the chlorine aluminic acid ionic liquid of aluminium chloride with quaternary ammonium salt formation.
A kind of preparation method according to secondary aluminium cell comprises the steps:
(1) preparation positive electrode active materials slurries: with C: the S mass ratio is 1: the carbyne polysulfide material of 1-5 preparation is a positive electrode active materials; Add super carbon black SUPER-P of conductive agent and adhesive Kynoar PVDF; Ratio is 7: 2: 1, processes the positive electrode active materials slurries
(2) the positive electrode active materials slurries are coated on the nickel foam substrate, oven dry is rolled into positive plate.Knit barrier film and be wound into the electric stamen nickel plating box hat of packing into positive plate and glass fiber are non-, add organic bath again, seal and process AA type cylinder secondary aluminium cell with any negative pole of processing as negative active core-shell material in aluminium powder or aluminium foil, the aluminium alloy.
A kind of preparation method of cell positive material carbyne polysulfide, carbyne polysulfide is to be taken off by hydrogeneous polyalkenyl halides to vulcanize behind the HCl again and make, and comprises the steps:
(1) earlier hydrogeneous polyalkenyl halides is mixed with elemental sulfur, Kynoar PVDC and elemental sulfur mixing, with Kynoar PVDC and sulphur by C: the S mass ratio is 1: 2-5 mixes; Under agitation slowly add in the 100ml DMF solution, slowly heat up, be dissolved in N fully at 70 ± 2 ℃ of Kynoar PVDC; Among the dinethylformamide DMF, 120 ± 2 ℃ of sulphur are dissolved among the DMF, and it is yellow that solution is; There is the elemental sulfur of a small amount of fused solution to be deposited on the bottom of flask simultaneously
(2) treat the dissolving of PVDC and sulphur after, stop heating, under stronger stirring, slowly drip 100ml methyl alcohol, separate out the homogeneous mixture of ecru Kynoar PVDC and sulphur in the above-mentioned solution gradually, it is subsequent use to filter final vacuum drying 12h.
(3) preparation of carbyne polysulfide: with said mixture in ammonia environment in tube furnace temperature be 300 ℃, reacting by heating 3 hours obtains carbyne polysulfide, comes out of the stove with after the stove cooling.
Beneficial effect: solution of the present invention is that negative pole adopts the metal aluminum or aluminum alloy, compares lithium anode, and both cheap, material source is extensive, again safety.
Electrolyte system adopts the nonaqueous ionic liquid electrolyte, assemble and sealing under the anaerobic water-less environment.Make the aluminium negative terminal surface not generate oxide-film like this, no wasteness burn into does not have the colloid accessory substance; Reduced the capacity of negative plates loss, the redox reaction of aluminium electrode in this electrolyte is reversible, and battery is chargeable; Thereby improved the electrochemical reversibility of negative pole, improved battery performance.
Positive active material is the very high organic polysulfide of specific capacity, and its structure can solve elemental sulfur active material poorly conductive simultaneously, and reduzate dissolves problems such as the skeleton that causes caves in.
Carbyne polysulfide preparation methods of the present invention and compared with present technology following beneficial effect is arranged as the aluminum secondary battery of positive electrode active materials and the preparation method of aluminum secondary battery:
1. the preparation process of positive electrode active materials of the present invention, negative pole and electrolyte is pollution-free, and preparation cost is low, and technology is simple, and is high with the secondary aluminium cell energy density of this method preparation, good cycle;
2. carbyne polysulfide material main chain is that conducting polymer gathers carbon skeleton, can improve the conductivity of material, thus can reduce the consumption of conductive agent in positive electrode, and then help improving anodal specific capacity; The S-S key of energy storage is connected on the polymer backbone as side chain; Skeleton is not degraded during discharge; Dissolubility in organic electrolyte can guarantee that much smaller than the micromolecule polysulfide anodal external form is stablized and most of sulphur is trapped in positive polar region, and cycle performance has been strengthened; Simultaneously, high, the good cycle of the secondary aluminium cell reversible capacity with this positive electrode active materials carbyne polysulfide preparation;
3. the present invention adopts NH
3Participate in the pyrolysismethod of reaction; Reduced the temperature that removes of HCl in the Kynoar PVDC unit, and then reduced Kynoar PVDC and take off the crosslinked of carbochain behind the HCl, with sulphur altogether after the heat; Increase the possibility that forms the carbyne polysulfide structure, improved the yield of positive electrode active materials; Simultaneously with ammonia as taking off HCl reagent; Can be directly and solid Kynoar PVDC haptoreaction, avoid in solvent, reacting the side reaction that is brought, preparation technology is simple; Secondary aluminium cell energy density with this method preparation is high, environment friendly and pollution-free, safe and reliable; Applicable multiple occasion, fields such as the for example occasion of removable power supplys such as mobile phone, notebook computer, mobile electronic device, and electric motor car, hybrid-power electric vehicle.
Embodiment
Below in conjunction with specific embodiment the present invention is done further detailed retouching.
A kind of secondary aluminium cell; Comprise anode, negative pole, electrolyte, barrier film, collector, battery case and lead-in wire; The material of said anode is the organic polysulfide compound, and the material of said GND is an aluminum or aluminum alloy, and said electrolyte is halogen aluminic acid ionic liquid.
Said organic polysulfide compound is a carbyne polysulfide; Said organic polysulfide compound is many sulfo-s cyclopentadiene or many sulfo-s naphthalene or many sulfo-s aniline or many sulfo-s pyridine or many sulfo-s pyrroles or many sulfo-s thiophene or many thio-furans.
Said halogen aluminic acid ionic liquid is an aluminum halide with any is formed in quaternary ammonium salt Huo quaternary alkylphosphonium salt or the season sulfosalt; Halogen aluminic acid ionic liquid is the chlorine aluminic acid ionic liquid that aluminium chloride forms with quaternary ammonium salt.
The preparation method of secondary aluminium cell comprises the steps:
(1) preparation positive electrode active materials slurries: with C: the S mass ratio is 1: the carbyne polysulfide material of 1-5 preparation is a positive electrode active materials; Add super carbon black SUPER-P of conductive agent and adhesive Kynoar PVDF, ratio is 7: 2: 1; Process the positive electrode active materials slurries
(2) the positive electrode active materials slurries are coated on the nickel foam substrate, oven dry is rolled into positive plate.Knit barrier film and be wound into the electric stamen nickel plating box hat of packing into positive plate and glass fiber are non-, add organic bath again, seal and process AA type cylinder secondary aluminium cell with any negative pole of processing as negative active core-shell material in aluminium powder or aluminium foil, the aluminium alloy.
The preparation method of cell positive material carbyne polysulfide, carbyne polysulfide is to be taken off by hydrogeneous polyalkenyl halides to vulcanize behind the HCl again and make, and comprises the steps:
(1) earlier hydrogeneous polyalkenyl halides is mixed with elemental sulfur, Kynoar PVDC and elemental sulfur mixing, with Kynoar PVDC and sulphur by C: the S mass ratio is to mix at 1: 3; Under agitation slowly add in the 100ml DMF solution, slowly heat up, be dissolved in fully among the dinethylformamide DMF at 70 ± 2 ℃ of Kynoar PVDC; 120 ± 2 ℃ of sulphur are dissolved among the DMF; It is yellow that solution is, and has the elemental sulfur of a small amount of fused solution to be deposited on the bottom of flask simultaneously
(2) treat the dissolving of Kynoar PVDC and sulphur after, stop heating, under stronger stirring, slowly drip 100ml methyl alcohol, separate out the homogeneous mixture of ecru Kynoar PVDC and sulphur in the above-mentioned solution gradually, it is subsequent use to filter final vacuum drying 12h.
(3) preparation of carbyne polysulfide: with said mixture in ammonia environment in tube furnace temperature be 300 ℃, reacting by heating 3 hours obtains carbyne polysulfide, comes out of the stove with after the stove cooling.
Above-mentioned negative pole is selected from any in aluminium and the alloy thereof; Aluminium alloy be selected from aluminium and lithium, sodium, potassium, gallium, indium, thallium, iron, cobalt, nickel, copper, zinc, manganese, tin, lead, magnesium, calcium, chromium, the germanium any or two or more; The form of aluminum or aluminum alloy is any in ultra micro, ultra-fine or nano powder, silk, net, sheet, paper tinsel, the foam
Conductive agent is selected from carbon back, graphite based conducting material and conducting polymer; Specifically: be selected from active carbon, carbon black, acetylene carbon black, super carbon black Super-P, graphite, polyaniline, polyacetylene, polypyrrole, the polythiophene any, above-mentioned electric conducting material uses separately or the combination use of two kinds or more how above-mentioned electric conducting material.
Binding agent is selected from polyvinyl acetate, polyvinyl alcohol, polyethylene glycol oxide, polyvinylpyrrolidone, polyvinylether, polymethyl methacrylate, Kynoar, polytetrafluoroethylene, polyvinyl chloride, polyacrylonitrile, polyvinyl pyridine, polystyrene, and in their derivative, mixture and the copolymer any or two or more.
Organic solvent is selected from any in acetonitrile, methyl alcohol, ethanol, acetone, oxolane, water and the isopropyl alcohol.
Collector is selected from any in the electric conducting material of stainless steel, carbon, copper, aluminium, nickel.Its form is selected from a kind of or carbon cloth in the foam, net, paper tinsel, sheet form of metal.
Described secondary aluminium cell is selected from the square of individual layer button, multilaminate coiled cylindrical, multilayer folding, any in various ways and the specification.
The preparation method of as previously discussed secondary aluminium cell positive electrode active materials sulfuration carbyne is to be taken off by hydrogeneous polyalkenyl halides to vulcanize behind the HCl again and make.Hydrogeneous polyalkenyl halides is selected from Kynoar, gathers 1,2-dichloroethene, in polyvinyl chloride, Vingon and their copolymer and the blend any or two or more.Be preferably and gather in 1,2-dichloroethene and their copolymer and the blend any, more preferably gather 1,2-dichloroethene.
The comparative example 1
Active carbon and elemental sulfur mix with mass ratio 1: 3 and are placed in the ball grinder, and with ratio of grinding media to material 1: 1, rotating speed 200r/min carried out ball milling 6h, places then in the resistance furnace, and under the condition of argon shield, 350 ℃ of compound 3h of heating obtain carbon sulphur composite material behind the natural cooling.With carbon sulphur composite material mass ratio is positive electrode at 1: 3; Add conductive agent SUPER-P and adhesive Kynoar PVDF, ratio is 7: 2: 1, processes the positive electrode active materials slurry and is coated with on the nickel foam substrate; Oven dry is rolled into positive plate; Knit barrier film and be wound into the electric stamen nickel plating box hat of packing into glass fiber is non-, add organic bath again, seal and process AA type cylinder secondary aluminium cell with the negative pole that aluminium flake is processed as negative active core-shell material.During the battery charging and discharging loop test, charge with 0.5C, the 1C discharge, discharge cut-off voltage is 1.2V, discharges and recharges data and lists in the table 1.
Embodiment 1
With C: the S mass ratio is that the carbyne polysulfide material of preparation in 1: 1 be a positive pole, and all the other preparation processes of positive pole are with comparative example 1.
The method of negative pole preparation is with comparative example 1, and the assembling of battery is with comparative example 1.During the battery charging and discharging loop test, charge to 2.4V with 1C, 0.5C is discharged to 1.2V, discharges and recharges data and lists in the table 1.
Embodiment 2
With C: the S mass ratio is that the carbyne polysulfide material of preparation in 1: 2 is a positive pole, and remaining preparation process of battery is with comparative example 1.During the battery charging and discharging loop test, charge to 2.4V with 1C, 0.5C is discharged to 1.2V, discharges and recharges data and lists in the table 1.
Embodiment 3
With C: the S mass ratio is that the carbyne polysulfide material of preparation in 1: 3 is a positive pole, and remaining preparation process of battery is with comparative example 1.During the battery charging and discharging loop test, charge to 2.4V with 1C, 0.5C is discharged to 1.2V, discharges and recharges data and lists in the table 1.
Embodiment 4
With C: the S mass ratio is that the carbyne polysulfide material of preparation in 1: 4 is a positive pole, and remaining preparation process of battery is with comparative example 1.During the battery charging and discharging loop test, charge to 2.4V with 1C, 0.5C is discharged to 1.2V, discharges and recharges data and lists in the table 1.
Embodiment 5
With C: the S mass ratio is that the carbyne polysulfide material of preparation in 1: 5 is a positive pole, and remaining preparation process of battery is with comparative example 1.During the battery charging and discharging loop test, charge to 2.4V with 1C, 0.5C is discharged to 1.2V, discharges and recharges data and lists in the table 1.
Table 1. battery charging and discharging tables of data
| Positive electrode active materials | Negative active core-shell material | Open circuit voltage/V | Initial discharge capacity/mAh | Capacity/mAh after 50 times circulates | |
| The comparative example 1 | The mass ratio of C-S composite material is 1: 3 | Al | 1.78 | 883 | 721 |
| Embodiment 1 | The C-S mass ratio is the carbyne polysulfide of preparation in 1: 1 | Al | 1.81 | 1009 | 887 |
| Embodiment 2 | The C-S mass ratio is the carbyne polysulfide of preparation in 1: 2 | Al | 1.81 | 1041 | 965 |
| Embodiment 3 | The C-S mass ratio is the carbyne polysulfide of preparation in 1: 3 | Al | 1.81 | 1106 | 1065 |
| Embodiment 4 | The C-S mass ratio is the carbyne polysulfide of preparation in 1: 4 | Al | 1.81 | 1063 | 997 |
| Embodiment 5 | The C-S mass ratio is the carbyne polysulfide of preparation in 1: 5 | Al | 1.81 | 1025 | 906 |
Can find out from the result of table 1: 1) among the comparative examples 1 as prior art: the mass ratio of C-S composite material is that the initial discharge capacity of the secondary cell that constitutes of 1: 3 positive electrode active materials is minimum; 2) with C: the S mass ratio is that the carbyne polysulfide material of 1: 1～5 preparations is that the initial discharge capacity of the secondary cell that constitutes of positive electrode active materials increases gradually; 3) C: the S mass ratio is that the carbyne polysulfide material of preparation in 1: 3 is that the initial discharge capacity of the secondary cell that constitutes of positive electrode active materials is the highest; 4) C: the S mass ratio is that the carbyne polysulfide material of preparation in 1: 4 to 1: 5 is that the initial discharge capacity of the secondary cell that constitutes of positive electrode active materials reduces 5 again gradually) situation of change of situation of change and the initial discharge capacity of capacity is similar after the circulation 50 times.
Therefore, use C: what the S mass ratio was the secondary cell that constitutes as positive electrode active materials of the carbyne polysulfide of preparation in 1: 1～5 o'clock than prior art is that the various performances of capacity are all good after initial discharge capacity and the circulation 50 times of the secondary cell that constitutes of the positive electrode active materials of 1: 3 C-S composite material with mass ratio.
Should be noted that; Above embodiment is just in order to do further detailed description to the present invention; Be not used for described claim is limited; In the scope that does not break away from design of the present invention and spirit, those of ordinary skills can carry out various improvement or change, still belong within protection scope of the present invention.
Claims (1)
1. secondary aluminium cell; Comprise anode, negative pole, electrolyte, barrier film, collector, battery case and lead-in wire; It is characterized in that: said battery anode active material is a carbyne polysulfide; Perhaps be many sulfo-s cyclopentadiene or many sulfo-s naphthalene or many sulfo-s aniline or many sulfo-s pyridine or many sulfo-s pyrroles or many sulfo-s thiophene or many thio-furans
Said GND active material is an aluminum or aluminum alloy,
Said electrolyte is the chlorine aluminic acid ionic liquid that aluminium chloride forms with quaternary ammonium salt.
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