CN104332592A - Carbon-sulfur composite positive electrode based on carbon nano-fiber array, and applications thereof - Google Patents
Carbon-sulfur composite positive electrode based on carbon nano-fiber array, and applications thereof Download PDFInfo
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- CN104332592A CN104332592A CN201410525861.1A CN201410525861A CN104332592A CN 104332592 A CN104332592 A CN 104332592A CN 201410525861 A CN201410525861 A CN 201410525861A CN 104332592 A CN104332592 A CN 104332592A
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- carbon
- carbon nanofiber
- nanofiber arrays
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
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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
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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
- 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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Abstract
The present invention discloses a carbon-sulfur composite positive electrode based on a carbon nano-fiber array, a preparation method and applications thereof. According to the composite positive electrode, a chemical deposition method is adopted to prepare a directionally-growing carbon nano-fiber array on an electric conduction substrate, and then a hot melt diffusion manner is adopted to make sulfur and the carbon nano-fiber array compound so as to form the carbon-sulfur composite positive electrode based on the carbon nano-fiber array. According to the present invention, the preparation of the composite positive electrode does not require the addition of the electric conduction agent and the binder, the electrode directly contacts the electric conduction substrate, the resistance is small, the rate capability is good, the energy density is high, and the secondary aluminum battery prepared by adopting the carbon-sulfur composite positive electrode has characteristics of high energy, environmental protection and safety.
Description
Technical field
The invention belongs to electrochemistry and new forms of energy product scope, relate to a kind of carbon sulphur anode composite based on carbon nanofiber arrays and preparation method, more relate to a kind of secondary aluminium cell adopting this anode composite to prepare.
Background technology
Regenerative resource is grid-connected, and the develop rapidly of the new energy technology such as electric automobile and intelligent grid is in the urgent need to developing the energy storage system of high-energy-density.The theoretical energy density of aluminium, up to 2980mAh/g, be only second to lithium (3682mAh/g), and chemical activity is relatively stable, is desirable negative material; Sulphur has the theoretical energy density of 1675mAh/g, is the positive electrode that known energy density is the highest, and the two aluminium-sulfur battery system formed is a kind of emerging high energy density cells system.But the shortcomings such as sulphur conductivity is low, cycle performance is poor seriously limit it and use.Therefore, elemental sulfur and the carbon-based material with electric conductivity are combined the electric conductivity and utilance that can improve material.
Carbon nano-fiber is a kind of material with excellent conductive capability, there is specific area large, the advantages such as mechanical property is good, and draw ratio is large, carbon nano-fiber is interlaced can form the conductive network having " confinement " and act on, and is conducive to the transmission of ion and suppresses the dissolving of sulphur reduzate.But traditional carbon nano-fiber mostly is unordered shape, easily reunites, cause its effective ratio area to reduce, have a strong impact on the load capacity of material to sulphur, simultaneously the skewness of sulphur in material with carbon element, sulphur active material utilization is low; During discharge and recharge, carbon nano-fiber surface has a large amount of sulphur active material and becomes poly sulphide dissolves in electrolyte.
Summary of the invention
(1) goal of the invention
For the problems referred to above and deficiency, the object of the present invention is to provide a kind of carbon sulphur anode composite based on carbon nanofiber arrays.This anode composite be by the carbon nano-fiber of ordering growth replace tradition easily to reunite carbon nano-fiber, carbon nano-fiber vertical-growth on conductive substrates material, and is obtained by hot melt diffusion sulphur compound.Carbon nanofiber arrays arrangement in order, favorable orientation, the pore structure of the storeroom pipeline that its arrangement is formed and material itself is nanoscale, and elemental sulfur can be made to be uniformly distributed wherein with nano shape, closely be combined with electric conducting material, improve the reactivity of sulphur.Meanwhile, the orderly passage that carbon nano-fiber arrangement is formed can produce the confinement effect than common material with carbon element more " long-range ", suppresses the dissolving of poly sulfide; Be conducive to the transmission of ion, electronics on the other hand, improve the conductivity of positive electrode.
In addition, due to without additional conductive agent and binding agent, can significantly improve the specific capacity of electrode, the energy density of electrode is also higher.
The present invention also aims to provide a kind of carbon sulphur anode composite based on carbon nanofiber arrays and preparation method.
The present invention also aims to provide a kind of secondary aluminium cell prepared with this anode composite.
(2) technical scheme
For achieving the above object, the invention provides following technical scheme:
Based on a carbon sulphur anode composite for carbon nanofiber arrays, comprising:
(a) conductive substrates;
(b) carbon nanofiber arrays;
(c) sulphur.
The carbon sulphur anode composite based on carbon nanofiber arrays described in scheme, it is characterized in that, the base material of described carbon nanofiber arrays includes but not limited to the metals or nonmetal such as carbon fiber, graphite, vitrescence carbon, titanium, nickel, stainless steel, iron, copper, zinc, lead, manganese, cadmium, gold, silver, platinum, tantalum, tungsten, conductive plastics, conductive rubber or highly doped silicon.
The carbon sulphur anode composite based on carbon nanofiber arrays described in scheme, is characterized in that, described anode composite after oriented growth carbon nanofiber arrays, is obtained by hot melt diffusion sulphur compound on conducting base by chemical vapour deposition (CVD).
The carbon sulphur anode composite based on carbon nanofiber arrays described in scheme, is characterized in that, the diameter of described carbon nanofiber arrays is 50 ~ 400nm, and length is 2 ~ 50 μm.
The carbon sulphur anode composite based on carbon nanofiber arrays described in scheme, is characterized in that, the mode that described sulphur is spread by hot melt and carbon nanofiber arrays compound.
A preparation method for the carbon sulphur anode composite based on carbon nanofiber arrays described in scheme, is characterized in that, comprise the steps:
Step 1, the preparation of carbon nanofiber arrays: adopting chemical vapour deposition technique, take acetylene as reacting gas, adds catalyst precursor prepares oriented growth carbon nanofiber arrays on conductive substrates surface;
Step 2, preparation based on the carbon sulphur anode composite of carbon nanofiber arrays: by the carbon nanofiber arrays prepared and elemental sulfur in mass ratio 1:5 ~ 1:10 put into the reactor of the airtight polytetrafluoroethylene containing nitrogen, be placed in baking oven to be heated to 120 ~ 300 DEG C and to make sulphur fully melt and spread, be cooled to the carbon sulphur anode composite that room temperature obtains based on carbon nanofiber arrays.
The preparation method of the carbon sulphur anode composite based on carbon nanofiber arrays described in scheme, it is characterized in that, the catalyst precursor in step 1 is copper colloidal sol or cupric tartrate.
The preparation method of the carbon sulphur anode composite based on carbon nanofiber arrays described in scheme, is characterized in that, adopts the mode being once heated to uniform temperature or heating-cooling-heating to carry out heat fused to sulphur.
A kind of secondary aluminium cell, comprising:
A () positive pole, is characterized in that, described just very based on the carbon sulphur anode composite of carbon nanofiber arrays;
B () is containing aluminum honeycomb active material;
C () non-water is containing aluminium electrolyte.
Secondary aluminium cell described in scheme, is characterized in that, also can comprise the barrier film between positive pole and negative pole.Suitable solid porous separator material includes but not limited to: polyolefin is as polyethylene and polypropylene, glass fiber filter paper and ceramic material.
Secondary aluminium cell described in scheme, is characterized in that, described containing aluminum honeycomb active material, includes but not limited to: metallic aluminium; Aluminium alloy, comprises the alloy containing at least one element be selected from Li, Na, K, Ca, Fe, Co, Ni, Cu, Zn, Mn, Sn, Pb, Ma, Ga, In, Cr, Ge and Al.
Secondary aluminium cell described in scheme, is characterized in that, described non-water is organic salt-aluminum halide system containing aluminium electrolyte, and wherein the mol ratio of organic salt and aluminum halide is 1:1.1 ~ 3.0.
Organic salt described in scheme-aluminum halide system, is characterized in that, the cation of described organic salt comprises imidazol ion, pyridinium ion, pyrrolidinium ion, piperidines ion, morpholinium ion, quaternary ammonium salt ion ， quaternary alkylphosphonium salt ion and tertiary sulfosalt ion; The anion of organic salt comprises Cl
-, Br
-, I
-, PF
6 -, BF
4 -, CN
-, SCN
-, [N (CF
3sO
2)
2]
-, [N (CN)
2]
-plasma.
Organic salt described in scheme-aluminum halide system, is characterized in that, described aluminum halide is the one in aluminium chloride, aluminium bromide or silver iodide.
Described in scheme, the preparation method of secondary aluminium cell is as follows: the carbon sulphur anode composite of above-mentioned preparation is dried be cut into 40mm wide × pole piece that 15mm length × 0.33mm is thick, the barrier film thick with 0.16mm and be wound into battery core with aluminium flake as the negative pole that negative active core-shell material is made and load nickel plating box hat, reinject electrolyte, and secondary aluminium cell is made in sealing.
(3) beneficial effect
1) the present invention utilizes carbon nanofiber arrays and sulphur by hot melt diffusion for carbon sulphur anode composite, this anode composite is on the one hand due to the ordered arrangement of carbon nano-fiber, define the passage that orientation is good, the pore structure of the passage of these nanoscales and material itself can make sulphur be uniformly distributed wherein with nano shape, improves the reactivity of sulphur; On the other hand, the passage that carbon nano-fiber aligns formation can produce the confinement effect than common material with carbon element more " long-range ", the effect of shuttling back and forth suppressing the dissolving of polysulfide better and occur at two interpolars.
2) preparation of this positive pole is without the need to adding conductive agent and binding agent, can further improve the specific capacity of electrode, and preparation process is simple, and cost is low.
3) apply that secondary aluminium cell energy density prepared by this positive pole is high, capacity large, good cycle, price economy, Environmental Safety and application prospect is extensive.
(4) embodiment
Be described further below with reference to the technique effect of embodiment to design of the present invention, concrete structure and generation, to understand object of the present invention, characteristic sum effect fully.The following examples describe several execution mode of the present invention, and they are only illustrative, and nonrestrictive.
embodiment 1:
1) preparation of carbon nanofiber arrays: the sodium potassium tartrate tetrahydrate taking 1.41g is dissolved in 50mL deionized water, be mixed with the solution that concentration is 0.lmol/L, and then take 1.25g copper sulphate and dissolve in 50mL deionized water, be mixed with the solution that concentration is 0.lmol/L, then the copper-bath prepared is added drop-wise in potassium sodium tartrate solution slowly, ceaselessly to stir in the process dripped, obtain cupric tartrate catalyst; Adopt chemical vapour deposition technique, cupric tartrate is that catalyst at room temperature passes into argon gas 20min with the flow of 150sccm, to discharge the air in quartz ampoule; Keep the flow of argon gas constant, be raised to 400 DEG C with the speed of 50 DEG C/min, after 10min, argon gas replaced by hydrogen (70sccm) and acetylene (30sccm).To be brought into by hydrogen and acetylene gas mixture by the catalyst of heat sublimation and carry out catalytic cracking reaction, reaction 30min, prepare the carbon nanofiber arrays of oriented growth on conductive substrates surface.
2) based on the preparation of the carbon sulphur anode composite of carbon nanofiber arrays: by the carbon nanofiber arrays prepared and elemental sulfur in mass ratio 1:5 put into the reactor of the airtight polytetrafluoroethylene containing nitrogen, be placed in baking oven to be once heated to 300 DEG C and to make sulphur fully melt and spread, be cooled to the carbon sulphur anode composite that room temperature obtains based on carbon nanofiber arrays.
3) preparation of secondary aluminium cell: by be cut into after the carbon sulphur anode composite drying of above-mentioned preparation 40mm wide × pole piece that 15mm length × 0.33mm is thick, the glass fibre thick with 0.16mm is non-to be knitted barrier film and is wound into battery core loading nickel plating box hat with aluminium flake as the negative pole that negative active core-shell material is made, reinject aluminium chloride-triethylamine hydrochloride ionic liquid electrolyte, and AA type secondary aluminium cell is made in sealing.
embodiment 2:
1) based on the preparation of the carbon sulphur anode composite of carbon nanofiber arrays: by the carbon nanofiber arrays prepared and elemental sulfur in mass ratio 1:5 put into the reactor of the airtight polytetrafluoroethylene containing nitrogen, under flowing argon gas atmosphere, carbon nanofiber arrays and elemental sulfur mixture are heated to about 180 DEG C, keep 2h at this temperature, after be heated to about 300 DEG C insulation 1h, 300 DEG C are heated to after cooling to 180 DEG C again, be incubated 1h at this temperature, repeated multiple timesly sulphur is fully melted and is diffused in carbon nanofiber arrays, naturally cool, obtain the carbon sulphur anode composite based on carbon nanofiber arrays.
2) other are with embodiment 1.
embodiment 3:
1) preparation of carbon nanofiber arrays: the protective agent polyvinylpyrrolidone of 1.6g is dissolved in deionized water the solution being mixed with 40mL, 10mL solution is prepared again with soluble copper salt copper sulphate 0.037g, be placed on 80 DEG C of waters bath with thermostatic control after mix and blend and be incubated one hour, then room temperature is cooled to, drip a certain amount of reducing agent 80% hydrazine hydrate (10mL), and keep reaction solution cumulative volume to be 50mL, heat and be stirred to 80 DEG C of insulations, aubergine is become to solution colour, insulation a period of time, copper colloidal sol can be obtained; Adopt chemical vapour deposition technique, copper colloidal sol is that catalyst at room temperature passes into argon gas 20min with the flow of 150sccm, to discharge the air in quartz ampoule; Keep the flow of argon gas constant, be raised to 400 DEG C with the speed of 50 DEG C/min, after 10min, argon gas replaced by hydrogen (70sccm) and acetylene (30sccm); To be brought into by hydrogen and acetylene gas mixture by the catalyst of heat sublimation and carry out catalytic cracking reaction, reaction 30min, prepare the carbon nanofiber arrays of oriented growth on conductive substrates surface.
2) other are with embodiment 1.
embodiment 4:
Carry out charge and discharge cycles test to made battery, charge to 2.2V with 1C, 0.5C discharges, and discharge cut-off voltage is 1.2V, and test result is as shown in the table:
| Battery | Open circuit voltage (V) | Discharge capacity (mAh) first | Cycle-index | Capacity attenuation rate |
| Embodiment 1 | 1.82 | 760 | 50 | 27.2% |
| Embodiment 2 | 1.83 | 755 | 50 | 26.2% |
| Embodiment 3 | 1.85 | 736 | 50 | 28.7% |
Although reference embodiment is to invention has been detailed description, but those skilled in the art is to be understood that, when not departing from the spirit and scope of the present invention described in appended claims and equivalent thereof, various amendment and replacement can be made to it.
Claims (9)
1., based on a carbon sulphur anode composite for carbon nanofiber arrays, it is characterized in that, described anode composite comprises:
(a) conductive substrates;
(b) carbon nanofiber arrays;
(c) sulphur.
2., as claimed in claim 1 based on the carbon sulphur anode composite of carbon nanofiber arrays, it is characterized in that, described anode composite by chemical vapour deposition (CVD) oriented growth carbon nanofiber arrays on conducting base, then with sulphur compound and obtaining.
3., as claimed in claim 1 based on the carbon sulphur anode composite of carbon nanofiber arrays, it is characterized in that, the diameter of described carbon nanofiber arrays is 50 ~ 400nm, and length is 2 ~ 50 μm.
4. as claimed in claim 1 based on the carbon sulphur anode composite of carbon nanofiber arrays, it is characterized in that, the mode that described sulphur is spread by hot melt and carbon nanofiber arrays compound.
5. a preparation method for the carbon sulphur anode composite based on carbon nanofiber arrays according to claim 1, is characterized in that comprising the following steps:
Step 1, the preparation of carbon nanofiber arrays: adopting chemical vapour deposition technique, take acetylene as reacting gas, adds catalyst precursor prepares oriented growth carbon nanofiber arrays on conductive substrates surface;
Step 2, preparation based on the carbon sulphur anode composite of carbon nanofiber arrays: by the carbon nanofiber arrays prepared and elemental sulfur in mass ratio 1:5 ~ 1:10 put into the reactor of the airtight polytetrafluoroethylene containing nitrogen, be placed in baking oven to be heated to 120 ~ 300 DEG C and to make sulphur fully melt and spread, be cooled to the carbon sulphur anode composite that room temperature obtains based on carbon nanofiber arrays.
6., as claimed in claim 5 based on the preparation method of the carbon sulphur anode composite of carbon nanofiber arrays, it is characterized in that, the catalyst precursor described in step 1 is copper colloidal sol or cupric tartrate.
7. a secondary aluminium cell, comprises positive pole, negative pole and electrolyte, it is characterized in that:
(a) carbon sulphur anode composite based on carbon nanofiber arrays just very as claimed in claim 1;
B () is containing aluminum honeycomb;
C () non-water is containing aluminium electrolyte.
8. secondary aluminium cell as claimed in claim 7, it is characterized in that, described containing aluminum honeycomb material, include but not limited to: metal aluminum and its alloy, aluminium alloy comprises the alloy containing at least one element be selected from Li, Na, K, Ca, Fe, Co, Ni, Cu, Zn, Mn, Sn, Pb, Ma, Ga, In, Cr, Ge and Al.
9. secondary aluminium cell as claimed in claim 7, is characterized in that, described non-water comprises organic salt-aluminum halide system ionic liquid containing aluminium electrolyte, and wherein, the mol ratio of organic salt and aluminum halide is 1:1.1 ~ 3.0.
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Application publication date: 20150204 |