CN101728538A - Ordered nanostructure sulphur/mesoporous carbon composite material for anode of lithium ion battery - Google Patents
Ordered nanostructure sulphur/mesoporous carbon composite material for anode of lithium ion battery Download PDFInfo
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- CN101728538A CN101728538A CN200910199577A CN200910199577A CN101728538A CN 101728538 A CN101728538 A CN 101728538A CN 200910199577 A CN200910199577 A CN 200910199577A CN 200910199577 A CN200910199577 A CN 200910199577A CN 101728538 A CN101728538 A CN 101728538A
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Abstract
The invention relates to an ordered nanostructure sulphur/mesoporous carbon composite material for anode of a lithium ion battery; the composite material is formed by taking the ordered carbon-based mesoporous material as a carrier and loading nanometer sulphur in porous channels; the composite material is sulphur-mesoporous carbon composite material which has high sulphur content, good dispersibility, high capacity and good stability, thereby overcoming the disadvantages of electricity-conducting material, finding good carrier material for the lithium-sulphur batteries and opening up new application field for the mesoporous material; the method in the invention has the advantages of low preparation process and low cost.
Description
Technical field
The present invention relates to a kind of ordered nano-structure sulphur/mesoporous carbon composite material that is used for lithium battery anode.
Technical background
Along with littler, lighter and developing rapidly of high performance electronic and communication apparatus more, people have especially proposed more and more higher requirement to specific energy to the battery performance that power supply is provided for these equipment.But the specific capacity of commercial lithium ion battery and MH/Ni battery has been difficult to continue to improve at present.Therefore, press for the higher battery of exploitation specific energy.Lithium-sulfur cell is a kind of serondary lithium battery that is celebrated with high-energy-density, high power density. it is S8+16Li-8Li that lithium-sulfur cell discharges and recharges reaction mechanism
2S, the right electrode potential of OR electricity is with respect to Li/Li
+Be 2.2V, be equivalent to 2/3 times of current potential of traditional positive electrode, and the course of reaction of its irregularity assimilation provides the theoretical capacity up to 1675mAh/g, made and work as Li
2S participates in reaction fully can provide the kg up to 2600Wh
-1Energy density.And the lithium-sulfur cell environmental friendliness, cost is low, and operating temperature is low, is widely used in the every aspect in national defence, space flight, machine power and the daily life.And the extremely low conductivity (5*10 of elemental sulfur self
-20S/cm) and the defective of the relatively poor and polysulfide of invertibity dissolving, these have all limited the practicability of lithium-sulfur cell.Therefore, the sulphur simple substance as positive active material must just can have significance of application with electric conducting material is compound.At present with regard to its employed electric conducting material, the polypropylene that mainly contains active carbon, carbon nano-tube, carbon fiber and pyrolysis fine (PAN) etc.And the ubiquitous problem of these material with carbon elements to be the contact area of sulphur and carbon be restricted, and then have influence on the content and the dispersiveness of sulphur, can't effectively resist problems such as polysulfide dissolving simultaneously, cause the poor stability of the lithium-sulfur cell assembled.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of ordered nano-structure sulphur/mesoporous carbon composite material that is used for lithium battery anode is provided.
For achieving the above object, the present invention adopts following technical scheme:
A kind of ordered nano-structure sulphur/mesoporous carbon composite material that is used for lithium battery anode is characterized in that this composite material is a carrier with orderly carbon back mesoporous material, has nanometer sulphur to form at its duct internal burden.
The content of nanometer sulphur is 10%～90% (mass fraction) in the described composite material.
Described orderly carbon back mesoporous material pore diameter range is 2～30nm.
Described orderly carbon back mesoporous material is: SUN-n series, CMK-n series or C-FDU-n series.
A kind of method for preparing the above-mentioned ordered nano-structure sulphur/mesoporous carbon composite material that is used for lithium battery anode, the concrete steps that it is characterized in that this method are: under inert atmosphere, the mixture of heating sulphur and orderly carbon back mesoporous material under 150～160 ℃ of temperature, the mass ratio of sulphur carbon is controlled at 1/9～4/1, and be incubated 3-6 hour, promptly obtain required ordered nano-structure sulphur/mesoporous carbon composite material.
A kind of method for preparing the above-mentioned ordered nano-structure sulphur/mesoporous carbon composite material that is used for lithium battery anode, the concrete steps that it is characterized in that this method are: the mass percent concentration of configuration sulphur is 8%～15% carbon disulfide solution, add orderly carbon back mesoporous material and constantly flood, dip time is 0.5～2 hour.
In order to test the electro-chemical activity of prepared material, it is 2016 lithium-sulfur cell that the present invention has prepared the model that can discharge and recharge with nano ordered sulphur/mesoporous carbon composite material as positive pole.Positive electrode preparation: mesoporous carbon-sulphur/Super-s carbon/PVDF=80%/10%/10% (mass ratio), after magnetic mixes 5-10h, blade coating is in the aluminium foil surface of cleaning, dry 12-24h under 80-120 ℃ in vacuum drying chamber, make the positive plate of certain diameter again, by forcing press anode pole piece is flattened at last; Negative pole adopts business-like lithium sheet; Electrolyte is the 1M LiPF of ethylene carbonate-dimethyl carbonate
6Solution.Prepared secondary lithium-sulfur cell at room temperature discharges and recharges with the current density of 0.1C, positive active material specific capacity 500-900mAh/g, and efficiency for charge-discharge is near 100%.
The present invention is big with conductivity height, specific surface first, the carbon back mesoporous material (SNU-n, CMK-n, C-FDU-n etc.) of aperture homogeneous, pore passage structure high-sequential is as the carrier material of the positive active material sulphur of lithium-sulfur cell, prepare the sulphur-mesoporous carbon composite material of sulfur content height, good dispersion, capacity height, good stability, not only overcome the shortcoming of above-mentioned electric conducting material, also for lithium-sulfur cell has found a kind of good carrier material, more mesoporous material has been opened up a kind of new application simultaneously.And the inventive method has, and preparation technology is simple, low cost and other advantages.
Description of drawings:
Fig. 1 is the TEM figure of the ordered mesoporous carbon material C-FDU-16 of 5-9nm for embodiment one used aperture.
Fig. 2 is the XRD photo of the ordered mesoporous carbon material C-FDU-16 of 5-9nm for embodiment one used aperture.
Fig. 3 is the TEM figure of the ordered mesoporous carbon material CMK-3 of 3-5nm for embodiment two used mesoporous apertures.
Fig. 4 is the XRD photo of the ordered mesoporous carbon material CMK-3 of 3-5nm for embodiment two used mesoporous apertures.
Fig. 5 heats the little angle XRD comparison diagram of compound front and back for sulphur-mesoporous carbon;
Fig. 6 heats compound front and back wide-angle XRD comparison diagram for sulphur-mesoporous carbon;
Fig. 7 is the electrochemical property test figure of the ordered nano-structure sulphur/mesoporous carbon composite material of embodiment one preparation.Wherein,
(a) be charging and discharging curve figure (voltage is to the time); (b) be the charging and discharging curve figure (voltage-contrast capacity) of this material;
(c) be the cyclic voltammogram first of this composite material; (d) be the cyclical stability curve chart.
Fig. 8 be ordered nano-structure sulphur/mesoporous carbon composite material of the present invention structural representation;
Embodiment
Embodiment 1: the employing aperture is that the ordered mesoporous carbon material C-FDU-16 of 5-9nm is a carrier.
(1) the lamina membranacea legal system preparation method that has a preface mesoporous carbon FDU-16 sees also Y.Meng, D.Gu, F.Q.Zhang, Y.F.Shi, H.F.Yang, Z.Li, C.Z.Yu, B.Tu, D.Y.Zhao, Angew.Chem.Int.Ed.2005,44,7053-7059.Specific as follows: as under 50 ℃,, to get 0.58mL in a clean beaker, add the NaOH liquid of the mass fraction 20% of 0.1mL simultaneously, magnetic agitation 30min with phenol liquefaction; Dropwise drip mass fraction 37% formalin of 1.30mL then, then be warmed up to 75 ℃ and stir 1h; 40 ℃ of-50 ℃ of dry 24h of vacuum get phenolic resins; Get 75 ℃ of stirrings of 1.6g surfactant F127, the rare HCl of 1g phenolic resins 1g0.2mol/L and 10mL ethanol continuation 2h and obtain a limpid yellow solution, in transfer and the evaporating dish, adopt the presoma of inducing the self assembly of volatilizing to synthesize mesoporous carbon; Under inert gas shielding, 1 ℃/min of presoma is heated to 600 ℃ then, 5 ℃/min is heated to 900 ℃ then, and is incubated 2-3 hour, and natural cooling fully grinds, and by 300 purpose sieves, promptly gets required meso-porous carbon material.
The TEM photo of prepared mesoporous carbon C-FDU-16 and XRD spectra are respectively referring to accompanying drawing 1,2, and Fig. 1 can see the orderly duct of prepared mesoporous carbon intuitively; Fig. 2 XRD figure spectrum characteristic peak occurs about 2 θ=1 °, proved the order of this nano material's structure indirectly.
(2) prepare composite material with dipping method: the mass fraction of configuration sulphur is 10% carbon disulfide solution; Mesoporous carbon is placed on the Buchner funnel, the mixed liquor of step 1 is cooked filtrate, with recirculated water filter pump continuous suction filtration, the time of control dipping, 0.5h-2h can get the composite material of different sulfur contents; The material of gained is dried by the fire 4-6h in 50 ℃ drying box; Nitrogen protection places 140 ℃ of insulations of tube furnace 0.5-1h, and purpose is removed carbon disulfide, promptly gets nano ordered sulphur/mesoporous carbon composite material at last.
Referring to accompanying drawing 6, sulphur-a ° diffraction peak intensity of locating diminishes even disappears in 2 θ=1 in carbon mix heating back, illustrates that the orderly duct of mesoporous carbon is filled by elemental sulfur; Referring to accompanying drawing 5, before the heating of sulphur-carbon mix, ° located to occur the three strongest ones peak of tangible elemental sulfur in 2 θ=1, and after the heating, the peak intensity of sulphur reduces significantly, has illustrated that crystallization sulphur successfully has been filled into the ordered nano duct of mesoporous carbon.If will detect the content of composite material sulphur, then can pass through the method for thermogravimetric (TGA).
Select sulphur-mesoporous carbon composite material of sulfur content wt60% for use, carried out electrochemical property test, referring to accompanying drawing 7, prepared as can be known composite material charging/discharging voltage is steady, is stabilized in 1.8-2.0V; Discharge capacity is bigger, and discharge capacity is near 1000mAh/g first; Good cycling stability, 20 times circulation volume is stabilized in about 560mAh/g.
Embodiment 2: adopting the CMK-3 in the mesoporous carbon CMK-n series is carrier.
(1) utilizes the hard template method preparation with nano ordered mesoporous material CMK-3, see also S.Jun, S.H.Joo, R.Ryoo., M.Kruk, M.Jaroniec, Z.Liu, T.Ohsuna, O.Terasaki, J.Am.Chem.Soc.2000,122,10712.Concrete steps are: 1. get SBA-15 about the 6nm of 1.0g aperture as template, 1.25g sucrose is carbon source, is dissolved in 5.0mL water, adds the 0.14g concentrated sulfuric acid simultaneously, ultrasonic mixing 1h, 100 ℃ of heating 12h, then 120 ℃ of heating 12h then; Step 2 is flooded once more, 0.8000g sucrose, and the 0.0900g concentrated sulfuric acid, 5.0mL water, heating condition is with step 1; Step 3, nitrogen protection places tube furnace, 900 ℃ of heating 6h; Step 4, the alkali alcoholic solution normal temperature of 20% hydrofluoric acid or mass fraction 40% stir 24h down, and purpose is to remove silicon dioxide.Prepared material C MK-3, its TEM picture and XRD spectra are seen accompanying drawing 3,4, can know the orderly duct of finding out mesoporous carbon by Fig. 3; As shown in Figure 4, about 2 θ=1 °, the obvious characteristics peak occurred, illustrated that prepared mesoporous nano material with carbon element has suitable order.
(2) prepare nano ordered sulphur-mesoporous carbon composite material: adopt the method for low temperature sulphur fusing to prepare sulphur-carbon complex: under inert gas shielding, with different proportion elemental sulfur/mesoporous carbon mixture, proportion is controlled at the mass fraction 10%-80% of sulphur.Place the tube furnace hall of temperature programmed control, the mixture of 155 ℃ of heating sulphur/mesoporous carbon, insulation 3-6h.
Same, can be by test, sulphur and mesoporous carbon are effectively compound, and this composite material has shown better electrochemical activation.
Embodiment 3: adopting the SNU-2 in the SNU-n series is carrier.
(1) altogether synthetic method prepares nano ordered meso-porous carbon material, the method document H.Q.Li that sees reference, R.L Liu, D.Y.Zhao, Y.Y.Xiao, Carbon.45 (2007) 2628-2635.
(2) prepare nano ordered sulphur/mesoporous carbon composite material: the mass fraction of configuration sulphur is 10% carbon disulfide solution; Mesoporous carbon is placed on the Buchner funnel, above-mentioned mixed liquor is cooked filtrate, with recirculated water filter pump continuous suction filtration, control time 0.5h-2h can get the composite material of sulphur different content; The material of gained is dried by the fire 4-6h in 50 ℃ drying box; Nitrogen protection places 140 ℃ of insulations of tube furnace 0.5-1h, promptly gets nano ordered sulphur/mesoporous carbon composite material at last.And be assembled into lithium-sulfur cell, showed excellent chemical property.
The schematic diagram of nano ordered sulphur/mesoporous carbon composite material that the present invention is prepared is seen accompanying drawing 8, and purpose all is the capillary attraction so as to mesoporous carbon, and liquid elemental sulfur is entered in the ordered nano duct of mesoporous carbon, and final and mesoporous carbon is compound preferably.
Claims (6)
1. an ordered nano-structure sulphur/mesoporous carbon composite material that is used for lithium battery anode is characterized in that this composite material is a carrier with orderly carbon back mesoporous material, has nanometer sulphur to form at its duct internal burden.
2. the ordered nano-structure sulphur/mesoporous carbon composite material that is used for lithium battery anode according to claim 1, the content that it is characterized in that nanometer sulphur in the described composite material is 10%～90%.
3. the ordered nano-structure sulphur/mesoporous carbon composite material that is used for lithium battery anode according to claim 1 is characterized in that described orderly carbon back mesoporous material pore diameter range is 2～30nm.
4. according to claim 1 or the 3 described ordered nano-structure sulphur/mesoporous carbon composite materials that are used for lithium battery anode, it is characterized in that described orderly carbon back mesoporous material is: SUN-n series, CMK-n series or C-FDU-n series.
5. method for preparing according to the ordered nano-structure sulphur/mesoporous carbon composite material that is used for lithium battery anode of claim 1, the concrete steps that it is characterized in that this method are: under inert atmosphere, the mixture of heating sulphur and orderly carbon back mesoporous material under 150～160 ℃ of temperature, the mass ratio of sulphur carbon is controlled at 1/9～4/1, and be incubated 3-6 hour, promptly obtain required ordered nano-structure sulphur/mesoporous carbon composite material.
6. one kind prepares the method that is used for the ordered nano-structure sulphur/mesoporous carbon composite material of lithium battery anode according to claim 1, the concrete steps that it is characterized in that this method are: the mass percent concentration of configuration sulphur is 8%～15% carbon disulfide solution, add orderly carbon back mesoporous material and constantly flood, dip time is 0.5～2 hour.
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| CN102299317A (en) * | 2011-07-14 | 2011-12-28 | 上海微纳科技有限公司 | High-rate LiFePO4/mesoporous carbon composite cathode material and preparation method thereof |
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Application publication date: 20100609 |