CN103700818A - Sulfur-carbon composite material with nitrogen-doped porous carbon nanofiber net-shaped structure, as well as preparation method and application of composite material - Google Patents
Sulfur-carbon composite material with nitrogen-doped porous carbon nanofiber net-shaped structure, as well as preparation method and application of composite material Download PDFInfo
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention belongs to the technical field of lithium sulfur batteries, specifically relates to a sulfur-carbon composite material with a nitrogen-doped porous carbon nanofiber net-shaped structure, as well as a preparation method and an application of the composite material. By taking a polypyrrole net-shaped structure which is synthesized by virtue of a soft template method as a raw material, taking the potassium hydroxide as a pore forming agent, and taking the nitrogen-doped carbon nanofiber net-shaped structure which is synthesized through high-temperature carbonization under nitrogen atmosphere and is in a porous structure as a precursor, the sulphur-carbon composite material which can be used as the anode of the lithium sulfur battery can be prepared through heat treatment with elemental sulfur. The preparation method provided by the invention is simple, and good in reproducibility, and the prepared composite material is uniform in structure distribution, and can be used as the anode of the lithium sulfur battery. Due to the nitrogen doping and the tridimensional net-shaped structure, for the material, the conductivity can be improved, a transmission path of lithium ions is shortened, meanwhile, the dissolving of the sulfur and intermediate product in an electrolyte can be prevented, the electrochemistry performance of a positive material of the lithium sulfur battery is improved, good specific discharge capacity, cycle performance and rate performance can be achieved.
Description
Technical field
The invention belongs to lithium-sulfur cell technical field, be specifically related to a kind of lithium sulfur battery anode material and its preparation method and application.
Background technology
Lithium-sulfur cell, it is anodal adopting elemental sulfur (or sulfur-containing compound), and lithium metal is negative pole, realizes a metalloid lithium secondary battery of mutually changing between chemical energy and electric energy by the chemical reaction between sulphur and lithium, and its theoretical specific capacity is 1675 mAh g
-1, theoretical energy density is 2600 Whkg
-1, actual energy density can reach 300 Whkg at present
-1, in the coming years, very likely bring up to 600 Whkg
-1left and right, with traditional lithium ion battery oxide electrode material, as cobalt acid lithium, LiMn2O4, LiFePO4 is compared, and sulfenyl positive electrode has unique advantage at aspects such as specific capacity, energy density and power densities.In addition, the advantages such as elemental sulfur also has that reserves are abundant, cost is lower, environmental friendliness, battery security are good, can meet preferably four aspects in following electrokinetic cell requirement, be high-energy-density, fail safe preferably, environmental protection and low cost, not only meet the requirement of electric automobile (EV) to electrokinetic cell, also meet portable type electronic product to chemical power source lightweight, miniaturization, low cost and nontoxic requirement, thereby lithium-sulfur cell is considered to one of secondary cell system of current tool research attraction.
But at present,, the development of lithium-sulfur cell and application are subject to all many-sided restrictions, are exactly wherein the impact of positive electrode.The conductivity of sulphur is low, and (5x 10
-30s/cm), and the polysulfide that lithium sulfur battery anode material produces in discharge process is soluble in organic electrolyte, this has not only caused the active material utilization that lithium-sulfur cell is lower, and the polysulfide after dissolving can move to negative pole, and is reduced into insoluble matter Li
2s
2/ Li
2s and being deposited on negative pole lithium, makes electrode structure suffer very havoc, causes battery capacity significantly to decay, poor [the J.H. Shin of cycle performance, E.J. Cairns, J. Electrochem. Soc. 155 (2008) A368 – A373], thereby limited its further Application and Development.In order to solve problem above, Recent study maximum are usingd the sulphur carbon anode composite material of carbon as carrier and conducting matrix grain, carbon not only has satisfactory electrical conductivity, also there is large pore volume and high-specific surface area, improved on the one hand the conductivity of composite material, on the other hand, its large pore volume having provides sulphur to become Li
2s
2/ Li
2the needed volumetric spaces of S, and the high-specific surface area having contributes to adsorb part polysulfide, thereby reduce dissolving [M. Rao, the X. Song of polysulfide in electrolyte, E.J. Cairns, Journal of Power Sources 205 (2012) 474 – 478].Structure by regulation and control material with carbon element is prepared active material utilization and the cycle performance that the composite material with different structure improves lithium-sulfur cell, obtained in this respect at present greater advance [S. Wei, H. Zhang, Y. Huang, W. Wang, Y. Xia, Z. Yu, Energy Environ. Sci. 4 (2011) 736 – 740].
Summary of the invention
The object of this invention is to provide cancellated lithium sulfur battery anode material of porous carbon nanofiber of the nitrogen doping that a kind of preparation technology is simple, chemical property is excellent and its preparation method and application.
It is raw material that the synthetic polypyrrole network structure of soft template method is take in the present invention, potassium hydroxide is pore creating material, under nitrogen atmosphere, after high temperature cabonization, the synthetic nitrogen-doped carbon nano-fiber network structure with loose structure is presoma, with elemental sulfur heat treatment, prepare the sulphur carbon composite that can be used for lithium-sulphur cell positive electrode, concrete steps are as follows:
A, synthesizing of polypyrrole template, concrete steps are: 0.02-0.03 mol CTAB is dissolved in 120-180 ml HCl solution (1 mol/L) completely, after magnetic agitation 5-10 min, the ammonium persulfate that adds 0.06-0.09 mol, continue to stir 0.5-1 h(and keep the temperature of reaction system all the time lower than 5 ℃), add the pyrrole monomer of 8.3-12.2 ml, sustained response 20-24 h in ice-water bath; Then by the solution filter obtaining extremely colourless and neutral with HCl solution and the deionized water washing of 1 mol/L, collect solid product and also in vacuum drying oven, at 70-80 ℃, be dried 10-12 h, obtain polypyrrole template;
B, synthesizing of porous carbon nanofiber (N-CNFWs) the network structure presoma of nitrogen doping, concrete steps are: the polypyrrole template obtaining in a step is risen to 600-700 ℃ and keep 1-2 h with 2-3 ℃/min in nitrogen atmosphere, then the carbon nano-fiber nitrogen of acquisition being adulterated and potassium hydroxide are dispersed in the 30-40 ml aqueous solution with the mass ratio of about 1:3, at room temperature stir 1-2 h, be warming up to subsequently 90-100 ℃ of evaporate to dryness solution, product is risen to 650-750 ℃ and keep 2-3 h with 2-4 ℃/min in nitrogen atmosphere, obtain the porous carbon nanofiber network structure presoma of nitrogen doping,
C, synthesizing of the network structure composite material (N-CNFWs/S) that the porous carbon nanofiber of nitrogen doping and sulphur form, concrete steps are: the porous carbon nanofiber network structure presoma of nitrogen doping is mixed with the mass ratio of sublimed sulfur with about 4:6, in mortar, grind 1-2 h, then mixture is sealed in the PTFE container that is full of nitrogen, at 155-160 ℃, heat treatment 50-70 h, obtains target product.
The inventive method, technique is simple, favorable reproducibility, carbon nano-fiber/sulphur network structure of the nitrogen doping of preparation is evenly distributed.Compared with the prior art, beneficial effect of the present invention is embodied in:
The doping of nitrogen element and tridimensional network, improved the conductivity of material greatly, and shortened the transmission path of lithium ion.The redox reaction of sulphur is limited in carrying out in abundant pore passage structure, stoped the dissolving in electrolyte of sulphur and intermediate product, greatly improved the chemical property of lithium sulfur battery anode material, obtained good specific discharge capacity, cycle performance and high rate performance.
Accompanying drawing explanation
Fig. 1 is ESEM and the transmission electron microscope photo of product N-CNFWs.Wherein, the scanning electron microscope (SEM) photograph that a is N-CNFWs, the transmission electron microscope picture that b is N-CNFWs.
Fig. 2 is ESEM and the transmission electron microscope photo of product N-CNFWs/S.Wherein, the scanning electron microscope (SEM) photograph that a is N-CNFWs/S, the transmission electron microscope picture that b is N-CNFWs/S.
Fig. 3 is that product N-CNFWs/S and conventional material CNF/S are at 175 mA g
-1electrochemistry cycle graph under discharging current.
Fig. 4 is the electrochemistry high rate performance figure of product N-CNFWs/S and CNF/S.The electric current of test is respectively 200 mA g
-1, 400 mA g
-1, 800 mA g
-1, 1200 mA g
-1, 1600 mA g
-1, 200 mA g
-1.
Embodiment
Below by embodiment, the present invention program is further described in detail.
1, the synthesis step of polypyrrole template is as follows: 0.02-0.03 mol CTAB is dissolved in 120-180 ml HCl solution (1-1.5 mol/L) completely, after magnetic agitation 5-10 min, the ammonium persulfate that adds 0.06-0.09 mol, continue to stir after 0.5-1 h and (keep the temperature of reaction system all the time lower than 5 ℃), the pyrrole monomer that adds 8.3-12.2 ml, sustained response 20-24 h in ice-water bath, then by the solution filter obtaining extremely colourless and neutral with HCl solution and the deionized water washing of 1-1.5 mol/L, collect solid product and in vacuum drying oven, at 70-80 ℃, be dried 10-12 h and can obtain.
2, the synthesis step of porous carbon nanofiber (N-CNFWs) the network structure presoma of nitrogen doping is as follows: the polypyrrole template obtaining in a step is risen to 650-700 ℃ and keep 1-2 h with 2-4 ℃/min in nitrogen atmosphere, then the carbon nano-fiber nitrogen of acquisition being adulterated and potassium hydroxide are dispersed in the 30-40 ml aqueous solution and at room temperature stir 1-2 h with the mass ratio of about 1:3, be warming up to subsequently 90-100 ℃ of evaporate to dryness solution, product is risen to 650-750 ℃ and keep 2-3 h to obtain with 2-4 ℃/min in nitrogen atmosphere.
3, the network structure composite material (N-CNFWs/S) that the porous carbon nanofiber of nitrogen doping and sulphur form, its synthesis step is, the porous carbon nanofiber network structure presoma of nitrogen doping and sublimed sulfur are mixed to be incorporated in the mass ratio of about 4:6 and in mortar, grind 1-2 h, then mixture is sealed in the PTFE container that is full of nitrogen, heat treatment 50-70 h can obtain product at 155-160 ℃.
Presentation of results:
(a) carbon nano-fiber of accompanying drawing 1 explanation nitrogen doping is that diameter is the tridimensional network of 80-100nm.
(b) accompanying drawing 2 explanation sulphur have been filled in the carbon nano-fiber network structure of nitrogen doping, and the structure of filling front and back material is not destroyed.
comparative example 1
By conventional carbon nano-fiber (Showa Giken Industrial Co., Ltd, Japan) by mixed being incorporated in of the mass ratio of about 4:6, in mortar, grind 1-2 h with sublimed sulfur, then mixture is sealed in the PTFE container that is full of nitrogen, heat treatment 50-70 h can obtain product at 155-160 ℃.
Presentation of results:
(a) accompanying drawing 3 explanations, under same test condition, N-CNFWs/S composite material shows higher initial specific discharge capacity and better cyclical stability;
(b) accompanying drawing 4 explanations, under same test condition, N-CNFWs/S composite material shows better high rate performance.
In sum, the present invention is raw material by take the synthetic polypyrrole network structure of soft template method, potassium hydroxide is pore creating material, under nitrogen atmosphere, after high temperature cabonization, the synthetic nitrogen-doped carbon nano-fiber network structure with loose structure is presoma, with elemental sulfur heat treatment, prepared the sulphur carbon composite for lithium-sulphur cell positive electrode.
On the one hand, the conductivity that the nitrogen doping of high-load and three-dimensional network structure have improved material, shortened the transmission path of lithium ion, on the other hand, sublimed sulfur is filled in the abundant pore passage structure of the carbon nano-fiber of nitrogen doping, has not only alleviated the volumetric expansion problem in discharge process, and reaction is limited in pore passage structure and is carried out, effectively stop active sulfur and intermediate product to the dissolving in organic electrolyte, finally improved cyclical stability and the high rate performance of material.Can in lithium-sulfur cell under field conditions (factors), apply.
Claims (4)
1. the preparation method of the cancellated sulphur carbon composite of porous carbon nanofiber of nitrogen doping, it is characterized in that take that the synthetic polypyrrole network structure of soft template method is raw material, potassium hydroxide is pore creating material, under nitrogen atmosphere, after high temperature cabonization, the synthetic nitrogen-doped carbon nano-fiber network structure with loose structure is presoma, with elemental sulfur heat treatment, prepare the sulphur carbon composite that can be used for lithium-sulphur cell positive electrode.
2. the preparation method of the sulphur carbon composite as described in claim 1, is characterized in that concrete steps are as follows:
Synthesizing of a, polypyrrole template, concrete steps are: 0.02-0.03 mol CTAB is dissolved in 120-180 ml 1-1.5 mol/L HCl solution completely, after magnetic agitation 5-10 min, the ammonium persulfate that adds 0.06-0.09 mol, continue to stir 0.5-1 h, keep the temperature of reaction system all the time lower than 5 ℃, add the pyrrole monomer of 8.3-12.2 ml, sustained response 20-24 h in ice-water bath; Then the solution filter obtaining is also extremely colourless and neutral with HCl solution and the deionized water washing of 1-1.5 mol/L, collect solid product and also in vacuum drying oven, at 70-80 ℃, be dried 10-12 h, obtain polypyrrole template;
B, synthesizing of the porous carbon nanofiber network structure presoma of nitrogen doping, concrete steps are: the polypyrrole template obtaining in step a is risen to 600-700 ℃ and keep 1-2 h with 2-4 ℃/min in nitrogen atmosphere, then the carbon nano-fiber nitrogen of acquisition being adulterated and potassium hydroxide are dispersed in the 30-40 ml aqueous solution with the mass ratio of about 1:3, at room temperature stir 1-2 h, be warming up to subsequently 90-100 ℃ of evaporate to dryness solution, product is risen to 650-750 ℃ and keep 2-3 h with 2-4 ℃/min in nitrogen atmosphere, obtain the porous carbon nanofiber network structure presoma of nitrogen doping,
Synthesizing of the network structure composite material that the porous carbon nanofiber of c, nitrogen doping and sulphur form, concrete steps are: the porous carbon nanofiber network structure presoma of nitrogen doping is mixed with the mass ratio of sublimed sulfur with about 2:3, in mortar, grind 1-2 h, then mixture is sealed in the PTFE container that is full of nitrogen, at 155-160 ℃, heat treatment 50-70 h, obtains target product.
3. the cancellated sulphur carbon composite of porous carbon nanofiber of the nitrogen doping being prepared by preparation method described in claim 1.
4. the cancellated sulphur carbon composite of porous carbon nanofiber of the nitrogen doping as described in claim 1 is as the application of lithium sulfur battery anode material.
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| CN105098185A (en) * | 2014-04-29 | 2015-11-25 | 华为技术有限公司 | Composite cathode material, preparation method thereof, lithium ion secondary battery negative plate and lithium ion secondary battery |
| CN105140490A (en) * | 2015-09-28 | 2015-12-09 | 中南大学 | Preparation method of lithium-sulfur battery flexible positive electrode |
| WO2015188726A1 (en) * | 2014-06-11 | 2015-12-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Nitrogen-doped graphene coated nano-sulfur anode composite material, and preparation method and application thereof |
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