CN109802105A - A kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material, controllable method for preparing and application - Google Patents
A kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material, controllable method for preparing and application Download PDFInfo
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- CN109802105A CN109802105A CN201811582992.8A CN201811582992A CN109802105A CN 109802105 A CN109802105 A CN 109802105A CN 201811582992 A CN201811582992 A CN 201811582992A CN 109802105 A CN109802105 A CN 109802105A
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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
Abstract
The invention belongs to the technical field of lithium sulphur one-shot battery positive electrode, specifically a kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material, controllable method for preparing and applications.The composite material is one-dimensional nano-array structure, and composite material is grouped as by polyaniline, metal nanometer line and containing three groups of S material, and the mass percent of each component is respectively polyaniline 5-15%, metal nanometer line 15-25%, 60-80% containing S material.Metal nano fiber has good electric conductivity, and nano-wire array can significantly improve the transmission of lithium ion and electronics, alleviate the volume expansion in cyclic process, improves the specific capacity of battery.Polyaniline nano tube packaging Fe nanowire array/sulphur composite material provided by the present invention has many advantages, such as to carry sulfur content height, stable structure, can carry out high power discharge；Also have the characteristics that morphology controllable and ingredient are controllable.
Description
Technical field
The invention belongs to the technical field of lithium sulphur one-shot battery positive electrode, a kind of specifically polyaniline nanotube packet
Fill metal nanometer line array/sulphur composite material, controllable method for preparing and application.
Background technique
Li-S battery theoretical volume specific energy and specific energy are up to 2800 Wh/L and 2600 Wh/ respectively
Kg is much higher than " rocking chair type " lithium ion battery.Currently, lithium-sulfur cell is due to its extremely low cost, high specific energy and environment
Friendly causes great concern in the whole world, becomes one of most promising power battery.Currently, Most scholars are inclined to
It is developed and used in using Li-S battery as secondary cell, it is opposite to ignore its great potential used as one-shot battery.It is real
On border, the cyclical stability of Li-S battery, there is also certain gap, is even difficult to meet power compared with commercial Li-ion batteries
The application request of power supply.But the battery system has very high initial discharge specific capacity, even up to theoretical value, this
Make it suitable for the application of high-energy-density one-shot battery.Also, Li-S battery one is assembled to be in full power state, can be direct
To load supplying, production and use process all meet the requirement of one-shot battery.On the other hand, in the research and development of Li-S one-shot battery
In the process, more theory and practice experiences can be accumulated for the development of Li-S secondary cell.Meanwhile Li-S system can
Charge characteristic keeps it more more competitive than the primary battery reported in the past.
Currently, developing the most challenging task of Li-S one-shot battery is to further increase its practical specific energy, make up
The deficiency of existing commercialization one-shot battery.This is needed while improving active material utilization, reduces the matter of inert matter
Amount ratio.Currently, the content of inactive ingredients electrolyte occupies 30%~50% mass ratio in Li-S battery, much higher than lithium from
10~20% dosage in sub- battery is the major obstacle for improving battery energy density.In lithium ion battery, the work of electrolyte
With only conducting lithium ions interior circuit is connected；And in Li-S battery, in addition to ion transmitting effect, electrolyte also needs
Enough amounts come dissolve electric discharge the more lithium sulfides of intermediate product, expose fresh electrode interface, constantly to guarantee that discharge capacity is filled
Distribution is waved.Therefore, to reduce the usage amount of electrolyte, must improve as far as possible the effective electrochemical active surface of electrode interior,
Shorten the mass transfer path of more lithium sulfides, to guarantee excellent battery performance.
In existing lithium-sulfur cell technology, its inherent shortcoming is mainly overcome by the modification of sulphur anode.Chinese patent
CN103219519A discloses a kind of graphene/sulphur composite construction lithium sulfur battery anode material preparation method, prepare first sulphur powder,
Organic amine dispersion liquid and graphene organic solvent, are mixed to get third dispersion liquid for the two, are consolidated by the way that water or acid solution is added dropwise
Liquid separation, finally obtains lithium sulfur battery anode material, although the material improves the performance of lithium-sulfur cell to a certain extent,
The payload amount of sulphur is low in positive electrode, reduces the energy density of battery；In addition, grapheme material is expensive, increase
The manufacturing cost of battery.Chinese patent: CN106025216A discloses a kind of biomass carbon that can be used for lithium-sulphur cell positive electrode
The preparation method of material, this method is by carrying out high temperature cabonization to biomass carbon material, acid handles modified, melting and mixes sulphur etc. to make
For the lithium sulfur battery anode material with porosity, adsorptivity, which can improve the electric conductivity of electrode material, alleviate electrode
The volume expansion of material, improves the chemical property of battery, but the chemical stability through peracid treated material is poor.In
State's patent: CN106663797A discloses a kind of carbon that can be used for lithium-sulphur cell positive electrode/sulphur composite material, which has carbon bone
The co-continuous structure of frame and hole crosslinking, and there is high-specific surface area, the advantages that electric conductivity, thermal conductivity, but involved by this method
And carbonisation need to provide very high temperature, preparation cost is higher.
Summary of the invention
The present invention is to provide a kind of can control for lithium sulphur one-shot battery nano anode material for the above technical issues
Preparation Method specifically a kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material, controllable method for preparing and is answered
With.
The technical solution of the present invention is as follows:
A kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material, which is characterized in that the composite material is one-dimensional
Nano array structure, composite material are grouped as by polyaniline, metal nanometer line and containing three groups of S material, the quality percentage of each component
Number is respectively polyaniline 5-15%, metal nanometer line 15-25%, 60-80% containing S material.Metal nano fiber has good conduction
Property, nano-wire array can significantly improve the transmission of lithium ion and electronics, alleviate the volume expansion in cyclic process, improve electric
The specific capacity in pond.Polyaniline nano tube packaging Fe nanowire array/sulphur composite material provided by the present invention have carry sulfur content it is high,
Stable structure can carry out the advantages that high power discharge；Also have the characteristics that morphology controllable and ingredient are controllable.
Metal nanometer line of the present invention is Fe nanowire, the polyaniline nano tube packaging metal nanometer line array/sulphur
Composite material is specially polyaniline nano tube packaging Fe nanowire array/sulphur composite material.
It is another object of the present invention to provide a kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite woods
The controllable method for preparing of material, which is characterized in that using aluminium oxide as template, grow metal nanometer line with the method for electrochemical deposition
Array, it is finally compound with sulphur again, prepare the polyaniline nano tube packaging metal nanometer line that can be used for lithium sulphur one-shot battery anode
Array/sulphur composite material；Further preferably, polyaniline nano tube packaging metal nanometer line array/sulphur composite material is controllable
Preparation Method grows Fe nanowire array with the method for electrochemical deposition using aluminium oxide as template, finally compound with sulphur again, system
It is standby to go out to can be used for polyaniline nano tube packaging Fe nanowire array/sulphur composite material of lithium sulphur one-shot battery anode.
A kind of controllable method for preparing of polyaniline nano tube packaging metal nanometer line array/sulphur composite material, feature exist
In including the following steps:
The first step prepares second level template:
Alumina formwork is immersed in 0.3 M-0.4 M aniline -1MHCl solution A；0.5M-0.6M is added into solution A to toluene
Sodium sulfonate and 0.12 M -0.15 M ammonium metavanadate -1MHCI solution, polymerization reaction is in N2It carries out under atmosphere, reacts at room temperature
1.5-2.5 hours, then, template is taken out from solution, polished with alumina powder；It is spare as second level template；
Second step prepares polyaniline nano tube packaging Fe nanowire array:
Before electrochemical deposition iron, the side for the second level template that the first step obtains is spread over silver paste, as working electrode；Electrification
Learn deposition solution are as follows: FeSO4·7H2O, 250-270 g/l, H3BO330-40 g/l, ascorbic acid 1g/l；Iron is under
Mode on and is deposited in the duct of second level template；The iron of spilling can use FeCl3Solution removes；By obtained product spend from
Sub- water is washed several times repeatedly and is dried, and obtains polyaniline nano tube packaging Fe nanowire array；
Third step prepares polyaniline nano tube packaging Fe nanowire array/sulphur composite material:
The polyaniline nano tube packaging Fe nanowire array and nanometer sulphur powder 1:(1-3 in mass ratio that second step washing is finished) it is mixed
It closes, then uses mortar grinder 20-30 min, 5-20ml carbon disulfide solution is added dropwise during the grinding process, polyaniline nanotube is made
Pack Fe nanowire array/sulphur composite material.
Preferably, in the first step, the volume ratio of 0.5M paratoluenesulfonic acid sodium salt and 0.12 M ammonium metavanadate -1MHCI solution
For 1:1.
Preferably, in the first step, 0.4 M aniline -1MHCl solution and 0.5M paratoluenesulfonic acid sodium salt and 0.12 M metavanadic acid
The volume ratio of ammonium -1MHCI total solution is 1:1-1:2.
Another object of the present invention is to provide obtained polyaniline nano tube packaging metal nanometer line array/sulphur composite materials
It is compound as the application of lithium sulphur one-shot battery nano anode material, especially polyaniline nano tube packaging Fe nanowire array/sulphur
Application of the material as lithium sulphur one-shot battery nano anode material.
A kind of above-mentioned polyaniline nano tube packaging metal nanometer line array/sulphur composite material of beneficial effects of the present invention can
Preparation Method etc. is controlled, wherein involved raw material are commercially available.
Polyaniline nano tube packaging metal nanometer line array/sulphur composite material of the invention, metal nano fiber have good
Good electric conductivity, nano-wire array can significantly improve the transmission of lithium ion and electronics, and the volume alleviated in cyclic process is swollen
It is swollen, improve the specific capacity of battery.The composite material has many advantages, such as to carry sulfur content height, stable structure, can carry out high power discharge；
Also have the characteristics that morphology controllable and ingredient are controllable.
Detailed description of the invention
Fig. 1 is polyaniline nano tube packaging Fe nanowire array/sulphur composite material prepared by embodiment 1 as lithium sulphur electricity
Constant-current discharge curve for the first time when the anode of pond, in the case where current density is 0.1C.
Fig. 2 is polyaniline nano tube packaging Fe nanowire array/sulphur composite material prepared by embodiment 2 as lithium sulphur electricity
Constant-current discharge curve for the first time when the anode of pond, in the case where current density is 0.1C.
Specific embodiment
Below in conjunction with specific embodiments of the present invention, apparent and completion is carried out to technical solution of the present invention and is explained
It states.Described embodiment is only a part of the embodiments of the present invention, and is not whole, all in spirit and original of the invention
Within then, any modification, equivalent substitution, improvement and etc. done be should all be included in the protection scope of the present invention.
A kind of controllable method for preparing of the polyaniline nano tube packaging metal nanometer line array/sulphur composite material of embodiment 1
The first step prepares second level template:
Alumina formwork is immersed in the 0.3 M aniline -1MHCl solution A of 13 ml；0.5M pairs of 10 ml is added into solution A
Toluenesulfonic acid sodium salt and 0.12 M ammonium metavanadate -1MHCI solution, polymerization reaction is in N2It is carried out under atmosphere, it is small to react 1.5 at room temperature
When, then, template is taken out from solution, polished with alumina powder.It is spare as second level template.
Second step prepares polyaniline nano tube packaging Fe nanowire array:
Before electrochemical deposition brill, the side for the second level template that the first step obtains is spread over silver paste, as working electrode.Electrification
Learn deposition solution are as follows: FeSO4·7H2O, 255 g/l, H3BO340 g/l, ascorbic acid 1g/l.Iron is with side from bottom to top
Formula is deposited in the duct of second level template.The iron of spilling can use FeCl3Solution removes, the product deionized water that then will be obtained
Drying is washed several times and dried repeatedly, obtains polyaniline nano tube packaging Fe nanowire array.
Third step prepares polyaniline nano tube packaging Fe nanowire array/sulphur composite material:
The polyaniline nano tube packaging Fe nanowire array that second step washing finishes is mixed with nanometer sulphur powder 1:3 in mass ratio,
Then 30 min of mortar grinder is used, the obtained polyaniline nano tube packaging iron of 20ml carbon disulfide solution is added dropwise during the grinding process and receives
Nanowire arrays/sulphur composite material.
Assembled battery
By polyaniline nano tube packaging Fe nanowire array/sulphur composite material obtained and conductive agent and binder according to mass ratio
It is placed in mortar for 8: 1: 1 ratio, ground and mixed uniformly scratches on carbon containing aluminium foil at slurry, by slurry, dry at 55 DEG C
For 24 hours, flakiness is pushed in 5MPa pressure using tablet press machine, obtains positive plate.With gained polyaniline nano tube packaging Fe nanowire
Array/sulphur composite material is anode, metal Li piece is cathode, and electrolyte is added, battery assembly is carried out in glove box, is detained
Formula CR2025 half-cell.
Chemical property analysis (BTS-800, new prestige) is carried out to prepared sample.
Fig. 1 is the present embodiment polyaniline nano tube packaging Fe nanowire array/sulphur composite material assembling battery in electric current
Density is the constant-current discharge curve for the first time under 0.1C.
A kind of controllable method for preparing of the polyaniline nano tube packaging metal nanometer line array/sulphur composite material of embodiment 2,
The first step prepares second level template:
Alumina formwork is immersed to the 0.4 M aniline -1MHCl solution of 15 ml.0.6M pairs of 10 ml is added into this solution
Toluenesulfonic acid sodium salt and 0.14 M ammonium metavanadate -1MHCI solution, polymerization reaction is in N2It is carried out under atmosphere, it is small to react 2.5 at room temperature
When, then, template is taken out from solution, polished with alumina powder；It is spare as second level template；
Second step prepares polyaniline nano tube packaging Fe nanowire array:
Before electrochemical deposition brill, the side for the second level template that the first step obtains is spread over silver paste, as working electrode.Electrification
Learn deposition solution are as follows: FeSO4·7H2O, 266 g/l, H3BO340 g/l, ascorbic acid 1g/l.Iron is with side from bottom to top
Formula is deposited in the duct of second level template.The brill of spilling can use FeCl3Solution removes, the product deionization that then will be obtained
Water is washed several times repeatedly and is dried, and obtains polyaniline nano tube packaging Fe nanowire array.
Third step prepares polyaniline nano tube packaging Fe nanowire array/sulphur composite material:
The polyaniline nano tube packaging Fe nanowire array that second step washing finishes is mixed with nanometer sulphur powder 1:2 in mass ratio,
Then 30 min of mortar grinder is used, the obtained polyaniline nano tube packaging iron of 5ml carbon disulfide solution is added dropwise during the grinding process and receives
Nanowire arrays/sulphur composite material.
Assembled battery
By polyaniline nano tube packaging Fe nanowire array/sulphur composite material obtained and conductive agent and binder according to mass ratio
It is placed in mortar for 7: 2: 1 ratio, ground and mixed uniformly scratches on carbon containing aluminium foil at slurry, by slurry, dry at 55 DEG C
For 24 hours, flakiness is pushed in 5MPa pressure using tablet press machine, obtains positive plate.With gained polyaniline nano tube packaging Fe nanowire
Array/sulphur composite material is anode, metal Li piece is cathode, and electrolyte is added, battery assembly is carried out in glove box, is detained
Formula CR2025 half-cell.
Fig. 2 is to prepare polyaniline nano tube packaging Fe nanowire array/sulphur composite material conduct prepared by the present embodiment
Constant-current discharge curve for the first time when lithium-sulphur cell positive electrode, in the case where current density is 0.1C.With polyaniline nano tube packaging iron nanometer
Linear array/sulphur composite material does positive lithium-sulfur cell, and constant-current discharge specific capacity is 1435mAh/g for the first time.
Unaccomplished matter of the present invention is well-known technique.
Claims (8)
1. a kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material, which is characterized in that the composite material is one
Nano array structure is tieed up, composite material is grouped as by polyaniline, metal nanometer line and containing three groups of S material, the quality hundred of each component
Score is respectively polyaniline 5-15%, metal nanometer line 15-25%, 60-80% containing S material.
2. polyaniline nano tube packaging metal nanometer line array/sulphur composite material according to claim 1, feature exist
In the metal nanometer line is Fe nanowire.
3. a kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material as described in claim 1 is controllable
Preparation Method, which is characterized in that using aluminium oxide as template, grow metal nanometer line array with the method for electrochemical deposition, finally
It is compound with sulphur again, prepare can be used for lithium sulphur one-shot battery anode polyaniline nano tube packaging metal nanometer line array/sulphur it is multiple
Condensation material.
4. a kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material according to claim 3 is controllable
Preparation method, which is characterized in that using aluminium oxide as template, grow Fe nanowire array with the method for electrochemical deposition, finally
It is compound with sulphur again, prepare can be used for lithium sulphur one-shot battery anode polyaniline nano tube packaging Fe nanowire array/sulphur it is compound
Material.
5. a kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material according to claim 4 is controllable
Preparation method, which comprises the steps of:
The first step prepares second level template:
Alumina formwork is immersed in 0.3 M-0.4 M aniline -1MHCl solution A；0.5M-0.6M is added into solution A to toluene
Sodium sulfonate and 0.12 M -0.15 M ammonium metavanadate -1MHCI solution, polymerization reaction is in N2It carries out under atmosphere, reacts at room temperature
1.5-2.5 hours, then, template is taken out from solution, polished with alumina powder；It is spare as second level template；
Second step prepares polyaniline nano tube packaging Fe nanowire array:
Before electrochemical deposition iron, the side for the second level template that the first step obtains is spread over silver paste, as working electrode；Electrification
Learn deposition solution are as follows: FeSO4·7H2O, 250-270 g/l, H3BO330-40 g/l, ascorbic acid 1g/l；Iron is under
Mode on and is deposited in the duct of second level template；The iron of spilling can use FeCl3Solution removes；By obtained product spend from
Sub- water is washed several times repeatedly and is dried, and obtains polyaniline nano tube packaging Fe nanowire array；
Third step prepares polyaniline nano tube packaging Fe nanowire array/sulphur composite material:
The polyaniline nano tube packaging Fe nanowire array and nanometer sulphur powder 1:(1-3 in mass ratio that second step washing is finished) it is mixed
It closes, then uses mortar grinder 20-30 min, 5-20ml carbon disulfide solution is added dropwise during the grinding process, polyaniline nanotube is made
Pack Fe nanowire array/sulphur composite material.
6. a kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material according to claim 5 is controllable
Preparation method, which is characterized in that in the first step, the volume of 0.5M paratoluenesulfonic acid sodium salt and 0.12 M ammonium metavanadate -1MHCI solution
Than for 1:1.
7. a kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material according to claim 5 is controllable
Preparation method, which is characterized in that in the first step, 0.4 M aniline -1MHCl solution and 0.5M paratoluenesulfonic acid sodium salt and 0.12 M are inclined
The volume ratio of ammonium vanadate -1MHCI total solution is 1:1-1:2.
8. a kind of polyaniline nano tube packaging metal nanometer line array/sulphur composite material as claimed in claim 1 or 2 is as lithium
The application of sulphur one-shot battery nano anode material.
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