CN106409523A - Electrostatic spinning composite electrode material with doped modified lithium manganate added thereto - Google Patents
Electrostatic spinning composite electrode material with doped modified lithium manganate added thereto Download PDFInfo
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- CN106409523A CN106409523A CN201610929703.1A CN201610929703A CN106409523A CN 106409523 A CN106409523 A CN 106409523A CN 201610929703 A CN201610929703 A CN 201610929703A CN 106409523 A CN106409523 A CN 106409523A
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- 239000007772 electrode material Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 11
- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 8
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical class [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 title abstract description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 14
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920000767 polyaniline Polymers 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000009987 spinning Methods 0.000 claims description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 claims description 13
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 230000003068 static effect Effects 0.000 claims description 9
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 6
- MIOPJNTWMNEORI-UHFFFAOYSA-N camphorsulfonic acid Chemical compound C1CC2(CS(O)(=O)=O)C(=O)CC1C2(C)C MIOPJNTWMNEORI-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims 1
- 229920006389 polyphenyl polymer Polymers 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 abstract 2
- MIOPJNTWMNEORI-GMSGAONNSA-N (S)-camphorsulfonic acid Chemical compound C1C[C@@]2(CS(O)(=O)=O)C(=O)C[C@@H]1C2(C)C MIOPJNTWMNEORI-GMSGAONNSA-N 0.000 abstract 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 abstract 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 abstract 1
- 230000001351 cycling effect Effects 0.000 abstract 1
- -1 polyoxyethylene Polymers 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 description 10
- 239000002041 carbon nanotube Substances 0.000 description 6
- 229910021393 carbon nanotube Inorganic materials 0.000 description 6
- 229910021389 graphene Inorganic materials 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000007765 extrusion coating Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/40—Fibres
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses an electrostatic spinning composite electrode material with doped modified lithium manganate added thereto. The electrostatic spinning composite electrode material is prepared by the following raw materials in parts by weight: 10-12 parts of multiwall carbon nanotubes, 1.5-1.6 parts of sodium dodecyl sulfate, a proper amount of deionized water, a proper amount of absolute ethyl alcohol, 10-12 parts of polyaniline, a proper amount of chloroform, 14-15 parts of polyoxyethylene, 12-13 parts of dl-10-camphorsulfonic acid, 2-3 parts of electrolytic manganese dioxide, 2-3 parts of lithium carbonate, 0.3-0.35 part of nanometer alundum (Al2O3) and 0.2-0.25 part of niobium pentaoxide. Through a series of technologies, such components as the nanometer alundum (Al2O3), the niobium pentaoxide and the like are doped for preparation of lithium manganate, and the prepared modified lithium manganate is added for preparing the electrode material, such that the high-temperature circularity and the volume energy density of the electrode material are enhanced; and the electrode material prepared through electrostatic spinning has the advantages of large specific surface area, large specific capacitance and high cycling stability.
Description
Technical field
The present invention relates to capacitor technology field, more particularly, to a kind of Static Spinning compound electric adding doping vario-property LiMn2O4
Pole material.
Background technology
Ultracapacitor, also known as electrochemical capacitor, has that power density is big, has extended cycle life, easy maintenance and cost
The features such as relative moderate.Ultracapacitor has the energy density bigger than traditional dielectric capacitor and the power higher than battery
Density, has broad application prospects in fields such as emergency power supply, hybrid power, digital product, telecommunications.CNT since
Since 1991 are found, due to having excellent mechanical property, thermal property, electric conductivity, and become scientist's research
Focus.CNT is that preferable composite adds phase, has up to more than 1000 draw ratio, simultaneously because sp2
Orbital hybridization forms a large amount of delocalization p electronics, and electric conductivity is excellent.Polyaniline is as the electricity of ultracapacitor electric conductive polymer
Pole material, the advantages of environmental stability due to being readily synthesized, good, high conductivity, has been widely studied application.However, it is poly-
The shortcomings of aniline is because of Volume Changes big and poor cycle charging/discharge capability, limits it in electrode of super capacitor material
The application of material aspect.These problems can be solved, thus realizing electrification by being merged polyaniline with c-based nanomaterial
Learn the synergy of double layer capacitor and fake capacitance capacitor.Therefore, the nano-carbon material of bigger serface and satisfactory electrical conductivity
It is used as support material to obtain the combination electrode of high-performance and long circulation life.
《Carbon nano-tube/poly aniline/Graphene composite nanometer carbon paper and its electrochemical capacitor performance》Pass through vacuum in one literary composition
The method of suction filtration prepares carbon nanotube paper, and it is circulated with a volt-ampere electrochemicial oxidation, with this electrochemicial oxidation
Carbon nanotube paper be matrix, using electrochemical polymer deposition polyaniline, subsequently adsorb Graphene, preparation has sandwich
Carbon nano-tube/poly aniline/Graphene the composite nanometer carbon paper of sandwich structure, this compound carbon paper has good capacitance characteristic, big
Current charge-discharge electrical characteristics and good stable circulation performance.But operating procedure complexity is it is difficult to control the structure of extrusion coating paper, with
As for being difficult to improve its specific surface area, limit the raising than electric capacity；And the carbon due to producing in actual production process is received
Mitron all can remain the catalyst impurities of a part, and some amorphous carbon, and the presence of these impurity limits carbon nanometer
The use of pipe, using sour purifying carbon nano-tube in article, nitration mixture eliminates most of amorphous carbon and gold while process
Metal particles, but processing procedure is loaded down with trivial details, seriously polluted, have also been introduced some functional groups, the presence pair of these functional groups simultaneously
The structure of CNT causes certain destruction, thus can produce certain impact to performance, limits its performance；To sum up institute
State, need to carry out certain improvement to process meanses such that it is able to prepared operation is controlled, electric conductivity is strong, specific surface area is big, ratio is electric
Hold big electrode material for super capacitor, meet the demand of development in science and technology.
Content of the invention
The object of the invention is exactly the defect in order to make up prior art, provides a kind of electrostatic adding doping vario-property LiMn2O4
Spin combination electrode material.
The present invention is achieved by the following technical solutions：
A kind of Static Spinning combination electrode material adding doping vario-property LiMn2O4, is prepared by the raw materials in：Many walls carbon
Nanotube 10-12, lauryl sodium sulfate 1.5-1.6, appropriate deionized water, appropriate absolute ethyl alcohol, polyaniline 10-12, chloroform
In right amount, polyethylene glycol oxide 14-15, DL camphorsulfonic acid 12-13, electrolytic manganese dioxide 2-3, lithium carbonate 2-3, nanometer three oxidation two
Aluminium 0.3-0.35, five oxidation two girl 0.2-0.25.
Described a kind of add doping vario-property LiMn2O4 Static Spinning combination electrode material, prepared by following concrete grammar and
Become：
（1）Multi-walled carbon nano-tubes is placed on graphite crucible stove, is placed in graphitizing furnace, it is vacuumized, with 10-15 DEG C/
Min is warming up to 2800 DEG C, is incubated 20-20 hour, natural cooling, obtains graphitized carbon nano pipe；By above-mentioned graphitized carbon nano
Pipe is put in ball mill and is turned/speed ball milling 90-120 the minute of part with 200-300, adds the deionized water being dissolved in 25-30 times amount
Lauryl sodium sulfate, after ultrasonic 20-30 minute be spray-dried, obtain modified carbon nano-tube；
（2）By electrolytic manganese dioxide, lithium carbonate, nano-aluminium oxide mixing, put in chamber type electric resistance furnace, be warming up to 800-
850 DEG C, natural cooling after being incubated 12 hours, pulverize, mix with five oxidation two girls after crossing 800 mesh sieves, be continuously heating to 800-850
DEG C, cool down after insulation 9-10 hour, pulverized with nano grinder, obtain doping vario-property LiMn2O4；
（3）Polyaniline is dissolved in the chloroform of 100 times amount, adds DL camphorsulfonic acid, with 300-400 rev/min under room temperature
Speed stirs 12-14 hour, is subsequently adding step（1）Step（2）The product obtaining, adds it after ultrasonic disperse 20-30 minute
Remaining residual components, continue to stir 10-12 hour with 300-400 rev/min of speed, obtain spinning solution；
（4）Spinning solution is drawn in syringe and using electrostatic spinning technique, spinning solution is collected on collector metallic nickel, control
Spinning solution flow processed is 0.2-0.3ml/h, and voltage is 15-20kV, and spinning distance is 8-14cm, spinning process 5-6 hour, is formed
There is the composite fibre electrode material of certain thickness network structure.
It is an advantage of the invention that：The method that the present invention carries out high temperature graphitization process to CNT first to reach purifying
Effect, metallic catalyst evaporates simultaneously graphited, and CNT will not be destroyed, simultaneously degree of crystallinity and leading
Electrically improve；Then using electrostatic spinning technique, the CNT after graphitization, polyaniline, polyethylene glycol oxide etc. are made for net
The composite cellulosic membrane of network structure, makes the fiber of preparation thinner by controlling spinning distance, spinning flow etc., enhances it and compare table
Area, so that electrolyte ion diffusional resistance diminishes, charge transferring channel is more unobstructed, thus shows more preferable capacitive character
Can, improve ratio electric capacity, and show good cyclical stability using the ultracapacitor that this electrode material is made, simultaneously
Process is simple, is easy to Industry Control.
The compositions such as nano-aluminium oxide, five oxidation two girls are entrained in LiMn2O4 by a series of technique by the present invention
In preparation, the modified lithium manganate made is added in the preparation of electrode material, enhance electrode material high temperature circulation and
Volume energy density；The electrode material that Static Spinning of the present invention is made, specific surface area is big, bigger than electric capacity, and cyclical stability is high.
Specific embodiment
A kind of Static Spinning combination electrode material adding doping vario-property LiMn2O4, by following weight portion（Kilogram）Raw material system
Become：Multi-walled carbon nano-tubes 10, lauryl sodium sulfate 1.5, appropriate deionized water, appropriate absolute ethyl alcohol, polyaniline 10, chloroform are fitted
Amount, polyethylene glycol oxide 14, DL camphorsulfonic acid 12, electrolytic manganese dioxide 2, lithium carbonate 2, nano-aluminium oxide 0.3, five oxidation
Two girls 0.2.
A kind of Static Spinning combination electrode material adding doping vario-property LiMn2O4 according to claims 1, by following
Concrete grammar is prepared from：
（1）Multi-walled carbon nano-tubes is placed on graphite crucible stove, is placed in graphitizing furnace, it is vacuumized, with 10 DEG C/min
It is warming up to 2800 DEG C, be incubated 20 hours, natural cooling, obtain graphitized carbon nano pipe；Above-mentioned graphitized carbon nano pipe is put into
With the speed ball milling 90 minutes of 200 turns/part in ball mill, add the lauryl sodium sulfate of the deionized water being dissolved in 25 times amount,
It is spray-dried after ultrasonic 20 minutes, obtain modified carbon nano-tube；
（2）By electrolytic manganese dioxide, lithium carbonate, nano-aluminium oxide mixing, put in chamber type electric resistance furnace, be warming up to 800 DEG C,
Natural cooling after being incubated 12 hours, pulverizes, and mixes with five oxidation two girls, be continuously heating to 800 DEG C, insulation 9 is little after crossing 800 mesh sieves
When after cool down, with nano grinder pulverize, obtain doping vario-property LiMn2O4；
（3）Polyaniline is dissolved in the chloroform of 100 times amount, adds DL camphorsulfonic acid, with 300 revs/min of speed under room temperature
Stirring 12 hours, is subsequently adding step（1）Step（2）The product obtaining, ultrasonic disperse added remaining residual components after 20 minutes,
Continue to stir 10 hours with 300 revs/min of speed, obtain spinning solution；
（4）Spinning solution is drawn in syringe and using electrostatic spinning technique, spinning solution is collected on collector metallic nickel, control
Spinning solution flow processed is 0.2ml/h, and voltage is 15kV, and spinning distance is 8cm, spinning process 5 hours, is formed and has certain thickness
Network structure composite fibre electrode material.
Teflon septum is immersed in polyvinyl alcohol-sulfogel electrolyte, keep 20 minutes, after taking-up
Under room temperature natural evaporation be dried, then described embodiment is made collection composite cellulosic membrane metallic nickel as electrode material with
Polyvinyl alcohol-sulfuric acid barrier film is stacked together by sandwich structure, and with polyester film, it is packaged, and obtains super capacitor
Device.Sweep speed be 5 mV s 1, potential region 0.8-0.2 V when Cyclic voltamogram curve obtain super capacitor
The ratio electric capacity of device is 95 F/g, remains to be remained above 90% than electric capacity after 1 000 cycle charge discharge electrical testings.
Claims (2)
1. a kind of Static Spinning combination electrode material adding doping vario-property LiMn2O4 is it is characterised in that former by following weight portion
Material is made：Multi-walled carbon nano-tubes 10-12, lauryl sodium sulfate 1.5-1.6, appropriate deionized water, appropriate absolute ethyl alcohol, polyphenyl
Amine 10-12, appropriate chloroform, polyethylene glycol oxide 14-15, DL camphorsulfonic acid 12-13, electrolytic manganese dioxide 2-3, lithium carbonate 2-3,
Nano-aluminium oxide 0.3-0.35, five oxidation two girl 0.2-0.25.
2. a kind of Static Spinning combination electrode material adding doping vario-property LiMn2O4 according to claims 1, its feature exists
In being prepared from by following concrete grammar：
（1）Multi-walled carbon nano-tubes is placed on graphite crucible stove, is placed in graphitizing furnace, it is vacuumized, with 10-15 DEG C/
Min is warming up to 2800 DEG C, is incubated 20-20 hour, natural cooling, obtains graphitized carbon nano pipe；By above-mentioned graphitized carbon nano
Pipe is put in ball mill and is turned/speed ball milling 90-120 the minute of part with 200-300, adds the deionized water being dissolved in 25-30 times amount
Lauryl sodium sulfate, after ultrasonic 20-30 minute be spray-dried, obtain modified carbon nano-tube；
（2）By electrolytic manganese dioxide, lithium carbonate, nano-aluminium oxide mixing, put in chamber type electric resistance furnace, be warming up to 800-
850 DEG C, natural cooling after being incubated 12 hours, pulverize, mix with five oxidation two girls after crossing 800 mesh sieves, be continuously heating to 800-850
DEG C, cool down after insulation 9-10 hour, pulverized with nano grinder, obtain doping vario-property LiMn2O4；
（3）Polyaniline is dissolved in the chloroform of 100 times amount, adds DL camphorsulfonic acid, with 300-400 rev/min under room temperature
Speed stirs 12-14 hour, is subsequently adding step（1）Step（2）The product obtaining, adds it after ultrasonic disperse 20-30 minute
Remaining residual components, continue to stir 10-12 hour with 300-400 rev/min of speed, obtain spinning solution；
（4）Spinning solution is drawn in syringe and using electrostatic spinning technique, spinning solution is collected on collector metallic nickel, control
Spinning solution flow processed is 0.2-0.3ml/h, and voltage is 15-20kV, and spinning distance is 8-14cm, spinning process 5-6 hour, is formed
There is the composite fibre electrode material of certain thickness network structure.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112397848A (en) * | 2020-12-11 | 2021-02-23 | 宁波启新精合新能源研究院有限公司 | High-performance lithium ion battery diaphragm and preparation thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101130431A (en) * | 2006-08-23 | 2008-02-27 | 中国科学院金属研究所 | Method for purifying nano carbon fiber of multi-wall carbon nano-tube |
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| CN105977043A (en) * | 2016-04-07 | 2016-09-28 | 铜陵泰力电子有限公司 | Supercapacitor electrode material added with modified lignite and preparation method thereof |
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| CN112397848B (en) * | 2020-12-11 | 2023-03-24 | 宁波启新精合新能源研究院有限公司 | High-performance lithium ion battery diaphragm and preparation thereof |
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