CN106571237A - Electrostatic spinning carbon nanotube polyaniline composite electrode material doped with modified oxidized graphite alkene - Google Patents
Electrostatic spinning carbon nanotube polyaniline composite electrode material doped with modified oxidized graphite alkene Download PDFInfo
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- CN106571237A CN106571237A CN201610929845.8A CN201610929845A CN106571237A CN 106571237 A CN106571237 A CN 106571237A CN 201610929845 A CN201610929845 A CN 201610929845A CN 106571237 A CN106571237 A CN 106571237A
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- electrostatic spinning
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/48—Conductive polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses an electrostatic spinning carbon nanotube polyaniline composite electrode material doped with modified oxidized graphite alkene. The electrostatic spinning carbon nanotube polyaniline composite electrode material is prepared by the following raw materials in parts by weight: 10-12 parts of multiwalled carbon nanotube, 1.5-1.6 parts of sodium dodecyl sulfate, an appropriate amount of deionized water, an appropriate amount of waterless ethanol, 10-12 parts of polyaniline, an appropriate amount of chloroform, 14-15 parts of polyoxyethylene, 12-13 parts of DL-10-Camphorsulfonic acid, 2.5-3 parts of oxidized graphite alkene, 2.8-3 parts of nickel nitrate hexahydrate, an appropriate amount of DMF, and 3-4 parts of formic acid. A network-shaped composite fiber film is produced via electrostatic spinning, contact area between electrode material and an electrolyte solution can be improved via a unique structure, and multiplying power characteristics and cycling stability of the material can be improved; compared with conventional technologies, the electrostatic spinning carbon nanotube polyaniline composite electrode material disclosed in the invention is advantaged by simplified manufacture processes, excellent performance and suitability for popularization.
Description
Technical field
The present invention relates to capacitor technology field, more particularly to a kind of electrostatic spinning carbon of addition modified graphene oxide is received
Mitron polyaniline composite electrode material.
Background technology
Ultracapacitor also known as electrochemical capacitor, with power density it is big, have extended cycle life, easy maintenance and cost
The features such as relative moderate.Ultracapacitor has the energy density and than battery higher power bigger than traditional dielectric capacitor
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 excellent mechanical property, thermal property, electric conductivity, and scientist's research is become
Focus.CNT is preferable composite addition phase, with 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.Electricity of the polyaniline as ultracapacitor electric conductive polymer
The advantages of pole material, environmental stability, high conductivity due to being readily synthesized, good, application has been widely studied.However, poly-
Aniline is because the shortcomings of Volume Changes are greatly with poor cycle charging/discharge capability, limits it in electrode of super capacitor material
Application in terms of material.These problems can be solved by the way that polyaniline is merged with c-based nanomaterial, so as to realize electrification
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 text
The method of suction filtration prepares carbon nanotube paper, and a volt-ampere electrochemicial oxidation is circulated to it, with the electrochemicial oxidation
Carbon nanotube paper based on, using electrochemical polymer deposition polyaniline, subsequently adsorb Graphene, prepare and there is sandwich
Carbon nano-tube/poly aniline/Graphene the composite nanometer carbon paper of sandwich structure, the compound carbon paper has good capacitance characteristic, big
Current charge-discharge electrical characteristics and good stable circulation performance.But operating procedure is complicated, it is difficult to control the structure of extrusion coating paper, with
As for being difficult to improve its specific surface area, the raising of specific capacitance is limited；And because the carbon produced in actual production process is received
Mitron can all 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, while nitration mixture process most of amorphous carbon and gold is eliminated
Metal particles, but processing procedure is loaded down with trivial details, it is seriously polluted, while some functional groups are have also been introduced, the presence pair of these functional groups
The structure of CNT causes certain destruction, so as to 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 which prepared operation is controllable, and 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.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of electrostatic of addition modified graphene oxide
Spinning CNT polyaniline composite electrode material.
The present invention is achieved by the following technical solutions：
A kind of electrostatic spinning CNT polyaniline composite electrode material of addition modified graphene oxide, by following weight portion
Raw material is made：It is multi-walled carbon nano-tubes 10-12, lauryl sodium sulfate 1.5-1.6, appropriate deionized water, appropriate absolute ethyl alcohol, poly-
Aniline 10-12, appropriate chloroform, polyethylene glycol oxide 14-15, DL camphorsulfonic acid 12-13, graphene oxide 2.5-3, six hydration nitre
Sour nickel 2.8-3, appropriate DMF, formic acid 3-4.
The electrostatic spinning CNT polyaniline composite electrode material of a kind of addition modified graphene oxide, by following
Concrete grammar is prepared from：
（1）Multi-walled carbon nano-tubes is placed on into graphite crucible stove, in being placed in graphitizing furnace, it is vacuumized, with 10-15 DEG C/
Min is warming up to 2800 DEG C, is incubated 20-20 hours, and natural cooling obtains graphitized carbon nano pipe；By above-mentioned graphitized carbon nano
Pipe was put in ball mill with the speed ball milling 90-120 minutes of 200-300 turn/part, and addition is dissolved in the 25-30 times of deionized water measured
Lauryl sodium sulfate, after ultrasonic 20-30 minutes be spray-dried, obtain modified carbon nano-tube；
（2）In the DMF that graphene oxide ultrasonic disperse to 8-10 times is measured, Nickelous nitrate hexahydrate, formic acid are subsequently adding, mixing is equal
Pour into after even in reactor, be placed in electrothermostat carries out solvent thermal reaction 20-24 hours, natural cooling at 95-100 DEG C
To room temperature, blackish green crystal is obtained, cleaned 3-4 time with DMF, be subsequently placed in vacuum drying chamber in 80-90 DEG C of drying, finally put
Enter in nano grinder and crush, obtain modified filler；
（3）Polyaniline is dissolved in the chloroform of 100 times of amounts, DL camphorsulfonic acid is added, with 300-400 rev/min under room temperature
Speed stirs 12-14 hours, is subsequently adding step（1）Step（2）The product for obtaining, ultrasonic disperse adds it after 20-30 minutes
Remaining residual components, continue to stir 10-12 hours with 300-400 rev/min of speed, obtain spinning solution；
（4）Spinning solution is drawn in syringe and spinning solution is collected on collector metallic nickel using electrostatic spinning technique, control
Spinning solution flow processed is 0.2-0.3ml/h, and voltage is 15-20kV, and spinning distance is 8-14cm, and spinning process 5-6 hour is formed
Composite fibre electrode material with certain thickness network structure.
It is an advantage of the invention that：The present invention carries out first the method for high temperature graphitization process to reach purifying to CNT
Effect, simultaneously metallic catalyst evaporates graphited, and CNT will not be destroyed, while degree of crystallinity and leading
Electrically improve；Then the CNT after graphitization, polyaniline, polyethylene glycol oxide etc. net has been made into using electrostatic spinning technique
The composite cellulosic membrane of network structure, causes the fiber of preparation thinner by controlling spinning distance, spinning flow etc., enhances it and compares table
Area, so that electrolyte ion diffusional resistance diminishes, charge transferring channel is more unobstructed, thus shows more preferable capacitive character
Can, specific capacitance is improve, and good cyclical stability is shown using ultracapacitor made by this electrode material, while
Process is simple, is easy to Industry Control.
The present invention is also reacted by using formic acid, Nickelous nitrate hexahydrate and graphene oxide, not only by graphite oxide
Alkene is reduced, and the graphene oxide layer cladding layer of Ni after reduction3(HCOO)6）, while increased specific surface area one is entered
Step improves the electric conductivity of material；The present invention makes network-like composite cellulosic membrane by electrostatic spinning, and this unique texture is favourable
In the contact area between electrode material and electrolyte solution is improved, the multiplying power property and cyclical stability of material are improved, and
And with traditional handicraft simplified in comparison manufacturing process, excellent performance, be obtained and promote.
Specific embodiment
A kind of electrostatic spinning CNT polyaniline composite electrode material of addition modified graphene oxide, by following weight
Part（Kilogram）Raw material make：Multi-walled carbon nano-tubes 10, lauryl sodium sulfate 1.5, appropriate deionized water, absolute ethyl alcohol are fitted
Amount, polyaniline 10, appropriate chloroform, polyethylene glycol oxide 14, DL camphorsulfonic acid 12, graphene oxide 2.5, Nickelous nitrate hexahydrate
2.8th, appropriate DMF, formic acid 3.
The electrostatic spinning CNT polyaniline composite electrode material of a kind of addition modified graphene oxide, by following
Concrete grammar is prepared from：
（1）Multi-walled carbon nano-tubes is placed on into graphite crucible stove, in being placed in graphitizing furnace, it is vacuumized, with 10 DEG C/min
2800 DEG C are warming up to, 20 hours are incubated, natural cooling obtains 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, addition is dissolved in the lauryl sodium sulfate of the deionized waters of 25 times of amounts,
Ultrasound is spray-dried after 20 minutes, obtains modified carbon nano-tube；
（2）By in the DMF of graphene oxide ultrasonic disperse to 8 times of amounts, Nickelous nitrate hexahydrate, formic acid are subsequently adding, are well mixed
After pour in reactor, be placed in electrothermostat carries out solvent thermal reaction 20 hours at 95 DEG C, naturally cools to room temperature, obtains
To blackish green crystal, cleaned with DMF 3 times, be subsequently placed in vacuum drying chamber in 80 DEG C of dryings, in being finally putting into nano grinder
Crush, obtain modified filler；
（3）Polyaniline is dissolved in the chloroform of 100 times of amounts, DL camphorsulfonic acid is added, with 300 revs/min of speed under room temperature
Stirring 12 hours, is subsequently adding step（1）Step（2）The product for obtaining, ultrasonic disperse adds remaining residual components after 20 minutes,
Continue to be stirred 10 hours with 300 revs/min of speed, obtain spinning solution；
（4）Spinning solution is drawn in syringe and spinning solution is collected on collector metallic nickel using electrostatic spinning technique, control
Spinning solution flow processed is 0.2ml/h, and voltage is 15kV, and spinning distance is 8cm, and 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 using made by the embodiment collect composite cellulosic membrane metallic nickel as electrode material with
Polyvinyl alcohol-sulfuric acid barrier film is stacked together by sandwich structure, and it is packaged with polyester film, obtains super capacitor
Device.Cyclic voltamogram curve when sweep speed is 5 mV s -1, potential region -0.8-0.2 V obtains super capacitor
The specific capacitance of device is 96F/g, and specific capacitance remains to be remained above 90% after 1 000 cycle charge discharge electrical testings.
Claims (2)
1. it is a kind of addition modified graphene oxide electrostatic spinning CNT polyaniline composite electrode material, it is characterised in that
It is prepared by the raw materials in：Multi-walled carbon nano-tubes 10-12, lauryl sodium sulfate 1.5-1.6, appropriate deionized water,
Appropriate absolute ethyl alcohol, polyaniline 10-12, appropriate chloroform, polyethylene glycol oxide 14-15, DL camphorsulfonic acid 12-13, graphite oxide
Alkene 2.5-3, Nickelous nitrate hexahydrate 2.8-3, appropriate DMF, formic acid 3-4.
2. according to claims 1 it is a kind of addition modified graphene oxide electrostatic spinning CNT polyaniline compound electric
Pole material, it is characterised in that be prepared from by following concrete grammar：
（1）Multi-walled carbon nano-tubes is placed on into graphite crucible stove, in being placed in graphitizing furnace, it is vacuumized, with 10-15 DEG C/
Min is warming up to 2800 DEG C, is incubated 20-20 hours, and natural cooling obtains graphitized carbon nano pipe；By above-mentioned graphitized carbon nano
Pipe was put in ball mill with the speed ball milling 90-120 minutes of 200-300 turn/part, and addition is dissolved in the 25-30 times of deionized water measured
Lauryl sodium sulfate, after ultrasonic 20-30 minutes be spray-dried, obtain modified carbon nano-tube；
（2）In the DMF that graphene oxide ultrasonic disperse to 8-10 times is measured, Nickelous nitrate hexahydrate, formic acid are subsequently adding, mixing is equal
Pour into after even in reactor, be placed in electrothermostat carries out solvent thermal reaction 20-24 hours, natural cooling at 95-100 DEG C
To room temperature, blackish green crystal is obtained, cleaned 3-4 time with DMF, be subsequently placed in vacuum drying chamber in 80-90 DEG C of drying, finally put
Enter in nano grinder and crush, obtain modified filler；
（3）Polyaniline is dissolved in the chloroform of 100 times of amounts, DL camphorsulfonic acid is added, with 300-400 rev/min under room temperature
Speed stirs 12-14 hours, is subsequently adding step（1）Step（2）The product for obtaining, ultrasonic disperse adds it after 20-30 minutes
Remaining residual components, continue to stir 10-12 hours with 300-400 rev/min of speed, obtain spinning solution；
（4）Spinning solution is drawn in syringe and spinning solution is collected on collector metallic nickel using electrostatic spinning technique, control
Spinning solution flow processed is 0.2-0.3ml/h, and voltage is 15-20kV, and spinning distance is 8-14cm, and spinning process 5-6 hour is formed
Composite fibre electrode material with certain thickness network structure.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610929845.8A CN106571237A (en) | 2016-10-31 | 2016-10-31 | Electrostatic spinning carbon nanotube polyaniline composite electrode material doped with modified oxidized graphite alkene |
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| CN201610929845.8A CN106571237A (en) | 2016-10-31 | 2016-10-31 | Electrostatic spinning carbon nanotube polyaniline composite electrode material doped with modified oxidized graphite alkene |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112609329A (en) * | 2020-12-11 | 2021-04-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of natural antibacterial and antiviral nanofiber membrane, product and application thereof |
Citations (1)
| 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 |
-
2016
- 2016-10-31 CN CN201610929845.8A patent/CN106571237A/en active Pending
Patent Citations (1)
| 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 |
Non-Patent Citations (3)
| Title |
|---|
| 付蓉蓉 等: ""Ni3（HCOO）6/还原氧化石墨烯复合电极材料的制备及电容性能"", 《高等学校化学学报》 * |
| 庞志鹏 等: ""碳纳米管导电纸的制备及改性研究"", 《功能材料》 * |
| 梁军生 等: ""静电纺丝PANI/CNT/PEO超级电容器电极的性能研究"", 《电子元件与材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112609329A (en) * | 2020-12-11 | 2021-04-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of natural antibacterial and antiviral nanofiber membrane, product and application thereof |
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