CN106531450A - Electrostatic spinning composite electrode material with added copper nitrate-modified active carbon - Google Patents
Electrostatic spinning composite electrode material with added copper nitrate-modified active carbon Download PDFInfo
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- CN106531450A CN106531450A CN201610929779.4A CN201610929779A CN106531450A CN 106531450 A CN106531450 A CN 106531450A CN 201610929779 A CN201610929779 A CN 201610929779A CN 106531450 A CN106531450 A CN 106531450A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000007772 electrode material Substances 0.000 title claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 13
- 239000002131 composite material Substances 0.000 title claims abstract description 11
- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title abstract 2
- 229910052802 copper Inorganic materials 0.000 title abstract 2
- 239000010949 copper Substances 0.000 title abstract 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 13
- -1 polyoxyethylene Polymers 0.000 claims abstract description 13
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920000767 polyaniline Polymers 0.000 claims abstract description 12
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003077 lignite Substances 0.000 claims abstract description 8
- MIOPJNTWMNEORI-UHFFFAOYSA-N camphorsulfonic acid Chemical compound C1CC2(CS(O)(=O)=O)C(=O)CC1C2(C)C MIOPJNTWMNEORI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000835 fiber Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000009987 spinning Methods 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 10
- 230000003068 static effect Effects 0.000 claims description 8
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- 239000004141 Sodium laurylsulphate Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 238000001035 drying 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
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 239000003990 capacitor Substances 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 6
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 abstract 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 abstract 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 abstract 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 abstract 1
- 239000002041 carbon nanotube Substances 0.000 description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 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
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000005041 Mylar™ Substances 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 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
- 238000001523 electrospinning Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007765 extrusion coating Methods 0.000 description 1
- 238000001914 filtration 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
- 230000006872 improvement Effects 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
- 239000002923 metal particle Substances 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 239000000203 mixture 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
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000003643 water by type Substances 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
- H01G11/24—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
-
- 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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- 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
- H01G11/84—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)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses an electrostatic spinning composite electrode material with added copper nitrate-modified active carbon. The electrostatic spinning composite electrode material is prepared from the following raw materials in parts by weight: 10-12 parts of multiwalled carbon nanotubes, 1.5-1.6 parts of lauryl sodium 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-camphorsulfonic acid, 3-4 parts of lignite, 1-1.5 parts of 3mol/L potassium hydroxide, a proper amount of 2wt% copper nitrate solution and 2-3 parts of molybdenum disulfide. The prepared fiber membrane-to-electrode material is simple in process, industrial control is facilitated, a super-capacitor assembled by the electrode material is high in specific capacitance, and the electrochemical properties of AC impedance and the like of the capacitor are improved.
Description
Technical field
The present invention relates to capacitor technology field, more particularly to a kind of Static Spinning of addition copper nitrate modified activated carbon is combined
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 is with 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 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 it has been widely studied.However, poly-
The shortcomings of aniline is because of change in volume big and poor cycle charging/discharge capability, limits which in electrode of super capacitor material
Application in terms of material.These problems can be solved by polyaniline is merged with c-based nanomaterial, so as to realize electrification
Learn the synergism 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 sucking filtration prepares carbon nanotube paper, and a volt-ampere electrochemicial oxidation is circulated to which, with the electrochemicial oxidation
Carbon nanotube paper based on, using electrochemical polymer deposition polyaniline, subsequently adsorb Graphene, prepare with sandwich
Carbon nano-tube/poly aniline/Graphene the composite nanometer carbon paper of sandwich structure, the compound carbon paper have 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 as 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, eliminates most of amorphous carbon and gold while nitration mixture process
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 certain improvement to be carried out 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 for the defect for making up prior art, there is provided a kind of addition copper nitrate modified activated carbon it is quiet
Electrospinning combination electrode material.
The present invention is achieved by the following technical solutions：
A kind of Static Spinning combination electrode material of addition copper nitrate modified activated carbon, is prepared by the raw materials in：Many walls
CNT 10-12, sodium lauryl sulphate 1.5-1.6, appropriate deionized water, appropriate dehydrated alcohol, polyaniline 10-12, chlorine
Imitative appropriate, polyethylene glycol oxide 14-15, DL camphorsulfonic acid 12-13, brown coal 3-4,3mol/L potassium hydroxide 1-1.5, concentration 2wt%
Copper nitrate solution is appropriate, molybdenum bisuphide 2-3.
A kind of Static Spinning combination electrode material of the addition copper nitrate modified activated carbon, prepared by following concrete grammar and
Into：
（1）Multi-walled carbon nano-tubes is placed on into graphite crucible stove, is placed in graphitizing furnace, evacuation is carried out to which, 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 is dissolved in the 25-30 times of deionized water measured with the speed ball milling 90-120 minutes of 200-300 turn/part, addition in being put into ball mill
Sodium lauryl sulphate, after ultrasonic 20-30 minutes be spray-dried, obtain modified carbon nano-tube；
（2）Brown coal are mixed with 3mol/L potassium hydroxide and is put in resistance furnace, with the speed liter of 10-20 DEG C/min under nitrogen protection
, to 800-850 DEG C, after activation 60-90 minutes, natural cooling is stand-by for temperature；2-3 times of activated carbon addition obtained in above-mentioned activation is measured
In the copper nitrate solution of concentration 2wt%, stirred 24 hours with 400-500 rev/min of speed, filtered, drying is then placed in carbonization
In stove, 200 DEG C are warming up to the heating rate of 15-20 DEG C/min under nitrogen protection, obtain copper nitrate modified activated carbon；
（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 add which after 20-30 minutes
Remaining residual componentss, continue the speed stirring 10-12 hours with 300-400 rev/min, obtain spinning liquid；
（4）Spinning liquid is drawn in syringe and spinning liquid 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 the method for high temperature graphitization process to reach purification first to CNT
Effect, there is evaporation in metallic catalyst, CNT will not be destroyed simultaneously graphited, 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 which and compare 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 obtains modified activated carbon by activating brown coal, the modified carbonization of copper nitrate, is added in electrostatic spinning liquid
Fibrous membrane is made, the porosity of fibrous membrane is further enhancing, is increased specific surface area, electrode material can be strengthened to electrolyte
Wettability so that ultracapacitor specific capacitance increase；Fibrous membrane made by the present invention turns electrode material process is simple,
It is easy to Industry Control, the ultracapacitor specific capacitance being assembled into using this electrode material is high, and the electricity such as the AC impedance of capacitor
Chemical property is improved.
Specific embodiment
A kind of Static Spinning combination electrode material of addition copper nitrate modified activated carbon, by following weight portion（Kilogram）Raw material
Make：Multi-walled carbon nano-tubes 10, sodium lauryl sulphate 1.5, appropriate deionized water, appropriate dehydrated alcohol, polyaniline 10, chloroform
In right amount, polyethylene glycol oxide 14, DL camphorsulfonic acid 12, brown coal 3, the copper nitrate solution of 3mol/L potassium hydroxide 1, concentration 2wt% are fitted
Amount, molybdenum bisuphide 2.
A kind of Static Spinning combination electrode material of the addition copper nitrate modified activated carbon, prepared by following concrete grammar and
Into：
（1）Multi-walled carbon nano-tubes is placed on into graphite crucible stove, is placed in graphitizing furnace, evacuation is carried out to which, 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 sodium lauryl sulphate of the deionized waters of 25 times of amounts,
Ultrasound was spray-dried after 20 minutes, obtained modified carbon nano-tube；
（2）Brown coal are mixed with 3mol/L potassium hydroxide and is put in resistance furnace, heated up with the speed of 10 DEG C/min under nitrogen protection
To 800 DEG C, after activating 60 minutes, natural cooling is stand-by；Activated carbon obtained in above-mentioned activation is added concentration 2wt% of 2 times of amounts
In copper nitrate solution, stirred 24 hours with 400 revs/min of speed, filtered, drying is then placed in retort, under nitrogen protection
200 DEG C are warming up to the heating rate of 15 DEG C/min, copper nitrate modified activated carbon is obtained；
（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 add remaining residual components after 20 minutes,
Continue to stir 10 hours with 300 revs/min of speed, obtain spinning liquid；
（4）Spinning liquid is drawn in syringe and spinning liquid 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, formation have 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-sulphuric acid barrier film is stacked together by sandwich structure, and which is packaged with mylar, obtains super capacitor
Device.Cyclic voltamogram curve when scanning speed is 5 mV s 1, potential region 0.8-0.2 V obtains super capacitor
The specific capacitance of device is 93F/g, and after 1 000 cycle charge discharge electrical testings, specific capacitance remains to be remained above 90%.
Claims (2)
1. it is a kind of addition copper nitrate modified activated carbon Static Spinning combination electrode material, it is characterised in that by following weight portion
Raw material is made：It is multi-walled carbon nano-tubes 10-12, sodium lauryl sulphate 1.5-1.6, appropriate deionized water, appropriate dehydrated alcohol, poly-
Aniline 10-12, appropriate chloroform, polyethylene glycol oxide 14-15, DL camphorsulfonic acid 12-13, brown coal 3-4,3mol/L potassium hydroxide 1-
1.5th, the copper nitrate solution of concentration 2wt% is appropriate, molybdenum bisuphide 2-3.
2. according to claims 1 it is a kind of addition copper nitrate modified activated carbon Static Spinning combination electrode material, its feature
It is to be prepared from by following concrete grammar：
（1）Multi-walled carbon nano-tubes is placed on into graphite crucible stove, is placed in graphitizing furnace, evacuation is carried out to which, 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 is dissolved in the 25-30 times of deionized water measured with the speed ball milling 90-120 minutes of 200-300 turn/part, addition in being put into ball mill
Sodium lauryl sulphate, after ultrasonic 20-30 minutes be spray-dried, obtain modified carbon nano-tube；
（2）Brown coal are mixed with 3mol/L potassium hydroxide and is put in resistance furnace, with the speed liter of 10-20 DEG C/min under nitrogen protection
, to 800-850 DEG C, after activation 60-90 minutes, natural cooling is stand-by for temperature；2-3 times of activated carbon addition obtained in above-mentioned activation is measured
In the copper nitrate solution of concentration 2wt%, stirred 24 hours with 400-500 rev/min of speed, filtered, drying is then placed in carbonization
In stove, 200 DEG C are warming up to the heating rate of 15-20 DEG C/min under nitrogen protection, obtain copper nitrate modified activated carbon；
（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 add which after 20-30 minutes
Remaining residual componentss, continue the speed stirring 10-12 hours with 300-400 rev/min, obtain spinning liquid；
（4）Spinning liquid is drawn in syringe and spinning liquid 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610929779.4A CN106531450A (en) | 2016-10-31 | 2016-10-31 | Electrostatic spinning composite electrode material with added copper nitrate-modified active carbon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610929779.4A CN106531450A (en) | 2016-10-31 | 2016-10-31 | Electrostatic spinning composite electrode material with added copper nitrate-modified active carbon |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106531450A true CN106531450A (en) | 2017-03-22 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101807682A (en) * | 2010-04-09 | 2010-08-18 | 曲阜毅威能源股份有限公司 | Power spinel lithium manganese oxide anode material and preparation method thereof |
| CN103088465A (en) * | 2011-10-28 | 2013-05-08 | 香港理工大学 | Hollow graphite carbon nanometer sphere in-situ modification amorphous carbon nanometer fibers or carbon nano-tubes and preparation method thereof |
| 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 |
| CN105977020A (en) * | 2016-06-21 | 2016-09-28 | 闽江学院 | Fiber capacitor and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101807682A (en) * | 2010-04-09 | 2010-08-18 | 曲阜毅威能源股份有限公司 | Power spinel lithium manganese oxide anode material and preparation method thereof |
| CN103088465A (en) * | 2011-10-28 | 2013-05-08 | 香港理工大学 | Hollow graphite carbon nanometer sphere in-situ modification amorphous carbon nanometer fibers or carbon nano-tubes and preparation method thereof |
| 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 |
| CN105977020A (en) * | 2016-06-21 | 2016-09-28 | 闽江学院 | Fiber capacitor and preparation method thereof |
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