CN106548874A - A kind of addition stannum antimony coats the Static Spinning combination electrode material of manganese dioxide - Google Patents

A kind of addition stannum antimony coats the Static Spinning combination electrode material of manganese dioxide Download PDF

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Publication number
CN106548874A
CN106548874A CN201610978759.6A CN201610978759A CN106548874A CN 106548874 A CN106548874 A CN 106548874A CN 201610978759 A CN201610978759 A CN 201610978759A CN 106548874 A CN106548874 A CN 106548874A
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electrode material
antimony
spinning
manganese dioxide
minutes
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万广文
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Tongling City Start Electronic Manufacturing Co Ltd
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Tongling City Start Electronic Manufacturing Co Ltd
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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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • 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
    • 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
    • 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
    • H01G11/46—Metal oxides
    • 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
    • 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
    • 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 a kind of addition stannum antimony coats the Static Spinning combination electrode material of manganese dioxide, it is prepared by the raw materials in：Multi-walled carbon nano-tubes 10 12, sodium lauryl sulphate 1.5 1.6, appropriate deionized water, appropriate dehydrated alcohol, polyaniline 10 12, appropriate chloroform, polyethylene glycol oxide 14 15, DL camphorsulfonic acid 12 13, manganese carbonate 1.2 1.3, concentration are the ethanol 56 60 of 95wt%, stannic chloride pentahydrate 0.8 1, Butter of antimony. 1 1.2.Manganese carbonate is coated herein by stannic chloride pentahydrate, Butter of antimony., stannum antimony is obtained by high-temperature calcination and coats manganese dioxide, with loose structure, so as to be conducive to the quick infiltration of electrolyte；Made by fibrous membrane electrode material there is good chemical property；Electrode material specific surface area made by the present invention is big, and specific capacitance is big, made by ultracapacitor possess higher capacity, good cyclical stability.

Description

A kind of addition stannum antimony coats the Static Spinning combination electrode material of manganese dioxide
Technical field
The present invention relates to capacitor technology field, more particularly to a kind of Static Spinning of addition stannum antimony cladding manganese dioxide 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 stannum antimony coats the quiet of manganese dioxide Electrospinning combination electrode material.
The present invention is achieved by the following technical solutions：
A kind of addition stannum antimony coats the Static Spinning combination electrode material of manganese dioxide, 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 The ethanol 56- of imitative appropriate, polyethylene glycol oxide 14-15, DL camphorsulfonic acid 12-13, manganese carbonate 1.2-1.3, concentration for 95wt% 60th, stannic chloride pentahydrate 0.8-1, Butter of antimony. 1-1.2.
A kind of Static Spinning combination electrode material of the addition stannum Sb doped manganese dioxide, 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）Ethanol of the concentration for 95wt% is mixed with deionized water, ethanol and deionized water ratio of the controlled concentration for 95wt% For 7:1, dispersed with stirring is uniform, adds stannic chloride pentahydrate, Butter of antimony., is heated to 30 DEG C, and stirring 30-40 minutes make its colloidal sol Change, be subsequently adding manganese carbonate, continue stirring 120-150 minutes after ultrasonic 60-90 minutes, solution left standstill 10-12 hours are centrifuged Separate, be vacuum dried at 60 DEG C, finally xerogel is put in tube furnace so that 2-3 hours are calcined at 400-500 DEG C, stannum is obtained Sb doped manganese dioxide；
（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.
Manganese carbonate is coated herein by stannic chloride pentahydrate, Butter of antimony., Xi Tibao is obtained by high-temperature calcination Manganese dioxide is covered, with loose structure, so as to be conducive to the quick infiltration of electrolyte；Made by fibrous membrane electrode material have it is good Good chemical property；Electrode material specific surface area made by the present invention is big, and specific capacitance is big, made by ultracapacitor possess more High capacity, good cyclical stability.
Specific embodiment
A kind of addition stannum antimony coats the Static Spinning combination electrode material of manganese dioxide, 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, the ethanol 56, stannic chloride pentahydrate of polyethylene glycol oxide 14, DL camphorsulfonic acid 12, manganese carbonate 1.2, concentration for 95wt% 0.8th, Butter of antimony. 1.
A kind of Static Spinning combination electrode material of the addition stannum Sb doped manganese dioxide, 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）Ethanol of the concentration for 95wt% is mixed with deionized water, ethanol and deionized water ratio of the controlled concentration for 95wt% For 7:1, dispersed with stirring is uniform, adds stannic chloride pentahydrate, Butter of antimony., is heated to 30 DEG C, and stirring makes its solation in 30 minutes, It is subsequently adding manganese carbonate, ultrasound continues stirring 120 minutes after 60 minutes, by solution left standstill 10 hours, centrifugation, at 60 DEG C Vacuum drying, is finally put in tube furnace xerogel to calcine 2 hours at 400 DEG C, obtains stannum Sb doped manganese dioxide；
（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 101F/g, and after 1 000 cycle charge discharge electrical testings, specific capacitance remains to be remained above 90%.

Claims (2)

1. a kind of addition stannum antimony coats the Static Spinning combination electrode material of manganese dioxide, 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, manganese carbonate 1.2-1.3, concentration are The ethanol 56-60 of 95wt%, stannic chloride pentahydrate 0.8-1, Butter of antimony. 1-1.2.
2. according to claims 1 it is a kind of addition stannum Sb doped manganese dioxide 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）Ethanol of the concentration for 95wt% is mixed with deionized water, ethanol and deionized water ratio of the controlled concentration for 95wt% For 7:1, dispersed with stirring is uniform, adds stannic chloride pentahydrate, Butter of antimony., is heated to 30 DEG C, and stirring 30-40 minutes make its colloidal sol Change, be subsequently adding manganese carbonate, continue stirring 120-150 minutes after ultrasonic 60-90 minutes, solution left standstill 10-12 hours are centrifuged Separate, be vacuum dried at 60 DEG C, finally xerogel is put in tube furnace so that 2-3 hours are calcined at 400-500 DEG C, stannum is obtained Sb doped manganese dioxide；
（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.
CN201610978759.6A 2016-11-08 2016-11-08 A kind of addition stannum antimony coats the Static Spinning combination electrode material of manganese dioxide Pending CN106548874A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111945252A (en) * 2020-08-19 2020-11-17 中国海洋大学 Method for preparing hollow antimony-based binary alloy composite nanofiber material based on electrostatic spinning and potassium storage application of hollow antimony-based binary alloy composite nanofiber material

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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
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
CN101849302A (en) * 2007-11-05 2010-09-29 纳米技术仪器公司 Nano graphene platelet-based composite anode compositions for lithium ion batteries
CN103811190A (en) * 2014-01-16 2014-05-21 天津大学 Antimony-doped tin dioxide coated porous manganese dioxide composite electrode material and preparation
CN103936987A (en) * 2014-05-08 2014-07-23 扬州大学 Carbon nanotube composite material and preparation method thereof
CN104495811A (en) * 2014-12-12 2015-04-08 盐城市新能源化学储能与动力电源研究中心 Graphene composite material and preparation method thereof
CN105206432A (en) * 2015-09-29 2015-12-30 南京绿索电子科技有限公司 Polyaniline nanometer tube array/copper oxide/manganese dioxide composite material electrode and manufacturing method and application thereof
CN105977020A (en) * 2016-06-21 2016-09-28 闽江学院 Fiber capacitor and preparation method thereof

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* Cited by examiner, † Cited by third party
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
CN101849302A (en) * 2007-11-05 2010-09-29 纳米技术仪器公司 Nano graphene platelet-based composite anode compositions for lithium ion batteries
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
CN103811190A (en) * 2014-01-16 2014-05-21 天津大学 Antimony-doped tin dioxide coated porous manganese dioxide composite electrode material and preparation
CN103936987A (en) * 2014-05-08 2014-07-23 扬州大学 Carbon nanotube composite material and preparation method thereof
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CN105977020A (en) * 2016-06-21 2016-09-28 闽江学院 Fiber capacitor and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111945252A (en) * 2020-08-19 2020-11-17 中国海洋大学 Method for preparing hollow antimony-based binary alloy composite nanofiber material based on electrostatic spinning and potassium storage application of hollow antimony-based binary alloy composite nanofiber material
CN111945252B (en) * 2020-08-19 2022-08-30 中国海洋大学 Method for preparing hollow antimony-based binary alloy composite nanofiber material based on electrostatic spinning and potassium storage application thereof

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