CN110136976A - A kind of fiber/graphene/carbon quantum dot/FeOF flexible electrode material preparation method - Google Patents

A kind of fiber/graphene/carbon quantum dot/FeOF flexible electrode material preparation method Download PDF

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CN110136976A
CN110136976A CN201910417504.6A CN201910417504A CN110136976A CN 110136976 A CN110136976 A CN 110136976A CN 201910417504 A CN201910417504 A CN 201910417504A CN 110136976 A CN110136976 A CN 110136976A
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graphene
quantum dot
carbon quantum
electrode material
fiber
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CN110136976B (en
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王薇
陆鑫
张技术
李涛
刘绍文
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Changshu Institute of Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/36Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention discloses a kind of fiber/graphene/carbon quantum dot/FeOF flexible electrode material preparation methods, the following steps are included: A, pretreated fabric being impregnated in containing graphene oxide suspension and being dried, repeats this step and obtain fiber/graphene oxide composite material several times;B, the step A material obtained is immersed in the hydrothermal reaction kettle containing carbon quantum dot, heating reaction synthesis obtains fiber/graphene/carbon quantum dot flexible electrode material.C, the step B material obtained is immersed in containing FeF3·3H2In the hydrothermal reaction kettle of O and alcoholic solution, heating reaction synthesis obtains fiber/graphene/carbon quantum dot/FeOF flexible electrode material.The area specific capacitance with higher of material made from the method for the present invention and power characteristic, cycle performance are superior.

Description

A kind of fiber/graphene/carbon quantum dot/FeOF flexible electrode material preparation method
Technical field
The present invention relates to a kind of preparation methods of flexible electrode material, more particularly to a kind of fiber/graphene/carbon quantum Point/FeOF flexible electrode material preparation method.
Background technique
Electrochemical capacitor is based on the specific functions such as its high capacity and high power density, is widely used in hybrid power vapour The fields such as vehicle, communication, national defence and wearable electronic.Become as current electronic equipment is just showing lightening and flexibility development Gesture, flexible display screen, distributed sensor, Electronic Paper and wearable multimedia device etc. be portable and wearable electronic day Benefit enters daily life.But traditional electrochemical capacitor volume is big, weight weight, shape are fixed, and far can not expire The demand for development of the current flexible electronic devices of foot.Urgent need develops that low with light weight and cost, small in size, chemical property is excellent Different and processing performance excellent flexible electrochemical capacitor and its electrode material.
Currently, the research and development of flexible electrochemical capacitor and electrode material have become international hot spot, it is existing both at home and abroad largely to close In the wearing comfort for how improving wearable energy storage device and chemical property etc. research how is improved, but high system Make cost, poor flexibility, lower durability and environmental factor dependence etc. and limits their real application.Carry green wood Material, design new construction are the important methods for improving wearable energy storage device performance and improving its environmental suitability.
Textile material is natural wearable material, and there is excellent wearing comfort, selection generality and mechanics to stablize Property etc..The material and surface nature of textile material have particularity, therefore the conductive materials such as carbon are difficult to be formed on its surface three-dimensional Continuous conductive network often uses a large amount of crosslinking agent, table to increase the interaction between conductive material and fabric Activating agent even binder in face enables conductive material preferably to adhere on the fabric, on the one hand the addition of these substances can block up Hole on plug fabric is unfavorable for the diffusion of electrolyte ion, influences the performance of its chemical property, on the other hand can make material Synthesis process is complicated, difficult, increases cost.
Summary of the invention
In view of the above-mentioned defects in the prior art, it is flexible that the present invention provides a kind of fiber/graphene/carbon quantum dot/FeOF The preparation method of electrode material solves textile material surface and is difficult to shaped conductive network, and cohesive force is not between conductive material and fabric The problem of foot, provides the material that can be applied to super capacitor and wearable product.The introducing of graphene and carbon quantum dot can At fiber surface and the internal composite electrode interface for forming high-specific surface area, the transmission rate of electronics can be enhanced, be convenient for Coming into full contact with for electrolyte and electrode material, is greatly improved electrode material performance.
Technical solution of the present invention is as follows: a kind of fiber/graphene/carbon quantum dot/FeOF flexible electrode material preparation side Method, comprising the following steps:
A, pretreated fabric is impregnated in graphene oxide suspension and dried, repeated this step and obtain several times To fiber/graphene oxide composite material, the graphene oxide suspension is by graphene oxide powder ultrasonic disperse in deionization It is made in water;
B, the fiber/graphene oxide composite material for obtaining step A is immersed in the hydrothermal reaction kettle containing carbon quantum dot, is added Thermal response synthesizes to obtain fiber/graphene/carbon quantum dot flexible electrode material;
C, fiber/graphene/carbon quanta point material that step B is obtained is immersed in containing FeF3·3H2O and alcoholic solution In hydrothermal reaction kettle, heating reaction synthesis obtains fiber/graphene/carbon quantum dot/FeOF flexible electrode material.
Further, the concentration of the graphene oxide suspension is 0.5-3mg/mL, and dip time is in the step A Drying temperature is 40-70 DEG C in 20-60min, the step A, drying time 2-3h.
Preferably, the number of repetition of the step A is 5-40 times.
Further, fiber/graphene oxide composite material is put into the aqueous solution containing carbon quantum dot and carries out by the step B Hydro-thermal reaction, carbon quantum dot concentration are 0.01mg/mL-0.08mg/mL, and hydrothermal temperature is 100-150 DEG C, time 1- 3h。
Further, the pretreated fabric is to pre-process fabric using aqueous slkali, then It is cleaned up, is dried with deionized water.
Preferably, the aqueous slkali is sodium hydroxide solution or sodium bicarbonate solution, and the concentration of the aqueous slkali is 0.5- 2mol/L, the pretreatment temperature are 90-120 DEG C, pretreatment time 1-3h, in the pretreatment drying temperature be 80 DEG C- 130 DEG C, drying time 1-3h.
Further, the alcohol is one of ethyl alcohol, propyl alcohol, isopropanol, butanol.
Preferably, the heating temperature that reaction is heated in the step C is 160 DEG C -220 DEG C, reaction time 4h-20h.
The advantages of technical solution provided by the present invention, is:
1, the carbon quantum dot for introducing high conductivity can be with containing these functional groups such as a large amount of carboxyl, hydroxyls in structure The effects of forming Van der Waals force, hydrogen bond with fabric power, meanwhile, carbon quantum dot partial size is small, can be easy to be embedded in fiber and fiber Between, this provides particularly important advantage for flexible electrode and coming into full contact with for electrolyte, to further increase material Quality specific capacitance, volumetric capacitance and energy density provide basis.
2, the present invention, which is combined using layer assembly with hydro-thermal method, is prepared for a kind of novel three-dimensional based on textile fabric growth Graphene/carbon quantum dot/FeOF super capacitance electrode material.The introducing of graphene and carbon quantum dot can be formed in fiber surface The composite electrode interface of high-specific surface area, can enhance the transmission rate of electronics, convenient for filling for electrolyte and electrode material Tap touching, is greatly improved electrode material performance.On this basis, that the carbon composite skeleton of good conductivity and specific capacitance is high, The FeOF of poorly conductive combines, and gives full play to advantage.
3, material prepared by the present invention can be used as the electrode material of supercapacitor, the material use flexible textile fiber Between the porous structure that has promote the diffusion of electrolyte ion, while 0 dimension carbon quantum dot and 2 also being made full use of to tie up graphene structures The more high-specific surface area that the three-dimensional conductive skeleton built has, the characteristics such as higher electron transfer rate, while also giving full play to carbon The high-ratio surface and high conduction performance of material effectively increase the contact interface of FeOF and carbon material, effectively dispersion FeOF, are that its is counterfeit Capacitive oxidation reduction reaction provides more reaction active sites, plays the advantage of the capacitor of FeOF, and ensure electronics in electrode material Quick transmission in material, to obtain high specific capacitance, high power density and high-energy density.
4, electrode material lightweight obtained, softness, area specific capacitance with higher and power characteristic, cycle performance are excellent More, synthesis is simple, and cost is relatively low, and durability is good, it is made to play bigger make in terms of wearable electronic product With value.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but not as a limitation of the invention.
The each implementation of fiber of the present invention/graphene/carbon quantum dot/FeOF flexible electrode material preparation method Graphene oxide powder is prepared by the following method in example: graphene oxide is carried out using improved Hummers synthetic method Preparation.1.5g powdered graphite is added to by 98% concentrated sulfuric acid of 10mL, 1.25g potassium thiosulfate and 1.25g phosphorus pentoxide group At mixture in, stir 4.5h under the conditions of 80 DEG C.Then obtained product is cleaned with deionized water, in vacuum oven In dried under the conditions of 50 DEG C.Product after drying is added in 98% concentrated sulfuric acid of 60mL, is slowly added into 7.5g high again later Potassium manganate, temperature is maintained at 20 DEG C hereinafter, then adding the deionized water of 125mL in the adition process of potassium permanganate.2h The hydrogen peroxide that 200mL deionized water and 10mL concentration are 30% is added afterwards, and solution becomes glassy yellow after 10min.Obtaining The solution of glassy yellow be centrifuged, then cleaned with diluted hydrochloric acid solution (concentrated hydrochloric acid/deionized water volume ratio is 1/10), Metal ion and sulfate ion are removed, is then cleaned again with deionized water to weakly acidic pH, finally in a vacuum drying oven in 50 DEG C drying obtains graphene oxide.
Carbon quantum dot is synthesized by hydro-thermal method, and the specific method is as follows: 2.298g monohydrate potassium is dissolved in 20mL deionization In water, 670 μ L ethylenediamines are added into citric acid solution, by closed in solution transfer reaction kettle, HMX1100-20 type atmosphere furnace In 200 DEG C of hydro-thermal reaction 5h, cooled to room temperature, product is dark-brown after hydro-thermal reaction, and reaction solution dialysis obtains most afterwards for 24 hours Final product.
Embodiment 1
Graphene oxide powder is add to deionized water, the oxidation stone that concentration is 1.5mg/mL is made in ultrasonic 60min Black alkene suspension.Cotton fabric, in 100 DEG C of processing 2h, is then cleaned up with deionized water with the sodium hydroxide solution of 1mol/L, 2h is dried in 110 DEG C of drying boxes.Pretreated cotton fabric is impregnated into the graphene oxide suspension prepared, in room Temperature after stirring 30min, is placed in 50 DEG C of vacuum drying ovens down and dries 2h, and repeated impregnations-drying course 20 times.By cotton/oxidation stone Black alkene compound fabric is immersed in the carbon quantum dot solution that concentration is 0.03mg/ml, 120 DEG C of reaction 2h in reaction kettle, then Taking-up is cleaned 3 times with deionized water, in 100 DEG C of drying 2h, obtains cotton/graphene/carbon quantum dot composite material.
Cotton/graphene/carbon quantum dot composite material is immersed in containing FeF3·3H2O and ethyl alcohol (quality (g): volume (ml)=2.08:1) in hydrothermal reaction kettle, 180 DEG C of reaction 12h, synthesis obtains fiber/graphene/carbon quantum dot/FeOF electrode Material carries out 80 DEG C of drying 2h to the material, and measuring sheet resistance is 108 Ω/sq, and when sweep speed is 5m V/s, specific capacitance can Up to 316F/g, and there is good flex capability.
Comparative example 1
Graphene oxide powder is add to deionized water, the oxidation stone that concentration is 1.5mg/mL is made in ultrasonic 60min Black alkene suspension.Cotton fabric, in 100 DEG C of processing 2h, is then cleaned up with deionized water with the sodium hydroxide solution of 1mol/L, 2h is dried in 110 DEG C of drying boxes.Pretreated cotton fabric is impregnated into the graphene oxide suspension prepared, in room Temperature after stirring 30min, is placed in 50 DEG C of vacuum drying ovens down and dries 2h, and repeated impregnations-drying course 20 times.By cotton/oxidation stone Black alkene compound fabric is immersed in the NaBH that concentration is 0.5mol/L4In solution, 12h is stirred in room temperature condition, then takes out and spends Ionized water cleans 3 times, and in 100 DEG C of drying 2h, reduction obtains cotton/graphene composite material.
Cotton/graphene composite material is immersed in containing FeF3·3H2O and ethyl alcohol (quality (g): volume (ml)= 2.08:1) in hydrothermal reaction kettle, 180 DEG C of reaction 12h, synthesis obtain fiber/graphene/FeOF electrode material, to the material into 80 DEG C of drying 2h of row, measuring sheet resistance is 126 Ω/sq, and when sweep speed is 5m V/s, specific capacitance has up to 256F/g There is good flex capability.
Embodiment 2
Graphene oxide powder is add to deionized water, the graphite oxide that concentration is 2mg/mL is made in ultrasonic 30min Alkene suspension.Cotton fabric, in 90 DEG C of processing 3h, is then cleaned up with deionized water with the sodium bicarbonate solution of 0.5mol/L, in 2.5h is dried in 100 DEG C of drying boxes.Pretreated cotton fabric is impregnated into the graphene oxide suspension prepared, in room Temperature after stirring 20min, is placed in 50 DEG C of vacuum drying ovens down and dries 3h, and repeated impregnations-drying course 30 times.By cotton/oxidation stone Black alkene compound fabric is immersed in the carbon quantum dot solution that concentration is 0.04mg/ml, 110 DEG C of reaction 3h in reaction kettle, then Taking-up is cleaned 3 times with deionized water, in 100 DEG C of drying 2h, obtains cotton/graphene/carbon quantum dot composite material.
Cotton/graphene/carbon quantum dot composite material is immersed in FeF3·3H2O and ethyl alcohol (quality (g): volume (ml) =2.08:1) in hydrothermal reaction kettle, 200 DEG C of reaction 8h, synthesis obtains fiber/graphene/carbon quantum dot/FeOF electrode material, 80 DEG C of drying 2h are carried out to the material, measuring sheet resistance is 115 Ω/sq, and when sweep speed is 5mV/s, specific capacitance is up to 322F/ G, and there is good flex capability.
Embodiment 3
Graphene oxide powder is add to deionized water, the graphite oxide that concentration is 3mg/mL is made in ultrasonic 30min Alkene suspension.Dacron, in 120 DEG C of processing 1.5h, is then cleaned with deionized water dry with the sodium bicarbonate solution of 2mol/L Only, 3h is dried in 80 DEG C of drying boxes.Pretreated terylene is impregnated into the graphene oxide suspension prepared, in room Temperature after stirring 50min, is placed in 60 DEG C of vacuum drying ovens down and dries 2.5h, and repeated impregnations-drying course 40 times.By dacron/ Graphene oxide compound fabric is immersed in the carbon quantum dot solution that concentration is 0.06mg/ml, 120 DEG C of reactions in reaction kettle 3h then takes out and is cleaned 3 times with deionized water, in 100 DEG C of drying 2h, obtains terylene/graphene/carbon quantum dot composite material.
Dacron/graphene/carbon quantum dot composite material is immersed in FeF3·3H2O and propyl alcohol (quality (g): volume (ml)=2.08:1) in hydrothermal reaction kettle, 160 DEG C of reaction 20h, synthesis obtains fiber/graphene/carbon quantum dot/FeOF electrode Material carries out 80 DEG C of drying 2h to the material, and measuring sheet resistance is 167 Ω/sq, and when sweep speed is 5mV/s, specific capacitance is reachable 299F/g, and there is good flex capability.
Comparative example 2
Graphene oxide powder is add to deionized water, the graphite oxide that concentration is 3mg/mL is made in ultrasonic 30min Alkene suspension.Dacron, in 120 DEG C of processing 1.5h, is then cleaned with deionized water dry with the sodium bicarbonate solution of 2mol/L Only, 3h is dried in 80 DEG C of drying boxes.Pretreated terylene is impregnated into the graphene oxide suspension prepared, in room Temperature after stirring 50min, is placed in 60 DEG C of vacuum drying ovens down and dries 2.5h, and repeated impregnations-drying course 40 times.By dacron/ Graphene oxide compound fabric is immersed in the NaBH that concentration is 1mol/L4In solution, 12h is stirred in room temperature condition, is then taken out It is cleaned 3 times with deionized water, in 100 DEG C of drying 2h, reduction obtains dacron/graphene composite material.
Dacron/graphene composite material is immersed in FeF3·3H2O and propyl alcohol (quality (g): volume (ml)= 2.08:1) in hydrothermal reaction kettle, 160 DEG C of reaction 20h, synthesis obtains fiber/graphene/carbon quantum dot/FeOF electrode material, right The material carries out 80 DEG C of drying 2h, and measuring sheet resistance is 188 Ω/sq, when sweep speed is 5mV/s, specific capacitance up to 242F/g, And there is good flex capability.
Embodiment 4
Graphene oxide powder is add to deionized water, the oxidation stone that concentration is 0.5mg/mL is made in ultrasonic 30min Black alkene suspension.Nylon fabric, in 120 DEG C of processing 2.5h, is then cleaned with deionized water with the sodium hydroxide solution of 1.5mol/L Completely, 1.5h is dried in 130 DEG C of drying boxes.Pretreated polyamide fibre is impregnated into the graphene oxide suspension prepared In, after stirring 60min at room temperature, it is placed in 70 DEG C of vacuum drying ovens and dries 2h, repeated impregnations-drying course 10 times.By polyamide fibre Fabric/graphene oxide compound fabric is immersed in the carbon quantum dot solution that concentration is 0.08mg/ml, 140 DEG C in reaction kettle 2h is reacted, then takes out and is cleaned 3 times with deionized water, in 100 DEG C of drying 2h, it is multiple to obtain nylon fabric/graphene/carbon quantum dot Condensation material.
Nylon fabric/graphene/carbon quantum dot composite material is immersed in containing FeF3·3H2O and ethyl alcohol (quality (g): Volume (ml)=2.08:1) in hydrothermal reaction kettle, 140 DEG C of reaction 20h, synthesis obtains fiber/graphene/carbon quantum dot/FeOF Electrode material carries out 80 DEG C of drying 2h to the material, and measuring sheet resistance is 388 Ω/sq, when sweep speed is 5mV/s, specific capacitance Up to 237F/g, and there is good flex capability.
Embodiment 5
Graphene oxide powder is add to deionized water, the graphite oxide that concentration is 1mg/mL is made in ultrasonic 30min Alkene suspension.Non-woven fabrics fabric, in 100 DEG C of processing 3h, is then cleaned with deionized water dry with the sodium hydroxide solution of 0.5mol/L Only, 1h is dried in 120 DEG C of drying boxes.Pretreated non-woven fabrics fabric is impregnated into the graphene oxide suspension prepared In, after stirring 30min at room temperature, it is placed in 40 DEG C of vacuum drying ovens and dries 3h, repeated impregnations-drying course 5 times.By nonwoven Cloth/graphene oxide compound fabric is immersed in the carbon quantum dot solution that concentration is 0.06mg/ml, in reaction kettle 140 DEG C it is anti- 2h is answered, then takes out and is cleaned 3 times with deionized water, in 100 DEG C of drying 2h, obtains non-woven fabrics/graphene/carbon quantum dot composite wood Material.
Non-woven fabrics/graphene/carbon quantum dot composite material is immersed in containing FeF3·3H2O and butanol (quality (g): body Product (ml)=2.08:1) in hydrothermal reaction kettle, 180 DEG C of reaction 12h, it is electric that synthesis obtains fiber/graphene/carbon quantum dot/FeOF Pole material carries out 80 DEG C of drying 2h to the material, and measuring sheet resistance is 412 Ω/sq, and when sweep speed is 5mV/s, specific capacitance can Up to 229F/g, and there is good flex capability.
Comparative example 3
Oxidation stone alkene powder is add to deionized water, the graphene oxide that concentration is 1mg/mL is made in ultrasonic 30min Suspension.Non-woven fabrics fabric, in 100 DEG C of processing 3h, is then cleaned with deionized water dry with the sodium hydroxide solution of 0.5mol/L Only, 1h is dried in 120 DEG C of drying boxes.Pretreated non-woven fabrics fabric is impregnated into the graphene oxide suspension prepared In, after stirring 30min at room temperature, it is placed in 40 DEG C of vacuum drying ovens and dries 3h, repeated impregnations-drying course 5 times.By nonwoven Cloth/graphene oxide compound fabric is immersed in the NaBH that concentration is 1mol/L4In solution, 12h is stirred in room temperature condition, is then taken It is cleaned 3 times with deionized water out, in 100 DEG C of drying 2h, reduction obtains non-woven fabrics/graphene composite material.
Non-woven fabrics/graphene composite material is immersed in containing FeF3·3H2O and butanol (quality (g): volume (ml)= 2.08:1) in hydrothermal reaction kettle, 180 DEG C of reaction 12h, synthesis obtain fiber/graphene/FeOF electrode material, to the material into 80 DEG C of drying 2h of row, measure 436 Ω of sheet resistance/sq, and when sweep speed is 5mV/s, specific capacitance has good up to 189F/g Flex capability.

Claims (8)

1. a kind of fiber/graphene/carbon quantum dot/FeOF flexible electrode material preparation method, which is characterized in that including following Step:
A, pretreated fabric is impregnated in graphene oxide suspension and dried, repeated this step and obtain fibre several times Dimension/graphene oxide composite material, the graphene oxide suspension be by graphene oxide powder ultrasonic disperse in deionized water It is made;
B, fiber/graphene oxide composite material is put into the aqueous solution containing carbon quantum dot, hydro-thermal reaction prepares fiber/graphite Alkene/carbon quantum dot electrode material;
C, fiber/graphene/carbon quanta point material that step B is obtained is immersed in containing FeF3·3H2The hydro-thermal of O and alcoholic solution In reaction kettle, heating reaction synthesis obtains fiber/graphene/carbon quantum dot/cobalt sulfide nickel flexible electrode material.
2. fiber according to claim 1/graphene/carbon quantum dot/FeOF flexible electrode material preparation method, special Sign is that the concentration of the graphene oxide suspension is 0.5-3mg/mL, and dip time is 20-60min in the step A, Drying temperature is 40-70 DEG C in the step A, drying time 2-3h.
3. fiber according to claim 1/graphene/carbon quantum dot/FeOF flexible electrode material preparation method, special Sign is that the number of repetition of the step A is 5-40 times.
4. fiber according to claim 1/graphene/carbon quantum dot/FeOF flexible electrode material preparation method, special Sign is that fiber/graphene oxide composite material is put into the aqueous solution containing carbon quantum dot and carries out hydro-thermal reaction by the step B, The concentration of aqueous solution of the carbon quantum dot is 0.01mg/mL-0.08mg/mL, and hydrothermal temperature is 100-150 DEG C, and the time is 1-3h。
5. fiber according to claim 1/graphene/carbon quantum dot/FeOF flexible electrode material preparation method, special Sign is that the pretreated fabric is to pre-process fabric using aqueous slkali, then uses deionized water It cleans up, dries.
6. fiber according to claim 5/graphene/carbon quantum dot/FeOF flexible electrode material preparation method, special Sign is that the aqueous slkali is sodium hydroxide solution or sodium bicarbonate solution, and the concentration of the aqueous slkali is 0.5-2mol/L, institute Stating pretreatment temperature is 90-120 DEG C, pretreatment time 1-3h, and drying temperature is 80 DEG C -130 DEG C in the pretreatment, drying Time is 1-3h.
7. fiber according to claim 1/graphene/carbon quantum dot/FeOF flexible electrode material preparation method, special Sign is that the alcohol is one of ethyl alcohol, propyl alcohol, isopropanol, butanol.
8. fiber according to claim 1/graphene/carbon quantum dot/FeOF flexible electrode material preparation method, special Sign is that the heating temperature that reaction is heated in the step C is 100 DEG C -180 DEG C, reaction time 4h-20h.
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CN108766783A (en) * 2018-06-13 2018-11-06 常熟理工学院 A kind of preparation method of fiber/graphene/zinc sulphide flexible electrode material
CN109137142A (en) * 2018-07-26 2019-01-04 南京工业大学 Spot film structure carbon quantum dot-graphene fiber and preparation and application

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