CN107082419A - A kind of preparation method of flexible fiber electrode - Google Patents
A kind of preparation method of flexible fiber electrode Download PDFInfo
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- CN107082419A CN107082419A CN201710243935.6A CN201710243935A CN107082419A CN 107082419 A CN107082419 A CN 107082419A CN 201710243935 A CN201710243935 A CN 201710243935A CN 107082419 A CN107082419 A CN 107082419A
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- fiber electrode
- flexible fiber
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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Abstract
The invention discloses a kind of preparation method of flexible fiber electrode, preparation process is to prepare graphene oxide dispersion and the multi-walled carbon nanotube aqueous solution respectively, then ultrasonication is carried out after being well mixed, add anti-bad sepsis acid, place and reacted in baking oven after implantation glass pipe interior sealing, finished product.Preparation technology of the present invention is simple, and using environmentally friendly reducing agent ascorbic acid, cost is low pollution-free, environmental protection.Obtained flexible electrode has excellent mechanical flexibility, and chemical property and mechanical property are protruded, and specific capacitance is high, can be widely used for the fields such as battery, super capacitor material and environmental protection automobile.
Description
Technical field
The present invention relates to new energy materialses field, particularly a kind of preparation method of flexible fiber electrode.
Background technology
As people are to the growing of wearable portable electric appts demand, study hotspot in new energy field by
Gradually turn to the flexible energy storage device of research and development.Wherein, flexible fiber type carbon electrode material is as most important in energy storage device
Part, becomes the research emphasis of researcher.For high-performance flexible energy storage device, with superior flexible and
The exploitation of the graphene fiber electrode of electric conductivity is of great interest.
Greatly, it can be rolled into fullerene structure, be curled into CNT or be stacked into three for the plasticity of graphene
The graphite and graphite-like structure of dimension.The graphene of individual layer has fabulous electronic transmission performance and powerful mechanical performance.Graphite
Alkene is that the connection in a kind of super light material, its cellular construction between carbon atom is highly stable.Based on these excellent performances, with graphite
Electrode material based on alkene will play great potentiality.The flexible electrode material of low-temperature reduction self assembly has following excellent
Point：From the electrode material that performance is stable, security is improved；The electrode material of ultra-thin and the assembling process simplified, significantly
Volume is reduced, makes whole device smaller lighter；Electrode material consumption is few, reduces production cost.
At present, the existing many preparation methods of graphene-based fiber electrode, although equally used the method for reduction self assembly
But mostly it is to use organic reducing agent, cost high pollution is big.How a kind of technique simple, environmental protection, electrochemistry and power are prepared
The fiber electrode of function admirable is learned, as popular research topic.
The content of the invention
It is an object of the invention to provide a kind of preparation method of flexible fiber electrode, technique is simple, environmental protection, made
The mechanical property and electric property of standby fiber electrode are protruded, and specific capacitance is high.
To reach above-mentioned purpose, the preparation method of flexible fiber electrode of the invention, step is as follows：
1）Graphene oxide is prepared using Hummers methods, the progress that adds water disperses to obtain graphene oxide dispersion；
2）Multi-walled carbon nanotube is modified processing, the dispersed multi-walled carbon nanotube aqueous solution is obtained；
3）Graphene oxide dispersion and the multi-walled carbon nanotube aqueous solution are uniformly mixed, ultrasonication is then carried out, obtains mixed
Close solution；
4）Ascorbic acid is added in mixed solution, after stirring, with needle tubing implantation glass pipe, two ends are close with rubber stopper
Envelope；
5）Glass tube is placed in baking oven, reacted 1 hour at 40 DEG C, glass tube is taken out and gets product.
Further, step 1）Described in graphene oxide dispersion concentration be 1~2 mg/mL.
Further, step 2）Described in the multi-walled carbon nanotube aqueous solution concentration be 1~2 mg/mL.
Further, step 3）Described in the concentration ratio of graphene oxide dispersion and the multi-walled carbon nanotube aqueous solution be 1:
1, the concentration of mixed solution is 1~2 mg/mL.
Further, step 4）The mass ratio of middle ascorbic acid and graphene oxide is 1:5.
Further, step 2）, step 3）Dispersion liquid for disperseing graphene oxide and multi-walled carbon nanotube is water.
Further, step 3）Ultrasonication is carried out using ultrasonic cell disruptor, frequency is 500W.
Further, step 4）Described in glass tube be glass tube that internal diameter is 5 mm, rubber stopper is and glass tube coordinates
Pipe cap.
Especially, using the flexible fiber electrode obtained by above-mentioned preparation method.
The substantive distinguishing features of the present invention and progress are：
Beneficial effects of the present invention are：（1）Preparation technology is simple, and preparation time is short, the only water, and using as dispersion liquid
Environmentally friendly reducing agent ascorbic acid, effectively reduces cost and pollution-free, environmental protection.
（2）Multi-walled carbon nanotube is doped with graphene fiber, the mechanical property and electricity of graphene fiber is enhanced
Performance, improves specific capacitance.Obtained flexible fiber electrode not only has high electroactive material loading capacity, while having excellent
Different mechanical flexibility.
（3）Obtained flexible fiber electrode possesses three-dimensional conductive network, and this structure can accelerate electrolyte ion
Diffusion, is effectively facilitated electrochemical reaction, critical effect is played in the lifting to its chemical property.
Flexible fiber electrode prepared by the present invention can be widely used for battery, super capacitor material and environmental protection automobile etc.
Field.
Brief description of the drawings
Fig. 1 is the profile scanning sem image of flexible fiber electrode prepared by the embodiment of the present invention 2.
Fig. 2 is the reaction unit schematic diagram of flexible fiber electrode prepared by the embodiment of the present invention 1.
Fig. 3 is flexible fiber electrode stress strain curve prepared by the embodiment of the present invention 1.
Fig. 4 is flexible fiber electrode cycle volt-ampere curve prepared by the embodiment of the present invention 2.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, below technical scheme in the present invention carry out it is clear
Chu, it is fully described by, it is clear that described embodiment is a part of embodiment of the invention, rather than whole embodiments.
Embodiment 1：
1g graphite powders and 2g sodium nitrate are put into round-bottomed flask ice bath, mechanical agitation is carried out and concentrated sulfuric acid 46ml is slowly added dropwise simultaneously,
Keep ice bath below 10 DEG C, react 1 hour.Be subsequently added 6g potassium permanganate react 4 hours, by temperature be adjusted to 35 DEG C after
Continuous reaction 20 hours.20ml 30% hydrogen peroxide is subsequently added, continues to stir 30 minutes, adds 200ml deionized waters.Centrifugation is washed
Wash and obtain graphene oxide, be dispersed in water, obtain graphene oxide dispersion.
By advance 500 DEG C of the progress high temperature purification treatment 1 hour of 1g CNTs, 23mL concentrated sulfuric acid stirring at normal temperature is then added
20 hours, 350mg sodium nitrate and 1g potassium permanganate are subsequently added, 10mL30% dioxygen is added after being stirred 2 hours at 40 DEG C
Water, centrifuge washing obtains the CNT of oxidation modification, is dispersed in water, obtains the multi-walled carbon nanotube aqueous solution.
Graphene oxide dispersion and many wall modified carbon nano-tube aqueous solution are pressed into concentration ratio 1:1 is dispersed in water,
The dispersion liquid that concentration is 2mg/mL is formed, uniform mixed solution is formed it into through ultrasound and magnetic agitation.In mixed solution
Ascorbic acid 0.2g is added, using syringe is by solution implantation glass pipe and is stoppered rubber stopper after stirring, in 40 DEG C of baking ovens
Middle reaction 1 hour, stands be dried as shown in Figure 2, obtain flexible fiber electrode.
The present embodiment, which obtains fiber electrode, has good pliability.Shown in Fig. 3, the flexible fiber obtained to the present embodiment
Electrode carries out tensile strength testing, and its tensile property is very excellent, and largest deformation is up to 150%.
Embodiment 2：
1g graphite powders and 2g sodium nitrate are put into round-bottomed flask ice bath, mechanical agitation is carried out and concentrated sulfuric acid 46ml is slowly added dropwise simultaneously,
Keep ice bath below 10 DEG C, react 1 hour.Be subsequently added 6g potassium permanganate react 4 hours, by temperature be adjusted to 35 DEG C after
Continuous reaction 20 hours.20ml 30% hydrogen peroxide is subsequently added, continues to stir 30 minutes, adds 200ml deionized waters.Centrifugation is washed
Wash and obtain graphene oxide, be dispersed in water, obtain graphene oxide dispersion.
By advance 500 DEG C of the progress high temperature purification treatment 1 hour of 1g CNTs, 23mL concentrated sulfuric acid stirring at normal temperature is then added
20 hours, 350mg sodium nitrate and 1g potassium permanganate are subsequently added, the double of 10mL 30% are added after being stirred 2 hours at 40 DEG C
Oxygen water, centrifuge washing obtains the CNT of oxidation modification, is dispersed in water, obtains the multi-walled carbon nanotube aqueous solution.
Graphene oxide dispersion and many wall modified carbon nano-tube aqueous solution are pressed into concentration ratio 1:1 is dispersed in water,
The dispersion liquid that concentration is 1mg/mL is formed, uniform mixed solution is formed it into through ultrasound and magnetic agitation.In mixed solution
Ascorbic acid 0.2g is added, using syringe is by solution implantation glass pipe and is stoppered rubber stopper after stirring, in 40 DEG C of baking ovens
Middle reaction 1 hour, stands be dried as shown in Figure 2, obtain flexible fiber electrode.
The present embodiment, which obtains fiber electrode, has good chemical property.As shown in figure 1, CNT is propped up as conduction
Frame so that fiber electrode has three-dimensional conductive network structure, is so conducive to the migration of electrolyte ion, promotes electrochemistry anti-
The generation answered.As shown in figure 4, carrying out the curve that electro-chemical test is obtained to it with cyclic voltammetry, good electrification is shown
Learn performance.
Claims (9)
1. a kind of preparation method of flexible fiber electrode, it is characterised in that step is as follows：
1）Graphene oxide is prepared using Hummers methods, the progress that adds water disperses to obtain graphene oxide dispersion；
2）Multi-walled carbon nanotube is modified processing, the dispersed multi-walled carbon nanotube aqueous solution is obtained；
3）Graphene oxide dispersion and the multi-walled carbon nanotube aqueous solution are uniformly mixed, ultrasonication is then carried out, obtains mixed
Close solution；
4）Ascorbic acid is added in mixed solution, after stirring, with needle tubing implantation glass pipe, two ends are close with rubber stopper
Envelope；
5）Glass tube is placed in baking oven, reacted 1 hour at 40 DEG C, glass tube is taken out and gets product.
2. the preparation method of flexible fiber electrode according to claim 1, it is characterised in that：Step 1）Described in aoxidize stone
The concentration of black alkene dispersion liquid is 1~2 mg/mL.
3. the preparation method of flexible fiber electrode according to claim 1, it is characterised in that：Step 2）Described in many wall carbon
The concentration of the nanotube aqueous solution is 1~2 mg/mL.
4. the preparation method of flexible fiber electrode according to claim 1, it is characterised in that：Step 3）Described in aoxidize stone
The concentration ratio of black alkene dispersion liquid and the multi-walled carbon nanotube aqueous solution is 1:1, the concentration of mixed solution is 1~2 mg/mL.
5. the preparation method of flexible fiber electrode according to claim 1, it is characterised in that：Step 4）Middle ascorbic acid with
The mass ratio of graphene oxide is 1:5.
6. the preparation method of flexible fiber electrode according to claim 1, it is characterised in that：Step 2）, step 3）For
The dispersion liquid of scattered graphene oxide and multi-walled carbon nanotube is water.
7. the preparation method of flexible fiber electrode according to claim 1, it is characterised in that：Step 3）It is thin using ultrasonic wave
Born of the same parents' pulverizer carries out ultrasonication, and frequency is 500W.
8. the preparation method of flexible fiber electrode according to claim 1, it is characterised in that：Step 4）Described in glass tube
For the glass tube that internal diameter is 5 mm, rubber stopper is the pipe cap coordinated with glass tube.
9. the flexible fiber electrode obtained by preparation method in a kind of 1-8 such as claim as described in any one.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111517312A (en) * | 2020-05-13 | 2020-08-11 | 三明学院 | Injection synthesis method of large-size graphene RGO sheet |
| CN114242464A (en) * | 2021-12-30 | 2022-03-25 | 江苏蒙正医疗科技有限公司 | Preparation method and application of graphene composite fiber electrode |
| CN115074865A (en) * | 2022-07-29 | 2022-09-20 | 青岛理工大学 | Graphene fiber preparation method, graphene fiber temperature sensor and application |
| CN115626633A (en) * | 2022-10-13 | 2023-01-20 | 佛山科学技术学院 | Purification method of single-walled carbon nanotube |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966699A (en) * | 2014-01-14 | 2014-08-06 | 中国科学院上海应用物理研究所 | Preparation method of graphene fibers |
| CN104036971A (en) * | 2014-05-29 | 2014-09-10 | 浙江大学 | Preparation method for graphene/carbon nano-tube composite fibre-based super capacitor |
| CN105590757A (en) * | 2014-11-18 | 2016-05-18 | 中国科学院宁波材料技术与工程研究所 | Carbon nanotube/graphene composite gel and preparation method thereof |
-
2017
- 2017-04-14 CN CN201710243935.6A patent/CN107082419A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103966699A (en) * | 2014-01-14 | 2014-08-06 | 中国科学院上海应用物理研究所 | Preparation method of graphene fibers |
| CN104036971A (en) * | 2014-05-29 | 2014-09-10 | 浙江大学 | Preparation method for graphene/carbon nano-tube composite fibre-based super capacitor |
| CN105590757A (en) * | 2014-11-18 | 2016-05-18 | 中国科学院宁波材料技术与工程研究所 | Carbon nanotube/graphene composite gel and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111517312A (en) * | 2020-05-13 | 2020-08-11 | 三明学院 | Injection synthesis method of large-size graphene RGO sheet |
| CN114242464A (en) * | 2021-12-30 | 2022-03-25 | 江苏蒙正医疗科技有限公司 | Preparation method and application of graphene composite fiber electrode |
| CN115074865A (en) * | 2022-07-29 | 2022-09-20 | 青岛理工大学 | Graphene fiber preparation method, graphene fiber temperature sensor and application |
| CN115626633A (en) * | 2022-10-13 | 2023-01-20 | 佛山科学技术学院 | Purification method of single-walled carbon nanotube |
| CN115626633B (en) * | 2022-10-13 | 2024-02-02 | 佛山科学技术学院 | Purification method of single-walled carbon nanotube |
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Application publication date: 20170822 |