CN106971860A - A kind of MnO2The preparation method of@graphene fiber super capacitor electrode materials - Google Patents
A kind of MnO2The preparation method of@graphene fiber super capacitor electrode materials Download PDFInfo
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- CN106971860A CN106971860A CN201710271591.XA CN201710271591A CN106971860A CN 106971860 A CN106971860 A CN 106971860A CN 201710271591 A CN201710271591 A CN 201710271591A CN 106971860 A CN106971860 A CN 106971860A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of MnO2The preparation method of@graphene fiber super capacitor electrode materials, the preparation method is to include redox graphene, obtains graphene fiber；And on the surface of graphene fiber, pass through hydro-thermal method cladding growth MnO2The steps such as nano wire.Obtained MnO2The micro-structural of@graphene fiber super capacitor electrode materials is MnO2Nano wire coated graphite alkene fiber, and MnO2Nano wire is interlaced to form the space pore space structure largely connected, with very big specific surface area, effectively raises the specific surface area and space availability ratio of electrode, improves specific capacitance, high rate performance and the electrochemical stability of electrode material.MnO produced by the present invention2@graphene fiber super capacitors electrode material is in three-electrode system test, and specific capacitance value reaches 64.4~105.3 F g‑1.And preparation method has simple, low cost and other advantages.
Description
Technical field
The present invention relates to ultracapacitor field, more particularly to a kind of electrode material for super capacitor and preparation method thereof.
Background technology
With the increasingly increase of the fast development, the continuous consumption of fossil energy, environmental pollution of global economy, research is a kind of
Efficiently, inexpensive, environmentally friendly, high performance energy conversion and storage system have seemed more and more important.Super capacitor
Device is wide with its high-duty density, temperature in use scope, long lifespan, it is friendly to environment the advantages of and receive much concern, in solar charging
Have in terms of the Aero-Space such as electrical equipment, the stand-by power supply of microcomputer, the igniter of aircraft and science and techniques of defence of crucial importance and wide
Wealthy application prospect, it has also become the study hotspot of countries in the world.
Ultracapacitor is a kind of electrochemical capacitor, and two classes can be divided into according to electric charge Ultrahigh：One class electrochemistry
Double layer capacitor, the electrode material of such capacitor is mainly carbon material；Another kind of is Faraday pseudo-capacitance device, such electric capacity
The electrode material of device is mainly transition-metal oxide.Current field personnel study having for electrode material for super capacitor
Carbon fiber, CNT（CNT, Carbon Nanotubes）, graphene, MnO2Deng oxide and CoSxDeng chalcogenide electricity
Pole material.Because graphene possesses excellent thermal conductivity, electric conductivity, mechanical property etc., it is in ultracapacitor, sensing
The fields such as device, electro-catalysis, polymer nanocomposites, photoelectric functional material, high-performance portable power supply, drug controlled release
Show potential application prospect.Fullerene and CNT also possess many excellent properties, but its cost is higher.And graphite
The raw material of alkene are readily obtained, and cheap, and preparation method is simple, therefore are considered to have the green wood extensively using value
Material, it is also more and more to its application study in the last few years.Graphene fiber is a kind of new graphite prepared in recent years
Alkene macroscopic material, its high conductivity, intensity and the flexible characteristic that can be woven receive the concern of researcher.But pure graphene is fine
The usual specific capacitance value of dimension material is relatively low, and capacitor element has low energy densities, so as to limit its extensive potential application.Will be counterfeit
It is considered as to improve the effective means of electrode capacitance that capacitance material, which introduces graphene fiber to form composite,.
The content of the invention
For the problems of the prior art, the present invention plans fake capacitance material and introduces graphene fiber to form composite
Come improve graphene fiber as electrode material specific capacitance is low, low energy densities the problem of.
To realize goal of the invention, the present invention is as follows using technical scheme：
The invention provides a kind of MnO2The preparation method of@graphene fiber super capacitor electrode materials, including step are as follows：
（1）By graphene oxide aqueous dispersions centrifugal concentrating, then ultrasonically treated, acquisition graphene oxide spinning solution；
（2）Graphene oxide spinning solution is expelled to by CaCl using syringe pump2In the coagulating bath of/ethanol solution composition, solidifying
Gu dipping is after 20 ~ 30 minutes in bath, by obtained fiber deionized water and ethanol repeated washing, the solidification for washing away residual is molten
Liquid, obtains graphene oxide fiber and simultaneously collects on support, will collect obtained fiber high temperature drying under vacuum；
（3）Graphene oxide fiber is reduced 8 ~ 12 hours at 90 ~ 120 DEG C in hydroiodic acid, then in H2/ Ar reproducibility gas
The lower 1000 DEG C of thermal reductions of atmosphere, naturally cool to and fiber are taken out after room temperature, prepare graphene fiber；
（4）Manganese sulfate, potassium permanganate and water are mixed, stirring obtains precursor solution, wherein manganese sulfate, potassium permanganate, water
Ratio is 1.3m mol：3.2m mol：10mL；
（5）Graphene fiber suspension is placed in reactor, precursor solution is added, hydro-thermal reaction is carried out, reaction temperature is 140
~ 180 DEG C, the time is 12 ~ 24h, is cooled to room temperature, collects fiber, is washed, and is dried, and in 300 DEG C of annealing, produces MnO2@graphite
Alkene fibre supercapacitors electrode material.
The step（1）Middle sonication treatment time is 20 ~ 30min.
The step（2）Middle repeated washing is to use ethanol, deionized water rinsing respectively 3 ~ 5 times.
The step（3）Middle H2The volume ratio of/Ar atmosphere is 1:1~1:4.
The step（4）Middle mixing time is 20 ~ 30min.
The step（5）Middle drying time is 12 ~ 24h.
Present invention also offers pass through MnO made from above-mentioned preparation method2@graphene fiber super capacitor electrode materials
Expect, the material microstructure is：The MnO of Hydrothermal Growth2Nano wire is coated on the surface of graphene fiber, and nano wire is mutually handed over
Mistake forms the space pore space structure largely connected, and it has very big specific surface area, effectively raises the ratio surface of electrode
Product and space availability ratio, improve specific capacitance, high rate performance and the electrochemical stability of electrode material.It is produced by the present invention
MnO2@graphene fiber super capacitors electrode material is in three-electrode system test, and specific capacitance value reaches 64.4~105.3 F
g-1, with very excellent specific capacitance.
The useful achievement of the present invention is：
（1）The present invention is designed by rational material microstructure, and MnO is realized using simple to operate, inexpensive preparation method2Receive
Nanowire structure, and by Hydrothermal Growth on the surface of graphene fiber.Nano wire is interlaced to form the space largely connected
Pore space structure, is conducive to the diffusion and migration of ion, and huge specific surface area is conducive to the absorption of ion, is received so as to add this
The specific surface area and the attaching space of electrode material and electrolyte of rice structure electrode, while the high conduction performance of graphene fiber
Enough make the electric charge fast transfer on electrode, reach the effect for the specific capacitance for effectively improving electrode material.
（2）MnO prepared by the present invention2@graphene fiber super capacitor electrode materials are applied to ultracapacitor
Very excellent specific capacitance is shown in electrode test, in 1.5 A g-1Current density under show 105.3 F g-1Height
Specific capacity, shows good chemical property, in addition on the premise of height ratio capacity is ensured, also has high intensity concurrently and flexibility can
The characteristic of braiding, has huge application prospect in wearable electronic.
（3）The method that the present invention uses Hydrothermal Synthesiss, it is simple to operate, it is not necessary to complex device, it is very suitable for industrialization
Batch production.
Brief description of the drawings
Fig. 1 is MnO prepared by embodiment 22The low power ESEM of@graphene fiber super capacitor electrode materials
（SEM）Figure.
Fig. 2 is MnO prepared by embodiment 22The high power ESEM of@graphene fiber super capacitor electrode materials
（SEM）Figure.
Fig. 3 is MnO prepared by embodiment 22The cyclic voltammogram of@graphene fiber super capacitor electrode materials.
Fig. 4 is MnO prepared by embodiment 22The constant current charge-discharge curve of@graphene fiber super capacitor electrode materials
Figure.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
（1）By graphene oxide aqueous dispersions centrifugal concentrating, then ultrasonically treated 30min, so as to obtain graphene oxide spinning
Liquid；
（2）Graphene oxide spinning solution is expelled to by CaCl using syringe pump2In the coagulating bath of/ethanol solution composition, solidifying
Gu, by obtained fiber deionized water and ethanol repeated washing 3 times, the solidification solution of residual is washed away after dipping 20min in bath,
So as to obtain graphene oxide fiber and collect on support, obtained fiber high temperature drying under vacuum will be collected；
（3）Graphene oxide fiber is reduced into 12h at 90 DEG C in hydroiodic acid, then in H2/Ar（Volume ratio is 1:1）Reduction
The property lower 1000 DEG C of thermal reductions of atmosphere, naturally cool to after room temperature and take out fiber, so as to prepare graphene fiber；
（4）Manganese sulfate, potassium permanganate and water are mixed, 30min is stirred, obtains precursor solution, wherein manganese sulfate, permanganic acid
Potassium, the ratio of water are 1.3m mol：3.2m mol：10mL；
（5）Graphene fiber suspension is placed in reactor, precursor solution is added, hydro-thermal reaction is carried out, reaction temperature is 140
DEG C, the time is 24h, is cooled to room temperature, collects fiber, and washing dries 24h, and in 300 DEG C of annealing, produce MnO2@graphene cores
Shell structure fibre supercapacitors material.
Embodiment 2
（1）By graphene oxide aqueous dispersions centrifugal concentrating, then ultrasonically treated 30min, so as to obtain graphene oxide spinning
Liquid；
（2）Graphene oxide spinning solution is expelled to by CaCl using syringe pump2In the coagulating bath of/ethanol solution composition, solidifying
Gu, by obtained fiber deionized water and ethanol repeated washing 3 times, the solidification solution of residual is washed away after dipping 30min in bath,
So as to obtain graphene oxide fiber and collect on support, obtained fiber high temperature drying under vacuum will be collected；
（3）Graphene oxide fiber is reduced into 8h at 120 DEG C in hydroiodic acid, then in H2/Ar（Volume ratio is 1:4）Reduction
The property lower 1000 DEG C of thermal reductions of atmosphere, naturally cool to after room temperature and take out fiber, so as to prepare graphene fiber；
（4）Manganese sulfate, potassium permanganate and water are mixed, 30min is stirred, obtains precursor solution, wherein manganese sulfate, permanganic acid
Potassium, the ratio of water are 1.3m mol：3.2m mol：10mL；
（5）Graphene fiber suspension is placed in reactor, precursor solution is added, hydro-thermal reaction is carried out, reaction temperature is 180
DEG C, the time is 24h, is cooled to room temperature, collects fiber, and washing dries 12h, and in 300 DEG C of annealing, produce MnO2@graphene cores
Shell structure fibre supercapacitors material.
Embodiment 3
（1）By graphene oxide aqueous dispersions centrifugal concentrating, then ultrasonically treated 20min, so as to obtain graphene oxide spinning
Liquid；
（2）Graphene oxide spinning solution is expelled to by CaCl using syringe pump2In the coagulating bath of/ethanol solution composition, solidifying
Gu, by obtained fiber deionized water and ethanol repeated washing 5 times, the solidification solution of residual is washed away after dipping 30min in bath,
So as to obtain graphene oxide fiber and collect on support, obtained fiber high temperature drying under vacuum will be collected；
（3）Graphene oxide fiber is reduced into 10h at 110 DEG C in hydroiodic acid, then in H2/Ar（Volume ratio is 1:2）Also
The lower 1000 DEG C of thermal reductions of originality atmosphere, naturally cool to and fiber are taken out after room temperature, so as to prepare graphene fiber；
（4）Manganese sulfate, potassium permanganate and water are mixed, 20min is stirred, obtains precursor solution, wherein manganese sulfate, permanganic acid
Potassium, the ratio of water are 1.3m mol：3.2m mol：10mL；
（5）Graphene fiber suspension is placed in reactor, precursor solution is added, hydro-thermal reaction is carried out, reaction temperature is 180
DEG C, the time is 12h, is cooled to room temperature, collects fiber, and washing dries 24h, and in 300 DEG C of annealing, produce MnO2@graphene cores
Shell structure fibre supercapacitors material.
Chemical raw material manganese sulfate, the potassium permanganate used in above example is that analysis is pure, and deionized water resistance is
18.0~18.5M Ω.
To MnO made from each embodiment2@graphene fiber super capacitors electrode material carry out microscopic appearance observation, with
And electrochemical property test.
If Fig. 1 and Fig. 2 is respectively MnO prepared by embodiment 22The low power of@graphene fiber super capacitor electrode materials
With high power ESEM（SEM）Figure.MnO in the Surface coating of graphene fiber2Nano wire, and the interlaced formation of nano wire
The space pore space structure largely connected, it has very big specific surface area.
With MnO made from each embodiment2@graphene fibers are electrode material for super capacitor, prepare three-electrode system, enter
Row test.If Fig. 3 is MnO prepared by embodiment 22The cyclic voltammogram of@graphene fiber super capacitor electrode materials, 1
mol L-1Na2SO4Under electrolyte, electrode material obtains approximate rectangular cyclic voltammetry curve, 10 mV s-1To 100 mV s-1
Sweep speed under show good electric double layer capacitance behavior, there is no obvious farad from 0 V to 0.6 V cyclic voltammetry curves
Electric current.In 1 mol L-1Na2SO4In three-electrode system test under electrolyte, in 1.5 A g-1Current density under, respectively
Embodiment specific capacitance value reaches 64.4~105.3 F g-1Specific capacity；If Fig. 4 is MnO prepared by embodiment 22@graphenes are fine
The constant current charge-discharge curve map of electrode material for super capacitor is tieed up, 105.3 F g are shown-1Height ratio capacity.
Claims (9)
1. a kind of MnO2The preparation method of@graphene fiber super capacitor electrode materials, it is characterised in that the preparation method
For：On the surface of graphene fiber, pass through hydro-thermal method method cladding growth MnO2Nano wire.
2. a kind of MnO according to claim 12The preparation method of@graphene fiber super capacitor electrode materials, it is special
Levy and be to include：
1）By graphene oxide aqueous dispersions centrifugal concentrating, then ultrasonically treated, acquisition graphene oxide spinning solution；
2）Graphene oxide spinning solution is expelled to by CaCl2/ ethanol solution composition coagulating bath in, in coagulating bath impregnate 20 ~
After 30 minutes, by obtained fiber deionized water and ethanol repeated washing, the solidification solution of residual is washed away, so as to be aoxidized
Graphene fiber is simultaneously collected on support, will collect obtained fiber high temperature drying under vacuum；
3）Graphene oxide fiber is reduced 8 ~ 12 hours at 90 ~ 120 DEG C in hydroiodic acid, then in H2/ Ar reducing atmosphere
Lower 1000 DEG C of thermal reductions, naturally cool to and fiber are taken out after room temperature, and graphene fiber is made；
4）Manganese sulfate, potassium permanganate and water are mixed, stirring obtains precursor solution, wherein manganese sulfate, potassium permanganate, water
Ratio is 1.3m mol：3.2m mol：10mL；
5）By graphene fiber suspension be placed in reactor, add precursor solution, carry out hydro-thermal reaction, reaction temperature be 140 ~
180 DEG C, the time is 12 ~ 24h, is cooled to room temperature, collects fiber, is washed, and is dried, and in 300 DEG C of annealing, produces the MnO2@
Graphene fiber super capacitor electrode material.
3. a kind of MnO according to claim 22The preparation method of@graphene fiber super capacitor electrode materials, it is special
Levy and be：The step 1）Middle sonication treatment time is 20 ~ 30min.
4. according to a kind of MnO of claim 22The preparation method of@graphene fiber super capacitor electrode materials, it is characterised in that：
The step 2）Middle repeated washing is to use ethanol, deionized water rinsing respectively 3 ~ 5 times.
5. according to a kind of MnO of claim 22The preparation method of@graphene fiber super capacitor electrode materials, it is characterised in that：
The step 3）Middle H2The volume ratio of/Ar atmosphere is 1:1~1:4.
6. according to a kind of MnO of claim 22The preparation method of@graphene fiber super capacitor electrode materials, it is characterised in that：
The step 4）Middle mixing time is 20 ~ 30min.
7. according to a kind of MnO of claim 22The preparation method of@graphene fiber super capacitor electrode materials, it is characterised in that：
The step 5）Middle drying time is 12 ~ 24h.
8. a kind of MnO according to made from any one of claim 1 to 7 preparation method2@graphene fiber super capacitors electricity
Pole material, it is characterised in that：The micro-structural of the material is MnO2Nano wire coated graphite alkene fiber, and MnO2Nano wire is mutual
It is staggered to form the space pore space structure largely connected.
9. a kind of MnO according to claim 82@graphene fiber super capacitor electrode materials, it is characterised in that：
The material is in ultracapacitor three-electrode system, and specific capacitance value reaches 64.4~105.3 F g-1。
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107754786A (en) * | 2017-10-16 | 2018-03-06 | 广西大学 | One kind utilizes KMnO4The method that electrocatalytic oxidation is improved on direct oxidation graphite paper |
| CN108642884A (en) * | 2018-05-18 | 2018-10-12 | 江南大学 | The preparation method and its resulting materials of a kind of painted graphite alkene fiber and application |
| CN109888225A (en) * | 2019-02-27 | 2019-06-14 | 桑顿新能源科技有限公司 | Positive electrode and preparation method thereof and lithium ion battery |
| CN110931270A (en) * | 2019-12-13 | 2020-03-27 | 电子科技大学 | Preparation method of graphene-based electrode fiber containing substrate |
| CN111540613A (en) * | 2020-05-09 | 2020-08-14 | 贵州梅岭电源有限公司 | Lithium ion capacitor based on 3D graphene @ MnO and preparation method thereof |
| CN112349909A (en) * | 2020-11-06 | 2021-02-09 | 常州大学 | Zinc-ion battery positive electrode composite material and preparation method and application thereof |
| CN115305706A (en) * | 2022-07-25 | 2022-11-08 | 南通大学 | MnO 2 Modified graphene nanocomposite material and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107754786A (en) * | 2017-10-16 | 2018-03-06 | 广西大学 | One kind utilizes KMnO4The method that electrocatalytic oxidation is improved on direct oxidation graphite paper |
| CN107754786B (en) * | 2017-10-16 | 2020-06-16 | 广西大学 | By using KMnO4Method for improving electrocatalytic oxidation on direct oxidized graphite paper |
| CN108642884A (en) * | 2018-05-18 | 2018-10-12 | 江南大学 | The preparation method and its resulting materials of a kind of painted graphite alkene fiber and application |
| CN109888225A (en) * | 2019-02-27 | 2019-06-14 | 桑顿新能源科技有限公司 | Positive electrode and preparation method thereof and lithium ion battery |
| CN110931270A (en) * | 2019-12-13 | 2020-03-27 | 电子科技大学 | Preparation method of graphene-based electrode fiber containing substrate |
| CN111540613A (en) * | 2020-05-09 | 2020-08-14 | 贵州梅岭电源有限公司 | Lithium ion capacitor based on 3D graphene @ MnO and preparation method thereof |
| CN112349909A (en) * | 2020-11-06 | 2021-02-09 | 常州大学 | Zinc-ion battery positive electrode composite material and preparation method and application thereof |
| CN115305706A (en) * | 2022-07-25 | 2022-11-08 | 南通大学 | MnO 2 Modified graphene nanocomposite material and preparation method and application thereof |
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