CN105206429B - A kind of fexible film electrode material and preparation method thereof - Google Patents
A kind of fexible film electrode material and preparation method thereof Download PDFInfo
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- CN105206429B CN105206429B CN201510713190.6A CN201510713190A CN105206429B CN 105206429 B CN105206429 B CN 105206429B CN 201510713190 A CN201510713190 A CN 201510713190A CN 105206429 B CN105206429 B CN 105206429B
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- 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 present invention relates to a kind of fexible film electrode materials and preparation method thereof, the electrode material is using ultra-thin titanium sheet as substrate, the vanadium trioxide nano-chip arrays of one layer of dense arrangement are distributed in substrate, one layer of carbon material is also wrapped on vanadium trioxide nano-chip arrays surface.Preparation method generates vanadium dioxide nano chip arrays in ultra-thin titanium on piece hydro-thermal first；Then carbon coating is carried out by carbon source of glucose, forms vanadium trioxide@carbon composite nano chip arrays, i.e. fexible film electrode material.It regard the electrode material as positive and negative electrode simultaneously, is assembled into ultracapacitor.The method is easy to operate, is easy to scale; the capacitor of acquisition has good flexibility; and entire only 40 microns of capacitor thickness; it is high to show asymmetric energy storage mechnism, voltage height, volume energy density; it can be used for the fields such as flexible wearable electronic product, be expected to generate good social and economic benefit.
Description
Technical field
The invention belongs to capacitor technology field, it is related to a kind of fexible film electrode material and preparation method thereof.
Background technology
With the continuous development of flexible electronic product, flexible energy storage device also comes into being, and wherein flexible thin film type is super
Capacitor is because the advantages such as its high power, quick charge capability show huge application prospect, such as in flexible display apparatus, flexibility
Electronic skin and wearable electronic etc. have potential application.Traditional flexible super capacitor usually has two classes：One
It is that electrode is used as using carbon-based material (such as carbon nanotube or graphene self-supported membrane), although having excellent flexibility and conduction
Property, but carbon material is the energy storage mechnism based on electric double layer, the fake capacitance material capacity relative to redox reaction mechanism is small；Two
It is directly to grow fake capacitance active material as electrode using on flexible carbon cloth, but carbon cloth collector is thicker and there are microns up to a hundred
Structural void, greatly waste many spatial volumes.Therefore traditional flexible film super capacitor volume energy density
It is relatively low with power density.
Invention content
The technical problem to be solved by the present invention is to aiming at the above shortcomings existing in the prior art, provide it is a kind of it is ultra-thin,
The fine and close fake capacitance electrode material and preparation method thereof with high power capacity, which is specially carbon in ultra-thin titanium piece substrate
The vanadium trioxide nano-chip arrays material of cladding builds asymmetric energy storage machine as positive and negative electrode simultaneously using the electrode material
The ultracapacitor volume energy density and power density of reason are high.
In order to solve the above technical problems, technical solution provided by the invention is：
A kind of fexible film electrode material is provided, the electrode material is distributed with using ultra-thin titanium sheet as substrate in substrate
The vanadium trioxide nano-chip arrays of one layer of dense arrangement are also wrapped on one layer of carbon material on vanadium trioxide nanometer sheet surface.
By said program, the ultra-thin titanium sheet thickness is 10-50 μm.
By said program, the vanadium trioxide nanometer sheet thickness is 30-40nm, vanadium trioxide nano-chip arrays thickness
Degree is 400-600nm, and the carbon material thickness is 5-10nm.
A kind of preparation method of fexible film electrode material is provided, steps are as follows：
1) vanadic anhydride, two oxalic acid hydrates are added to the in the mixed solvent of acetone and water, blue solution is obtained by the reaction；
2) blue solution and ultra-thin titanium sheet obtained by step 1) are placed in hydrothermal reaction kettle, ultra-thin titanium sheet is hidden on one side
Gear, in 160-200 DEG C of hydro-thermal reaction 12-18 hour, in titanium plate surface generation vanadium dioxide nano piece battle array after hydro-thermal reaction
Row after titanium sheet is taken out washing and drying, are having vanadium dioxide nano chip arrays one side that glucose solution is added dropwise, are drying, in repetition
It states and glucose solution and drying course is added dropwise, be subsequently placed in quartz tube furnace and made annealing treatment, obtained in titanium sheet substrate
Carbon-coated vanadium trioxide nano-chip arrays material, i.e. fexible film electrode material.
By said program, the step 1) vanadic anhydride and two oxalic acid hydrate molar ratios are 1:3；The acetone and water
Mixed solvent is acetone and water 1-4 by volume:3-6 is mixed to get.
By said program, the step 1) reaction condition is to be stirred for 24 hours under 40 DEG C of water bath conditions.
By said program, the step 2) glucose concentration is 0.11-0.44mol/L.
By said program, the technique of the step 2) annealing is：Under argon gas atmosphere 550 are warming up to 10 DEG C/min
DEG C, 1 hour is kept the temperature, then with stove natural cooling.
The present invention also provides using above-mentioned fexible film electrode material as all solid state asymmetric fexible film of positive and negative electrode
Ultracapacitor.
By said program, all solid state asymmetric flexible film super capacitor is with lithium chloride/polyvinyl alcohol gel
As quasi-solid electrolyte.
By said program, the preparation method of the lithium chloride/polyvinyl alcohol gel is：The lithium chloride for first preparing 5mol/L is molten
Then pva powder is added in liquid, the quality of pva powder and the volume ratio of lithium chloride solution are 0.1g/mL, in 85
DEG C stirring in water bath 2-3 hours stands cooling and obtains.
The beneficial effects of the present invention are：1, the present invention directly grows metal oxidation using ultra-thin titanium sheet (10 μm) as substrate
Object nano-chip arrays (vanadium oxide nano-chip arrays) establish the direct channel of electron-transport, while ultra-thin titanium sheet has very well
Flexibility, and the carbon-base film electrode thick relative to up to a hundred microns greatly reduces the overall volume of capacitor, avoids hole
Gap space waste, to improve the volume energy density of capacitor；2, one layer of carbon-coating is coated on vanadium oxide nano-chip arrays,
Vanadium oxide nano-chip arrays electrode material electric conductivity enhancing after carbon coating, and carbon-coating reduces metal oxide as protective layer
Unstability in the electrolyte, prepared electrode material surface have very high specific surface area, enable electrolyte and electricity
Pole material comes into full contact with, and greatly shortens ion diffusion path, has compared to typical electrode materials (metal oxide powder)
Better high rate performance；3, ultracapacitor (about 40 μm of thickness) is prepared by positive and negative electrode of fexible film electrode material, just,
Negative electrode material is identical, but different redox reactions occurs and forms asymmetric high-efficiency energy-storage mechanism, facilitates
Capacitor manufactures, meanwhile, the metal oxide of nanoscale can be reacted by fake capacitance provides higher charge storage, and
Traditional double electric layers supercapacitor compares the specific capacity that can provide bigger, in addition quasi- solid-state lithium chloride/polyvinyl alcohol (LiCl/
PVA) gel electrolyte further suppresses caving in for metal oxide structures, enhances the stability of electrode, improves capacitance
The cycle performance of device, and the problem of liquid electrolyte is revealed is avoided, improve the actual use value of capacitor.
Description of the drawings
Fig. 1 is the optical photograph and scanning electron microscope diagram of ultra-thin titanium sheet used in the embodiment of the present invention 1, and wherein a is light
Photo is learned, b is scanning electron microscope diagram；
Fig. 2 be embodiment 1 prepared by ultra-thin titanium piece substrate on carbon-coated vanadium trioxide nano-chip arrays scanning
Electron microscope picture；
Fig. 3 be embodiment 1 prepared by ultra-thin titanium piece substrate on carbon-coated vanadium trioxide nanometer sheet transmitted electron
Microscope figure；
Fig. 4 is vanadium dioxide nano chip arrays (b), carbon packet on ultra-thin titanium sheet (a), ultra-thin titanium piece substrate described in embodiment 1
The X-ray diffractogram of the vanadium trioxide nano-chip arrays (c) covered；
Fig. 5 is vanadium dioxide nano chip arrays (a) in ultra-thin titanium piece substrate described in embodiment 1, carbon-coated three oxidation two
The Raman spectrogram of vanadium nano-chip arrays (b)；
Fig. 6 is the photo of fexible film electrode material prepared by embodiment 1；
Fig. 7 is three of carbon-coated vanadium trioxide nano-chip arrays assembling in the ultra-thin titanium piece substrate of the preparation of embodiment 1
The positive and negative electrode cyclic voltammogram of electrode；
Fig. 8 is that carbon-coated vanadium trioxide nano-chip arrays are used as anode in the ultra-thin titanium piece substrate of the preparation of embodiment 1
Constant current charge-discharge diagram；
Carbon-coated vanadium trioxide nano-chip arrays are as cathode in the ultra-thin titanium piece substrate that Fig. 9 is prepared for embodiment 1
Constant current charge-discharge diagram；
Figure 10 be in ultra-thin titanium piece substrate prepared by embodiment 1 carbon-coated vanadium trioxide nano-chip arrays as just,
The electricity matching figure of negative electrode；
Figure 11 is identical positive and negative electrode (carbon-coated vanadium trioxide nanometer in ultra-thin titanium piece substrate prepared by embodiment 2
Chip arrays) composition solid flexible asymmetric type supercapacitor cross section scanning electron microscope diagram；
Figure 12 is the cyclic voltammetry curve figure of solid flexible asymmetric type supercapacitor prepared by embodiment 2；
Figure 13 is that constant current of the solid flexible asymmetric type supercapacitor of the preparation of embodiment 2 under different current densities is filled
Discharge curve；
Figure 14 is multiplying power of the solid flexible asymmetric type supercapacitor of the preparation of embodiment 2 under different scanning rates
Performance map；
Figure 15 is the power density-energy density figure of solid flexible asymmetric type supercapacitor prepared by embodiment 2；
Figure 16 is that solid flexible asymmetric type supercapacitor prepared by embodiment 2 lights LED material objects in the bent state
Photo.
Specific implementation mode
To make those skilled in the art more fully understand technical scheme of the present invention, below in conjunction with the accompanying drawings to the present invention make into
One step is described in detail.
Embodiment 1
Fexible film electrode material is prepared, is as follows：
1) by 0.2g vanadic anhydrides (V2O5) and 0.45 gram of two oxalic acid hydrate (H2C2O4·2H2O 10 milliliters of acetone) are added
(CH3COCH3) and the mixed solution of 25 milliliters of water in, with water-bath magnetic stirring apparatus in 40 DEG C stirring for 24 hours, obtain uniformly blue it is molten
Liquid；
2) by the 10 microns of ultra-thin titanium sheet successively supersound washing in hydrochloric acid and deionized water, drying, use on one side thick titanium sheet into
Row blocks, and is then placed in the hydrothermal reaction kettle of polytetrafluoroethylliner liner substrate with together with the above-mentioned solution being stirred, in 180 DEG C
18 hours of hydro-thermal reaction generate vanadium dioxide nano chip arrays, then by the titanium sheet with nano-chip arrays in titanium plate surface
It takes out, after drying is washed with deionized, has vanadium dioxide nano chip arrays one side that (0.165mol/L) grape is added dropwise in titanium sheet
Sugar juice, drying, repeats above-mentioned dropwise addition glucose solution and drying course is primary, is subsequently placed in quartz tube furnace and anneals
Processing is warming up to 550 DEG C with 10 DEG C/min under an argon atmosphere, 1 hour is kept the temperature, then with stove natural cooling in ultra-thin titanium chip base
Carbon-coated vanadium trioxide nano-chip arrays material, i.e. fexible film electrode material are obtained on bottom.
Fig. 1 is the optical photograph and scanning electron microscope diagram of ultra-thin titanium sheet used in the present embodiment, ultra-thin as can be seen from Figure
Titanium sheet thickness is 10 μm, and flexible good.
Fexible film electrode material obtained by the present embodiment is tested, Fig. 2 is carbon-coated three in ultra-thin titanium piece substrate
The scanning electron microscope diagram of V 2 O nano-chip arrays, as seen from the figure, carbon-coated vanadium trioxide nanometer sheet thickness is
30-40nm, it is 400-600nm to be formed by vanadium trioxide nano-chip arrays thickness, and vanadium trioxide nanometer sheet is interlaced,
It is intensive, be evenly distributed in titanium sheet substrate.Fig. 3 is the transmission of carbon-coated vanadium trioxide nanometer sheet in ultra-thin titanium piece substrate
Electron microscope picture, as can be seen from the figure the thickness of nanometer sheet carbon layer on surface is 5-10nm.
Fig. 4 is vanadium dioxide nano chip arrays (b), carbon packet on ultra-thin titanium sheet (a), ultra-thin titanium piece substrate described in the present embodiment
The X-ray diffractogram of the vanadium trioxide nano-chip arrays (c) covered, as seen from the figure, the main peak position of nano-chip arrays and titanium dioxide
Vanadium is identical, but 69 ° of peaks for a faint titanium dioxide nearby occur, derived from titanium sheet by slight oxygen in hydrothermal reaction process
Change, main peak position is identical with vanadium trioxide after annealing, this is because carbon at high temperature goes back vanadium dioxide in situ
Originally it was vanadium trioxide.Fig. 5 is vanadium dioxide nano chip arrays (a) in ultra-thin titanium piece substrate described in the present embodiment, carbon-coated
The Raman spectrogram of vanadium trioxide nano-chip arrays (b), after can be seen that annealing in figure, hence it is evident that there is the peaks D of carbon and the peaks G,
Illustrate that vanadium trioxide nanometer sheet surface layer has coated the graphited carbon of a layer segment.Fig. 6 is carbon in the ultra-thin titanium piece substrate prepared
The photo of the vanadium trioxide nano-chip arrays material of cladding, it can be seen that it is flexible good.Fig. 7 is with above-mentioned ultra-thin titanium piece substrate
Upper carbon-coated vanadium trioxide nano-chip arrays material makees working electrode, and platinum electrode is made to electrode, and saturated calomel electrode work is joined
Positive and negative electrode cyclic voltammetry curve figure than three electrodes of electrode assembling (presses arrow direction, sweep speed distinguishes 10mV/
S, 25mV/s, 50mV/s and 100mV/s), as can be seen from Figure：Carbon-coated vanadium trioxide nano-array in ultra-thin titanium piece substrate
Electrode makees cathode, and a pair of apparent oxidation reaction peak is shown in -1.0-0.1V potentials section, and makees anode in 0.1-1.0V electricity
Gesture section shows the cyclic voltammetry curve of more rectangle, illustrates to assemble using the array material while as positive and negative electrode material
The capacitor arrived is asymmetric capacitor.Fig. 8 and Fig. 9 is close in different electric currents when being respectively using the electrode material as positive and negative electrode
Constant current charge-discharge curve graph under degree, image approximate isosceles triangle, charging and discharging curve is symmetrical, and it is special to show good capacitance
Sign, is respectively 1,2,4 and 8mA/cm in current density2Under the conditions of constant current charge-discharge when, positive discharge electricity is respectively
176.6,164.2,136.4 and 101.6mC/cm2, capacity retention ratio (is respectively 1mA/cm with current density2When capacitance
Compared to) 100%, 93.0%, 77.2% and 57.5%.Negative discharge electricity is respectively 189.1,155.4,129.2 and
108.8mC/cm2When, capacity retention rate (is respectively 1mA/cm with current density2When capacitance compare) 100%, 82.2%,
68.3% and 57.5%.Figure 10 is carbon-coated vanadium trioxide nano-array electricity in ultra-thin titanium piece substrate manufactured in the present embodiment
Pole is matched as the electricity of supercapacitor positive electrode and cathode schemes, it can be seen that it is with preferable electricity matching degree and good times
Rate performance.
Embodiment 2
All solid state asymmetric flexible film super capacitor is prepared, is as follows：
Carbon-coated vanadium trioxide (the V in 10 microns of ultra-thin titanium piece substrates prepared with embodiment 12O3@C) nanometer sheet
Array is as anode and cathode, and as quasi-solid electrolyte, (preparation method is lithium chloride/polyvinyl alcohol (LiCl/PVA) gel：
The lithium chloride solution for first preparing 5mol/L, is then added pva powder, the quality and lithium chloride solution of pva powder
Volume ratio be 0.1g/mL, in 85 DEG C of stirring in water bath 2-3 hour, stand to cool down obtains), be assembled into all solid state asymmetric soft
Property film ultracapacitor.Such as the scanning electron microscope diagram that Figure 11 is the ultracapacitor cross section, electrode and electrolysis in figure
Matter comes into full contact with, and the thickness of entire device is about 40 microns.
Electrochemical property test is carried out to the ultracapacitor, Figure 12 is cycle of the capacitor under different scanning rates
Volt-ampere curve figure (in the direction of arrows, from inside to outside sweep speed be respectively 5mV/s, 10mV/s, 25mV/s, 50mV/s and
100mV/s), as can be seen from Figure, cyclic voltammetry curve is similar to rectangle, and with the significantly change of sweep speed, the shape of curve
Shape does not have significant change, even if illustrating that the flexible super capacitor can also keep good electricity in fast charging and discharging
Hold feature.Figure 13 is constant current charge-discharge curve graph (in the direction of arrows, current density point of the capacitor under different current densities
It Wei not 0.25,0.5,1,2,4,8,16 and 32mA/cm2), it is respectively 0.25,0.5,1,2,4,8,16 and 32mA/ in current density
cm2Under the conditions of constant current discharge when, capacitance is respectively 102.7,103,103.5,99.3,86,77.6 and 69.4mF/cm2,
Capacity retention ratio (is respectively 0.25mA/cm with current density2When capacitance compare) 100%, 100%, 100%, 96.7%,
87.3% and 67.6%, current density increases 128 times (by 0.25mA/cm2Increase to 32mA/cm2) afterwards specific capacity remain to keep
67.6%, the above results illustrate that the flexibility asymmetric type supercapacitor has excellent high rate performance.Figure 14 is the capacitor
High rate performance figure under different scanning rates, sweep speed increases to 400mv/s from 5mv/s, and capacity still retains 47%.Figure 15 is should
The power density-energy density figure (a) of capacitor, maximum energy-density are higher than lithium thin film battery (b), and close in identical energy
Under the conditions of degree, high two orders of magnitude of power density ratio lithium thin film battery.Under equal-wattage density conditions, energy density compares quotient
With high 10 times of ultracapacitor (c) energy density or more of 5.5V/100mF, maximum power density is more than activated carbon/activated carbon
The commercial ultracapacitor (d) of system and the ultracapacitor (e) based on photoetching Graphene electrodes, and energy density is them
10 times or more.The above results show that the flexible super capacitor can possess high-energy density and high power density simultaneously.Figure 16
LED material object photos are lighted in the bent state for solid flexible asymmetric type supercapacitor manufactured in the present embodiment, illustrate this
Capacitor has good energy storage effect and flexibility.
Obviously, above-described embodiment be only intended to clearly illustrate made by example, and not limitation to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation or change therefore amplified
It moves within still in the protection domain of the invention.
Claims (10)
1. a kind of fexible film electrode material, it is characterised in that：The electrode material divides using ultra-thin titanium sheet as substrate in substrate
The vanadium trioxide nano-chip arrays of one layer of dense arrangement are furnished with, one layer of carbon materials are also wrapped on vanadium trioxide nanometer sheet surface
Material；
Preparation methods steps are as follows：
1) vanadic anhydride, two oxalic acid hydrates are added to the in the mixed solvent of acetone and water, blue solution is obtained by the reaction；
2) blue solution and ultra-thin titanium sheet obtained by step 1) being placed in hydrothermal reaction kettle, ultra-thin titanium sheet is blocked on one side, in
160-200 DEG C of hydro-thermal reaction 12-18 hours generates vanadium dioxide nano chip arrays after hydro-thermal reaction in titanium plate surface, will
After titanium sheet takes out washing and drying, there is vanadium dioxide nano chip arrays one side that glucose solution is added dropwise, drying repeats above-mentioned dropwise addition
Glucose solution and drying course, are subsequently placed in quartz tube furnace and are made annealing treatment, and carbon coating is obtained in titanium sheet substrate
Vanadium trioxide nano-chip arrays material, i.e. fexible film electrode material.
2. fexible film electrode material according to claim 1, it is characterised in that：The vanadium trioxide nanometer sheet thickness
For 30-40nm, vanadium trioxide nano-chip arrays layer thickness is 400-600nm, and the carbon material thickness is 5-10nm.
3. the preparation method of fexible film electrode material described in a kind of claims 1 or 2, it is characterised in that steps are as follows：
1) vanadic anhydride, two oxalic acid hydrates are added to the in the mixed solvent of acetone and water, blue solution is obtained by the reaction；
2) blue solution and ultra-thin titanium sheet obtained by step 1) being placed in hydrothermal reaction kettle, ultra-thin titanium sheet is blocked on one side, in
160-200 DEG C of hydro-thermal reaction 12-18 hours generates vanadium dioxide nano chip arrays after hydro-thermal reaction in titanium plate surface, will
After titanium sheet takes out washing and drying, there is vanadium dioxide nano chip arrays one side that glucose solution is added dropwise, drying repeats above-mentioned dropwise addition
Glucose solution and drying course, are subsequently placed in quartz tube furnace and are made annealing treatment, and carbon coating is obtained in titanium sheet substrate
Vanadium trioxide nano-chip arrays material, i.e. fexible film electrode material.
4. the preparation method of fexible film electrode material according to claim 3, which is characterized in that step 1) five oxygen
It is 1 to change two vanadium and two oxalic acid hydrate molar ratios:3；The mixed solvent of the acetone and water is acetone and water 1-4 by volume:3-6
It is mixed to get.
5. the preparation method of fexible film electrode material according to claim 3, which is characterized in that the step 1) reaction
Condition is to be stirred for 24 hours under 40 DEG C of water bath conditions.
6. the preparation method of fexible film electrode material according to claim 3, which is characterized in that the step 2) grape
A concentration of 0.11-0.44mol/L of sugar juice.
7. the preparation method of fexible film electrode material according to claim 3, which is characterized in that the step 2) annealing
The technique of processing is：550 DEG C are warming up to 10 DEG C/min under argon gas atmosphere, 1 hour is kept the temperature, then with stove natural cooling.
8. a kind of using fexible film electrode material as claimed in claim 1 or 2 as all solid state asymmetric flexibility of positive and negative electrode
Film ultracapacitor.
9. all solid state asymmetric flexible film super capacitor according to claim 8, which is characterized in that with chlorination
Lithium/polyvinyl alcohol gel is as quasi-solid electrolyte.
10. all solid state asymmetric flexible film super capacitor according to claim 9, which is characterized in that the chlorine
Change lithium/polyvinyl alcohol gel preparation method be：The lithium chloride solution for first preparing 5mol/L, is then added pva powder,
The quality of pva powder and the volume ratio of lithium chloride solution are 0.1g/mL, and in 85 DEG C of stirring in water bath 2-3 hour, standing was cold
But it obtains.
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| CN108962628A (en) * | 2018-07-10 | 2018-12-07 | 常州大学 | A method of flexible capacitor is prepared using semiconductor laser direct write |
| CN109449005B (en) * | 2018-11-16 | 2021-09-14 | 华中师范大学 | Integrated super capacitor |
| CN110132120B (en) * | 2019-04-15 | 2021-06-15 | 华南理工大学 | Stretchable pressure and stretching deformation sensor |
| CN111029573B (en) * | 2019-12-24 | 2021-07-27 | 武汉理工大学 | Titanium potassium phosphate oxide film negative electrode material and preparation method and application thereof |
| CN114220947B (en) * | 2021-12-09 | 2024-04-02 | 厦门大学 | Lithium metal battery negative electrode, current collector, preparation method of current collector and battery |
| CN114613975A (en) * | 2022-04-21 | 2022-06-10 | 重庆科技学院 | Preparation method of carbon-coated cobaltous oxide nanowire array/carbon cloth composite lithium ion battery flexible negative electrode material |
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