CN105206429A - Flexible thin film electrode material and preparation method thereof - Google Patents
Flexible thin film electrode material and preparation method thereof Download PDFInfo
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- CN105206429A CN105206429A CN201510713190.6A CN201510713190A CN105206429A CN 105206429 A CN105206429 A CN 105206429A CN 201510713190 A CN201510713190 A CN 201510713190A CN 105206429 A CN105206429 A CN 105206429A
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Abstract
The invention relates to a flexible thin film electrode material and a preparation method thereof. The electrode material adopts an ultrathin titanium sheet as a substrate, a layer of intensively arranged vanadium trioxide nanosheet array is distributed on the substrate; the surface of the vanadium trioxide nanosheet array is also coated with a layer of carbon material. The preparation method comprises the following steps: firstly, hydrothermally generating the vanadium trioxide nanosheet array on the ultrathin titanium sheet, and then conducting carbon coating by taking glucose as a carbon source to form the vanadium trioxide @ carbon compound nanosheet array, namely the flexible thin film electrode material. The electrode material can be used as a positive electrode and a negative electrode at the same time to assemble a supercapacitor. The method is simple to operate and facilitates realization of mass production, the obtained capacitor has excellent flexibility, the whole capacitor is only 40 micrometers in thickness, dissymmetrical energy storage principle, high voltage and high volume energy density are shown, and the flexible thin film electrode material can be used for the fields of flexible wearable electronic products and the like, and is hopeful to generate excellent social and economic benefits.
Description
Technical field
The invention belongs to capacitor technology field, relate to a kind of fexible film electrode material and preparation method thereof.
Background technology
Along with the development of flexible electronic product, flexible energy storage device also arises at the historic moment, wherein flexible thin film type ultracapacitor demonstrates huge application prospect, as having potential application in flexible display apparatus, flexible electronic skin and wearable electronic etc. because of its advantage such as high power, quick charge capability.Traditional flexible super capacitor has two classes usually: one is adopt carbon-based material (as carbon nano-tube or Graphene self-supported membrane) etc. as electrode, although have excellent flexibility and conductivity, but material with carbon element is the energy storage mechnism based on electric double layer, little relative to the fake capacitance material capacity of redox reaction mechanism; Two is to adopt on flexible carbon cloth direct growth fake capacitance active material as electrode, but carbon cloth collector is thicker and there is the structural void of up to a hundred microns, greatly wastes many spatial volumes.Therefore traditional flexible film super capacitor volume energy density and power density lower.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, a kind of ultra-thin, fine and close fake capacitance electrode material with high power capacity and preparation method thereof is provided, this electrode material is specially the coated vanadium trioxide nano-chip arrays material of carbon in ultra-thin titanium sheet substrate, using this electrode material simultaneously as positive and negative electrode build the ultracapacitor volume energy density of asymmetric energy storage mechnism and power density high.
For solving the problems of the technologies described above, technical scheme provided by the invention is:
There is provided a kind of fexible film electrode material, described electrode material for substrate, substrate is distributed with the vanadium trioxide nano-chip arrays of one deck dense arrangement with ultra-thin titanium sheet, is also coated with one deck material with carbon element on vanadium trioxide nanometer sheet surface.
By such scheme, described ultra-thin titanium sheet thickness is 10-50 μm.
By such scheme, described vanadium trioxide nanometer sheet thickness is 30-40nm, and vanadium trioxide nano-chip arrays layer thickness is 400-600nm, and described material with carbon element thickness is 5-10nm.
There is provided a kind of preparation method of fexible film electrode material, step is as follows:
1) vanadic oxide, two oxalic acid hydrates are added in the mixed solvent of acetone and water, be obtained by reacting blue solution;
2) by step 1) gained blue solution and ultra-thin titanium sheet be placed in hydrothermal reaction kettle, ultra-thin titanium sheet one side is blocked, in 160-200 DEG C of hydro-thermal reaction 12-18 hour, vanadium dioxide nano chip arrays is generated at titanium plate surface after hydro-thermal reaction terminates, after titanium sheet is taken out washing and drying, glucose solution is dripped there being vanadium dioxide nano chip arrays one side, dry, repeat above-mentioned dropping glucose solution and drying course, then be placed in quartz tube furnace and carry out annealing in process, titanium sheet substrate obtains the vanadium trioxide nano-chip arrays material that carbon is coated, i.e. fexible film electrode material.
By such scheme, step 1) described vanadic oxide and two oxalic acid hydrate mol ratios are 1:3; The mixed solvent of described acetone and water be acetone and water by volume 1-4:3-6 be mixed to get.
By such scheme, step 1) described reaction condition is stir 24h under 40 DEG C of water bath condition.
By such scheme, step 2) described glucose concentration is 0.11-0.44mol/L.
By such scheme, step 2) technique of described annealing in process is: is warming up to 550 DEG C with 10 DEG C/min under argon gas atmosphere, is incubated 1 hour, then naturally cools with stove.
The all solid state asymmetric flexible film super capacitor that it is positive and negative electrode that the present invention also provides with above-mentioned fexible film electrode material.
By such scheme, described all solid state asymmetric flexible film super capacitor is using lithium chloride/polyvinyl alcohol gel as quasi-solid electrolyte.
By such scheme, the preparation method of described lithium chloride/polyvinyl alcohol gel is: the lithium chloride solution first preparing 5mol/L, then adds pva powder, and the quality of pva powder and the volume ratio of lithium chloride solution are 0.1g/mL, in 85 DEG C of stirring in water bath 2-3 hour, standing cooling obtains.
Beneficial effect of the present invention is: 1, the present invention is using ultra-thin titanium sheet (10 μm) as substrate direct growth metal oxide nano-sheet array (vanadium oxide nano-chip arrays), establish the direct channel of electric transmission, ultra-thin titanium sheet has good flexibility simultaneously, and relative to the carbon-base film electrode of micron thickness up to a hundred greatly reduce capacitor overall volume, avoid interstitial space waste, thus improve the volume energy density of capacitor, 2, coated one deck carbon-coating on vanadium oxide nano-chip arrays, vanadium oxide nano-chip arrays electrode material conductivity after carbon is coated strengthens, and carbon-coating decreases metal oxide unsteadiness in the electrolyte as protective layer, prepared electrode material surface has very high specific area, electrolyte is fully contacted with electrode material, greatly shorten ion diffuse path, compared to typical electrode materials (metal oxide powder), there is better high rate performance, 3, just be with fexible film electrode material, negative electrode prepares ultracapacitor (thickness about 40 μm), just, negative electrode material is identical, but there is different redox reactions and form asymmetric high-efficiency energy-storage mechanism, facilitate capacitor manufacture, simultaneously, the metal oxide of nanoscale provides higher charge storage by fake capacitance reaction, compare with traditional double electric layers supercapacitor and larger specific capacity can be provided, accurate solid-state lithium chloride/polyvinyl alcohol (LiCl/PVA) gel electrolyte further suppress caving in of metal oxide structures in addition, enhance the stability of electrode, improve the cycle performance of capacitor, and avoid the problem of liquid electrolyte leakage, improve the actual use value of capacitor.
Accompanying drawing explanation
Fig. 1 is optical photograph and the scanning electron microscope diagram of the embodiment of the present invention 1 ultra-thin titanium sheet used, and wherein a is optical photograph, and b is scanning electron microscope diagram;
The scanning electron microscope diagram of the vanadium trioxide nano-chip arrays that carbon is coated in the ultra-thin titanium sheet substrate of Fig. 2 prepared by embodiment 1;
The transmission electron microscope figure of the vanadium trioxide nanometer sheet that carbon is coated in the ultra-thin titanium sheet substrate of Fig. 3 prepared by embodiment 1;
The X-ray diffractogram of vanadium trioxide nano-chip arrays (c) that Fig. 4 is vanadium dioxide nano chip arrays (b) in ultra-thin titanium sheet (a), ultra-thin titanium sheet substrate described in embodiment 1, carbon is coated;
The Raman spectrogram of vanadium trioxide nano-chip arrays (b) that Fig. 5 is vanadium dioxide nano chip arrays (a) in titanium sheet substrate ultra-thin described in embodiment 1, carbon is coated;
Fig. 6 is the photo of fexible film electrode material prepared by embodiment 1;
Fig. 7 be embodiment 1 prepare ultra-thin titanium sheet substrate on carbon coated vanadium trioxide nano-chip arrays assembling three electrode positive and negative electrode cyclic voltammogram;
Fig. 8 be in the ultra-thin titanium sheet substrate prepared of embodiment 1 the coated vanadium trioxide nano-chip arrays of carbon as positive pole constant current charge-discharge figure;
Fig. 9 be in the ultra-thin titanium sheet substrate prepared of embodiment 1 the coated vanadium trioxide nano-chip arrays of carbon as negative pole constant current charge-discharge figure;
Figure 10 be in the ultra-thin titanium sheet substrate prepared of embodiment 1 the coated vanadium trioxide nano-chip arrays of carbon as the electricity match map of positive and negative electrode;
Figure 11 is the scanning electron microscope diagram of the solid flexible asymmetric type supercapacitor cross section that the identical positive and negative electrode (the vanadium trioxide nano-chip arrays that in ultra-thin titanium sheet substrate, carbon is coated) of embodiment 2 preparation forms;
Figure 12 is the cyclic voltammetry curve figure of solid flexible asymmetric type supercapacitor prepared by embodiment 2;
Figure 13 is the constant current charge-discharge curve chart of solid flexible asymmetric type supercapacitor under different current density prepared by embodiment 2;
Figure 14 be embodiment 2 prepare solid flexible asymmetric type supercapacitor under different scanning rates high rate performance figure;
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 photo in kind in the bent state.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment 1
Prepare fexible film electrode material, concrete steps are as follows:
1) by 0.2g vanadic oxide (V
2o
5) and 0.45 gram of two oxalic acid hydrate (H
2c
2o
42H
2o) 10 milliliters of acetone (CH are added
3cOCH
3) and 25 ml waters mixed solution in, with water-bath magnetic stirring apparatus in 40 DEG C stir 24h, obtain even blue solution;
2) 10 microns of ultra-thin titanium sheet are washed at hydrochloric acid and deionized water for ultrasonic successively, dry, one side is blocked by thick titanium sheet, then the hydrothermal reaction kettle of polytetrafluoroethylliner liner substrate is placed in together with the above-mentioned solution be stirred, in 180 DEG C of hydro-thermal reactions 18 hours, vanadium dioxide nano chip arrays is generated at titanium plate surface, then the titanium sheet of nano-chip arrays is had to take out by long, after spending deionized water oven dry, vanadium dioxide nano chip arrays one side is had to drip (0.165mol/L) glucose solution in titanium sheet, dry, repeat above-mentioned dropping glucose solution and drying course once, then be placed in quartz tube furnace and carry out annealing in process, 550 DEG C are warming up under an argon atmosphere with 10 DEG C/min, be incubated 1 hour, then naturally cool with stove and obtain the coated vanadium trioxide nano-chip arrays material of carbon in ultra-thin titanium sheet substrate, i.e. fexible film electrode material.
Fig. 1 is optical photograph and the scanning electron microscope diagram of the present embodiment ultra-thin titanium sheet used, and ultra-thin titanium sheet thickness is 10 μm as can be seen from Figure, and flexible good.
The present embodiment gained fexible film electrode material is tested, Fig. 2 is the scanning electron microscope diagram of the vanadium trioxide nano-chip arrays that in ultra-thin titanium sheet substrate, carbon is coated, as seen from the figure, the coated vanadium trioxide nanometer sheet thickness of carbon is 30-40nm, the vanadium trioxide nano-chip arrays thickness formed is 400-600nm, vanadium trioxide nanometer sheet is interlaced, intensive, be evenly distributed in titanium sheet substrate.Fig. 3 is the transmission electron microscope figure of the vanadium trioxide nanometer sheet that in ultra-thin titanium sheet substrate, carbon is coated, and as can be seen from the figure the thickness of nanometer sheet carbon layer on surface is 5-10nm.
The X-ray diffractogram of vanadium trioxide nano-chip arrays (c) that Fig. 4 is titanium sheet (a) ultra-thin described in the present embodiment, vanadium dioxide nano chip arrays (b) in ultra-thin titanium sheet substrate, carbon are coated, as seen from the figure, the main peak position of nano-chip arrays is identical with vanadium dioxide, but the peak of the titanium dioxide that appearance one is faint near 69 °, come from titanium sheet in hydrothermal reaction process by slight oxidation, after annealing in process, main peak position is identical with vanadium trioxide, this is because vanadium dioxide in-situ reducing is at high temperature vanadium trioxide by carbon.The Raman spectrogram of vanadium trioxide nano-chip arrays (b) that Fig. 5 is vanadium dioxide nano chip arrays (a) in titanium sheet substrate ultra-thin described in the present embodiment, carbon is coated, after can annealing being found out in figure, obvious D peak and the G peak having occurred carbon, illustrates the coated graphited carbon of a layer segment in vanadium trioxide nanometer sheet top layer.Fig. 6 be preparation ultra-thin titanium sheet substrate on the photo of the coated vanadium trioxide nano-chip arrays material of carbon, can find out that it is flexible good.Fig. 7 makes work electrode with the vanadium trioxide nano-chip arrays material that carbon in the substrate of above-mentioned ultra-thin titanium sheet is coated, platinum electrode is done electrode, saturated calomel electrode does the just three electrode of reference electrode assembling, negative electrode cyclic voltammetry curve figure (presses arrow direction, sweep speed is 10mV/s respectively, 25mV/s, 50mV/s and 100mV/s), as can be seen from Figure: the vanadium trioxide nano-array electrode that in ultra-thin titanium sheet substrate, carbon is coated makes negative pole, a pair obvious oxidation reaction peak is shown in-1.0-0.1V electromotive force interval, and make positive pole shows comparatively rectangle cyclic voltammetry curve in 0.1-1.0V electromotive force interval, illustrate using this array material simultaneously as just, it is asymmetric capacitor that negative material assembles the capacitor obtained.Constant current charge-discharge curve chart when Fig. 8 and Fig. 9 is respectively using this electrode material as positive and negative electrode under different current density, image approximate isosceles triangle, charging and discharging curve is symmetrical, shows good capacitive characteristics, is respectively 1,2,4 and 8mA/cm in current density
2under condition during constant current charge-discharge, positive discharge electricity is respectively 176.6,164.2,136.4 and 101.6mC/cm
2, it (is 1mA/cm with current density that its capability retention is respectively
2time electric capacity compare) 100%, 93.0%, 77.2% and 57.5%.Negative discharge electricity is respectively 189.1,155.4,129.2 and 108.8mC/cm
2time, it (is 1mA/cm with current density that its capacity retention rate is respectively
2time electric capacity compare) 100%, 82.2%, 68.3% and 57.5%.Figure 10 is vanadium trioxide nano-array electrode that in the ultra-thin titanium sheet substrate prepared of the present embodiment, carbon is coated as the electricity match map of supercapacitor positive electrode and negative pole, can find out that it has good electricity matching degree and good high rate performance.
Embodiment 2
Prepare all solid state asymmetric flexible film super capacitor, concrete steps are as follows:
Vanadium trioxide (the V that the 10 microns of suprabasil carbon of ultra-thin titanium sheet prepared with embodiment 1 is coated
2o
3c) nano-chip arrays is as positive pole and negative pole, as quasi-solid electrolyte, (compound method is lithium chloride/polyvinyl alcohol (LiCl/PVA) gel: the lithium chloride solution first preparing 5mol/L, then pva powder is added, the quality of pva powder and the volume ratio of lithium chloride solution are 0.1g/mL, in 85 DEG C of stirring in water bath 2-3 hour, standing cooling obtains), be assembled into all solid state asymmetric flexible film super capacitor.As the scanning electron microscope diagram that Figure 11 is this ultracapacitor cross section, in figure, electrode fully contacts with electrolyte, and the thickness of whole device is about 40 microns.
Electrochemical property test is carried out to this ultracapacitor, Figure 12 be the cyclic voltammetry curve figure of this capacitor under different scanning rates (in the direction of arrows, sweep speed is respectively 5mV/s, 10mV/s, 25mV/s, 50mV/s and 100mV/s from inside to outside), as can be seen from Figure, cyclic voltammetry curve is similar to rectangle, and along with the significantly change of sweep speed, the shape of curve does not change significantly, even if illustrate that this flexible super capacitor also can keep good capacitive characteristics in fast charging and discharging situation.Figure 13 is that (in the direction of arrows, current density is respectively 0.25,0.5,1,2,4,8,16 and 32mA/cm to the constant current charge-discharge curve chart of this capacitor under different current density
2), be respectively 0.25,0.5,1,2,4,8,16 and 32mA/cm in current density
2under condition during constant current discharge, its electric capacity is respectively 102.7,103,103.5,99.3,86,77.6 and 69.4mF/cm
2, it (is 0.25mA/cm with current density that its capability retention is respectively
2time electric capacity compare) 100%, 100%, 100%, 96.7%, 87.3% and 67.6%, current density increases 128 times (by 0.25mA/cm
2increase to 32mA/cm
2) afterwards specific capacity still can keep 67.6%, the above results illustrates that this flexible asymmetric type supercapacitor has excellent high rate performance.Figure 14 is the high rate performance figure of this capacitor under different scanning rates, and sweep speed and be increased to 400mv/s from 5mv/s, capacity still retains 47%.Figure 15 is power density-energy density figure (a) of this capacitor, its maximum energy-density higher than lithium thin film battery (b), and under identical energy density conditions, high two orders of magnitude of power density ratio lithium thin film battery.Under equal-wattage density conditions, its energy density is higher than ultracapacitor (c) energy density of commercial 5.5V/100mF more than 10 times, its maximum power density is greater than the commercial ultracapacitor (d) of active carbon/active carbon system and the ultracapacitor (e) based on photoetching Graphene electrodes, and energy density is their more than 10 times.The above results shows that this flexible super capacitor can have high-energy-density and high power density simultaneously.Figure 16 is that solid flexible asymmetric type supercapacitor prepared by the present embodiment lights LED photo in kind in the bent state, illustrates that this capacitor has good energy storage effect and flexibility.
Obviously, above-described embodiment is only for the example done clearly is described, and the restriction not to execution mode.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all execution modes.And therefore amplified apparent change or variation are still within the protection range of the invention.
Claims (10)
1. a fexible film electrode material, is characterized in that: described electrode material for substrate, substrate is distributed with the vanadium trioxide nano-chip arrays of one deck dense arrangement with ultra-thin titanium sheet, is also coated with one deck material with carbon element on vanadium trioxide nanometer sheet surface.
2. fexible film electrode material according to claim 1, is characterized in that: described vanadium trioxide nanometer sheet thickness is 30-40nm, and vanadium trioxide nano-chip arrays layer thickness is 400-600nm, and described material with carbon element thickness is 5-10nm.
3. a preparation method for fexible film electrode material described in claim 1 or 2, is characterized in that step is as follows:
1) vanadic oxide, two oxalic acid hydrates are added in the mixed solvent of acetone and water, be obtained by reacting blue solution;
2) by step 1) gained blue solution and ultra-thin titanium sheet be placed in hydrothermal reaction kettle, ultra-thin titanium sheet one side is blocked, in 160-200 DEG C of hydro-thermal reaction 12-18 hour, vanadium dioxide nano chip arrays is generated at titanium plate surface after hydro-thermal reaction terminates, after titanium sheet is taken out washing and drying, glucose solution is dripped there being vanadium dioxide nano chip arrays one side, dry, repeat above-mentioned dropping glucose solution and drying course, then be placed in quartz tube furnace and carry out annealing in process, titanium sheet substrate obtains the vanadium trioxide nano-chip arrays material that carbon is coated, i.e. fexible film electrode material.
4. the preparation method of fexible film electrode material according to claim 3, is characterized in that, step 1) described vanadic oxide and two oxalic acid hydrate mol ratios are 1:3; The mixed solvent of described acetone and water be acetone and water by volume 1-4:3-6 be mixed to get.
5. the preparation method of fexible film electrode material according to claim 3, is characterized in that, step 1) described reaction condition is stir 24h under 40 DEG C of water bath condition.
6. the preparation method of fexible film electrode material according to claim 3, is characterized in that, step 2) described glucose concentration is 0.11-0.44mol/L.
7. the preparation method of fexible film electrode material according to claim 3, is characterized in that, step 2) technique of described annealing in process is: is warming up to 550 DEG C with 10 DEG C/min under argon gas atmosphere, is incubated 1 hour, then naturally cools with stove.
8. all solid state asymmetric flexible film super capacitor that is positive and negative electrode with the fexible film electrode material described in claim 1 or 2.
9. all solid state asymmetric flexible film super capacitor according to claim 8, is characterized in that, using lithium chloride/polyvinyl alcohol gel as quasi-solid electrolyte.
10. all solid state asymmetric flexible film super capacitor according to claim 9, it is characterized in that, the preparation method of described lithium chloride/polyvinyl alcohol gel is: the lithium chloride solution first preparing 5mol/L, then pva powder is added, the quality of pva powder and the volume ratio of lithium chloride solution are 0.1g/mL, in 85 DEG C of stirring in water bath 2-3 hour, standing cooling obtains.
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CN110132120A (en) * | 2019-04-15 | 2019-08-16 | 华南理工大学 | A kind of stretchable formula pressure and tensile deformation sensor |
CN111029573A (en) * | 2019-12-24 | 2020-04-17 | 武汉理工大学 | Titanium potassium phosphate oxide film negative electrode material and preparation method and application thereof |
CN114220947A (en) * | 2021-12-09 | 2022-03-22 | 厦门大学 | Lithium metal battery cathode, 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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CN108962628A (en) * | 2018-07-10 | 2018-12-07 | 常州大学 | A method of flexible capacitor is prepared using semiconductor laser direct write |
CN109449005A (en) * | 2018-11-16 | 2019-03-08 | 华中师范大学 | Integrate supercapacitor |
CN109449005B (en) * | 2018-11-16 | 2021-09-14 | 华中师范大学 | Integrated super capacitor |
CN110132120A (en) * | 2019-04-15 | 2019-08-16 | 华南理工大学 | A kind of stretchable formula pressure and tensile deformation sensor |
CN110132120B (en) * | 2019-04-15 | 2021-06-15 | 华南理工大学 | Stretchable pressure and stretching deformation sensor |
CN111029573A (en) * | 2019-12-24 | 2020-04-17 | 武汉理工大学 | Titanium potassium phosphate oxide film negative electrode material and preparation method and application thereof |
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 |
CN114220947A (en) * | 2021-12-09 | 2022-03-22 | 厦门大学 | Lithium metal battery cathode, current collector, preparation method of current collector and battery |
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 |
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