CN108172405A - The method of electrochemical reduction oxidation graphene and the quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene - Google Patents
The method of electrochemical reduction oxidation graphene and the quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene Download PDFInfo
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2022—Light-sensitive devices characterized by he counter electrode
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/0029—Processes of manufacture
-
- 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
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
Abstract
The quasi-solid-state dye sensitized solar cell that the present invention is disclosed the method for electrochemical reduction oxidation graphene and prepared using electrochemical reduction oxidation graphene, the method for electrochemical reduction oxidation graphene include the following steps：(1) graphene oxide solution is configured；(2) by the graphene oxide solution drop coating in step (1) in FTO electro-conductive glass substrates；(3) redox graphene is prepared with the method for electrochemical reduction.It is prepared using quasi-solid-state dye sensitized solar cell prepared by electrochemical reduction oxidation graphene using following steps：(1) liquid electrolyte and quasi-solid electrolyte is configured；(2) light anode is prepared；(3) it prepares to electrode；(4) encapsulation of battery.The J V curves of battery, which are shown, measures that open-circuit photovoltage is 673mV, short-circuit photocurrent is 8.74mA cm based on quasi-solid electrolyte system‑2, fill factor 65%, corresponding photoelectric efficiency is 3.83%.
Description
Technical field
The present invention relates to dye-sensitized solar cells.More particularly, to a kind of electrochemical reduction oxidation graphene
Method and the quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene.
Background technology
Traditional carbon material because they inexpensive, high surface area, high conductivity be used as DSSCs to electrode material
Material.Abundant carbon material includes the allotrope of the carbon such as carbon black, graphene, carbon nanotube, fullerene.
In early days, M.The material that the carbon black on function graphite and high surface is mixed composition by group for the first time is used as DSSCs
CE.Result of study show the effect of graphite in mixing material improve the conduction of electronics and carbon black for increase catalytic activity and
The specific surface of electrode can obtain desired sheet resistance in this way, and 6.67% opto-electronic conversion effect is obtained to electrode based on this material
Rate.This work opens road for the non-Pt of developing low-cost to electrode material.
As a member of carbon simple substance, the unique structure of graphene and property are provided for multi-functional nanometer material research
Ideal platform.Xu etc. stablizes the suspension of reduced graphene (RGO) using 1- pyrenes butyric acid for the first time, and the membrane electrode of preparation is used as
DSSC to electrode.But 2.2% photoelectric efficiency is only obtained to the DSSCs of electrode based on this.This explanation, with Pt to electrode
Material is compared, and also much needs improved space.The research of L.Kavan seminars finds I3 -/I–In graphene solution again
Life is better than in traditional organic solvent.In addition, they have found the catalytic activity of graphene and edge defect and oxide group
Concentration is directly proportional.I.Aksay seminars are research shows that the ratio of functionalization graphene C/O also has its catalytic activity very strong shadow
It rings.By optimizing the ratio of functionalization graphene C/O, (obtained as the efficiency that 5.0% is obtained to electrode material with Pt close
Efficiency 5.5%).These conclusions show that the quantity of oxygen functional group and optimization C/O ratios are expected to obtain best catalytic activity.
Graphene oxide is reduced to redox graphene method is common chemical method, usually in graphene oxide
Reducing agent, such as hydrazine hydrate, sodium hydroxide, ethylenediamine or glucose are added in solution, can be drawn in the solution after reduction in this way
Enter impurity, make troubles to the processing in later stage.
Invention content
It is an object of the present invention to provide a kind of method of electrochemical reduction oxidation graphene and using electrochemistry also
Quasi-solid-state dye sensitized solar cell prepared by former graphene oxide.
In order to achieve the above objectives, the present invention uses following technical proposals：
The method of electrochemical reduction oxidation graphene, includes the following steps：
(1) graphene oxide solution is configured；
(2) by the graphene oxide solution drop coating in step (1) in FTO electro-conductive glass substrates；
(3) redox graphene is prepared with the method for electrochemical reduction.
The method of above-mentioned electrochemical reduction oxidation graphene, in step (1)：It is molten that graphene oxide is weighed with assay balance
Xie Yushui, first ultrasound, sees whether fully dissolved, after fully dissolved, adds in absolute ethyl alcohol, obtains graphene oxide solution.
The method of above-mentioned electrochemical reduction oxidation graphene, in step (2)：It is configured in liquid-transfering gun removing step (1)
Graphene oxide solution, drip in FTO electro-conductive glass substrates in the square of rubberized fabric, after drop is good, dried in infrared lamp；
The graphene oxide solution of similary operating method difference drop coating different volumes contains in FTO electro-conductive glass substrates to prepare difference
The redox graphene of amount.
The method of above-mentioned electrochemical reduction oxidation graphene, in step (3)：The good electrode of drop coating in step (2) is used
Graphene oxide is reduced to redox graphene by the method for electrochemical reduction；Specific method is：Using three-electrode system, work
Making electrode has the FTO electro-conductive glass substrates of graphene oxide solution for homemade drop coating in step (2), is Pt electrodes to electrode,
Reference electrode is Ag/AgCl；Buffer solution is the 0.1M PBS that pH is 7.4, and specific preparation method is as follows：5.76g KH2PO4、
20.64g Na2HPO4·12H2O and 7.45g KCl are dissolved in 1L secondary waters, and with hydrochloric acid tune pH to 7.4 to obtain the final product；Current potential is set
It is 0 to -1.4V, sweeps speed as 100mV/s.
The method of above-mentioned electrochemical reduction oxidation graphene, in step (1)：2.3 mg oxidation stones are weighed with assay balance
Black alkene is dissolved in 6mL water, and first ultrasound 30-50min, sees whether fully dissolved, after fully dissolved, adds in 4mL absolute ethyl alcohols；
In step (2)：It pipettes the graphene oxide solution prepared in 10 μ L steps (1) every time with liquid-transfering gun, drips to FTO
In electro-conductive glass substrate in the square of rubberized fabric, square size is the cm of 0.6cm × 0.6, after drop is good, is dried in infrared lamp
Dry, the graphene oxide solution of similary operating method difference drop coating different volumes prepares different content in FTO electro-conductive glass substrates
Redox graphene；
In step (3)：Graphene oxide is reduced to restore by the method for the good electrode electrochemical reduction of (2) drop coating
Graphene oxide；Specific method is：Using three-electrode system, working electrode is that homemade drop coating has graphite oxide in step (2)
The FTO electro-conductive glass substrates of alkene solution, to electrode be Pt electrodes, reference electrode Ag/AgCl；Buffer solution is that pH is 7.4
0.1M PBS, specific preparation method are as follows：5.76g KH2PO4、20.64g Na2HPO4·12H2O and 7.45g KCl are dissolved in 1L
In secondary water, and with hydrochloric acid tune pH to 7.4 to obtain the final product；Current potential is set as 0 to -1.4V, sweeps speed as 100mV/s.
Using electrochemical reduction oxidation graphene prepare quasi-solid-state dye sensitized solar cell, it is quasi-solid-state dye sensitized too
Positive electricity pond is prepared using following steps：
(1) pretreatment of FTO：FTO is first used into detergent ultrasound 40min in ultrasonic cleaner.Then by cleaning solution
It pours out, is rinsed well again with secondary water after rinsing.Then after the isopropanol saturated solution ultrasound 40min of NaOH, then one
Ultrasound 40min in secondary water.EtOH Sonicate 20min is finally used, nitrogen dries up, for use.
(2) liquid electrolyte and quasi-solid electrolyte is configured；
(3) light anode is prepared；
(4) it prepares to electrode：Including graphene oxide solution is configured, prepared graphene oxide solution drop coating is in FTO
Redox graphene is prepared in electro-conductive glass substrate and with the method for electrochemical reduction；
(5) encapsulation of battery.
The above-mentioned quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene, in step (2)：
Using the anhydrous acetonitrile steamed again as solvent, LiI a concentration of 0.1mol/L, I are configured in glove box2A concentration of 0.05mol/L,
The liquid electrolyte of a concentration of 0.5mol/L of DMPII a concentration of 0.6mol/L, TBP, DMPII 1,2- dimethyl -3- propyl iodides
Change imidazoles, TBP is 4- tert .-butylpyridines；The preparation method of quasi-solid electrolyte is as follows：It is added in above-mentioned liquid electrolyte
The vinylidene fluoride hexafluoropropylene copolymer solution of a concentration of 5wt%, solvent are 3- methyl propionitrile.
The above-mentioned quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene, in step (3)：
Thickness is loaded with as 15 μm of TiO2The FTO electro-conductive glass of film immerses the TiCl of a concentration of 0.05mol/L4In aqueous solution, it is placed in 70
DEG C baking oven in half an hour, rinsed after taking-up with deionized water, nitrogen drying, be then placed in Muffle furnace 450 DEG C annealing, it is cold
But it to 120 DEG C, puts the electrodes into rapidly in prepared 1mmol/LN719 ruthenium dyes acetonitrile solution, after standing 16h, takes out electricity
Pole cleans the dyestuff of film surface physical absorption, nitrogen drying with anhydrous acetonitrile.
The above-mentioned quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene, in step (4)：
Square of its patch into 0.6cm × 0.6cm on the FTO conducting surfaces of 3M stickers after the pre-treatment, will be made；It is weighed with assay balance
2.3mg graphene oxides are dissolved in 6mL water, and first ultrasound 30-50min, sees whether fully dissolved, after fully dissolved, add in 4mL
Absolute ethyl alcohol；It pipettes the graphene oxide solution of 10 μ L preparations every time with liquid-transfering gun, drips to rubberized fabric in FTO electro-conductive glass substrates
Square in, after drop is good, dried in infrared lamp, the graphene oxide solution of similary operating method difference drop coating different volumes
In FTO electro-conductive glass substrates, the redox graphene of different content is prepared；Using three-electrode system, working electrode is above-mentioned
Homemade drop coating has the FTO electro-conductive glass substrates of graphene oxide solution, to electrode be Pt electrodes, reference electrode Ag/AgCl；
Buffer solution is the 0.1M PBS that pH is 7.4, and specific preparation method is as follows：5.76g KH2PO4、20.64g Na2HPO4·12H2O
It is dissolved in 1L secondary waters with 7.45g KCl, and with hydrochloric acid tune pH to 7.4 to obtain the final product；Current potential is set as 0 to -1.4V, and sweeping speed is
100mV/s。
The above-mentioned quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene, in step (5)：
The Surlyn films that thickness is 30 μm are placed in the TiO to electrode and dye sensitization2Between light anode, then in instrument is sealed
Hot pressing under the conditions of 120 DEG C is clung；It is cooled to room temperature, electrolyte is added dropwise on the hole to the electrode back side, makes the electrolyte on hole whole
Into inside battery, that is, complete cell package.
Beneficial effects of the present invention are as follows：
In the present invention, electrochemical reducing is directly by the solution drop coating of graphene oxide to electro-conductive glass substrate, is used
Graphite oxide is quickly reduced to redox graphene by three-electrode method.Whole process does not introduce other toxic chemicals,
It is a kind of green method for preparing redox graphene.Different amounts of RGO will be loaded with to be used as to electrode, assemble " sandwich " formula
Battery studies its photoelectric properties.The J-V curves of battery show that measuring open-circuit photovoltage based on quasi-solid electrolyte system is
673mV, short-circuit photocurrent are 8.74 mA cm-2, fill factor 65%, corresponding photoelectric efficiency is 3.83%.
Description of the drawings
The specific embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 a are the cyclic voltammetry curve figure that 40 μ L graphene oxide solution electrochemical reductions are RGO；
Fig. 1 b are the cyclic voltammetry curve figure that 80 μ L graphene oxide solution electrochemical reductions are RGO；
Fig. 1 c are the cyclic voltammetry curve figure that 120 μ L graphene oxide solution electrochemical reductions are RGO；
Fig. 1 d are the cyclic voltammetry curve figure that 150 μ L graphene oxide solution electrochemical reductions are RGO；
Fig. 2 a are the color before electrochemical reduction；
Fig. 2 b are the color after electrochemical reduction；
Fig. 3 is the variation diagram of XRD before and after electrochemical reduction；
Fig. 4 a are the scanning electron microscope (SEM) photograph of GO before electrochemical reduction；
Fig. 4 b are the scanning electron microscope (SEM) photograph of RGO after electrochemical reduction；
Fig. 5 is the identical to electrode assembling of the GO drop coatings of same concentrations different volumes (40 μ L, 80 μ L, 120 μ L, 150 μ L)
Battery respectively complete the Nyquist spectrograms after primary CV-EIS tests (frequency 800KHZ-0.1HZ is biased as 0V)；
Fig. 6 is is loaded with Tafel polarization curves after 150 μ LGO electrochemical reductions；
Fig. 7 a are that RGO is J-V (a) curves to the DDSCs of electrode；
Fig. 7 b are that RGO is IPCE curves (b) to electrode.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar component is indicated with identical reference numeral in attached drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
First, the method for electrochemical reduction oxidation graphene
(1) 2.3mg graphene oxides (GO) are weighed with assay balance and is dissolved in 6mL water, first ultrasound 30-50min, observation
Whether fully dissolved.After fully dissolved, 4mL absolute ethyl alcohols are added in.
(2) it pipettes the graphene oxide solution prepared in 10 μ L steps (1) every time with liquid-transfering gun, drips to FTO glass rubberizings
In the square of cloth (square size 0.6cm × 0.6cm), after drop is good, dried in infrared lamp, similary operating method is dripped respectively
The graphene oxide solution of different volumes is applied in FTO substrates, prepares the redox graphene of different content.
(3) it is RGO (reduction-oxidation graphite by the method for the good electrode electrochemical reduction of drop coating in step (2) reduction GO
Alkene).
Specific method is as follows：Using three-electrode system, working electrode is that the FTO that homemade drop coating has GO in step (2) is led
Electric glass, to electrode be Pt electrodes, reference electrode Ag/AgCl；Buffer solution is the 0.1M PBS that pH is 7.4, specific to prepare
Method is as follows：5.76g KH2PO4、20.64g Na2HPO4·12H2O and 7.45g KCl are dissolved in 1L secondary waters, and use hydrochloric acid
Adjust pH to 7.4 to obtain the final product.Current potential is set as 0 to -1.4V, sweeps speed as 100mV/s.
2nd, following steps system is used using quasi-solid-state dye sensitized solar cell prepared by electrochemical reduction oxidation graphene
It is standby：
The pretreatment of FTO：FTO is first used into detergent ultrasound 40min in ultrasonic cleaner；Then cleaning solution is fallen
Go out, rinsed well again with secondary water after rinsing；Then after the isopropanol saturated solution ultrasound 40min of NaOH, then primary
Ultrasound 40min in water；EtOH Sonicate 20min is finally used, nitrogen dries up, for use.
It (is steamed again) by solvent of anhydrous acetonitrile, LiI a concentration of 0.1mol/L, I is configured in glove box2It is a concentration of
The liquid electrolyte of a concentration of 0.5mol/L of 0.05mol/L, DMPII a concentration of 0.6mol/L, TBP, DMPII 1,2- diformazans
Base -3- propyl iodate imidazoles, TBP are 4- tert .-butylpyridines；The preparation method of quasi-solid electrolyte is as follows：In above-mentioned liquid electricity
Xie Zhizhong adds in vinylidene-perfluoropropene copolymer solution of a concentration of 5wt%, and solvent is 3- methyl propionitrile.
The preparation of light anode：It is loaded with 15 μm of TiO2The FTO electro-conductive glass of film immerses the TiCl of a concentration of 0.05 mol/L4
In aqueous solution, half an hour in 70 DEG C of baking oven is placed in, is rinsed after taking-up with deionized water, nitrogen drying, is then placed in Muffle furnace
Middle annealing (450 DEG C), is cooled to 120 DEG C, puts the electrodes into rapidly in prepared N719 ruthenium dyes solution.After standing 16h, take
Go out electrode, the dyestuff of film surface physical absorption, nitrogen drying are cleaned with anhydrous acetonitrile.
Preparation to electrode：Its patch on the FTO conducting surfaces of 3M stickers after the pre-treatment, will be made into 0.6cm × 0.6cm's
Square；2.3mg graphene oxides are weighed with assay balance and are dissolved in 6mL water, first ultrasound 30-50min, are seen whether complete molten
Solution after fully dissolved, adds in 4mL absolute ethyl alcohols；It pipettes the graphene oxide solution of 10 μ L preparations every time with liquid-transfering gun, drips to
In FTO electro-conductive glass substrates in the square of rubberized fabric, after drop is good, dried in infrared lamp, similary operating method distinguishes drop coating
The graphene oxide solution of different volumes prepares the redox graphene of different content in FTO electro-conductive glass substrates；Using three
Electrode system, working electrode have the FTO electro-conductive glass substrates of graphene oxide solution for above-mentioned homemade drop coating, are Pt to electrode
Electrode, reference electrode Ag/AgCl；Buffer solution is the 0.1 M PBS that pH is 7.4, and specific preparation method is as follows：5.76g
KH2PO4、20.64g Na2HPO4·12H2O and 7.45g KCl are dissolved in 1L secondary waters, and with hydrochloric acid tune pH to 7.4 to obtain the final product；
Current potential is set as 0 to -1.4V, sweeps speed as 100mV/s.
The encapsulation of battery：The Surlyn films that thickness is 30 μm are placed in the TiO to electrode and dye sensitization2Light anode it
Between, then in heat-sealing instrument (120 DEG C) hot pressing, cling.It is cooled to room temperature, electrolyte is added dropwise on the hole to the electrode back side, makes hole
On electrolyte fully enter inside battery, that is, complete cell package.
3rd, result and analysis
The characterization of 3.1 electrochemical reduction GO
3.1.1 cyclic voltammetric
Graphene oxide since itself has the hydrophilic radicals such as hydroxyl, carboxyl, cause its in the application of DSSC by
Limitation.In order to overcome these shortcomings, we are taken on the mixed solution drop coating of the second alcohol and water of GO and electro-conductive glass first, then
Redox graphene is reduced to using the method for electrochemical reduction.Electrochemistry is relative to common chemical reduction method method
(being usually added into hydrazine hydrate reduction agent) has many advantages, such as quick, simple, pollution-free.
RGO is for GO, the catalytic activity and electric conductivity that have had, therefore we have drop coating in PBS solution
GO is reduced electrochemically as RGO (Fig. 1 a-d).Since RGO is reduced relative to GO, the oxygen-containing group of molecule after reduction, therefore
It will appear peak current to continuously decrease, finally stablize.Gradually decreasing for peak current has absolutely proved that GO is reduced to RGO.
By Fig. 2 a-b, it can also be seen that, drop coating is being posted rectangular for graphene oxide in adhesive tape before reduction, and color is shallow
Brown.After electrochemical process restores, color becomes the redox graphene of black, and the variation of this color can intuitively be seen
Go out the process that GO is reduced to RGO.
3.1.2XRD collection of illustrative plates
Fig. 3 gives the variation diagram of XRD before and after electrochemical reduction.In the diffracting spectrum of GO, near 2 θ=10.61 °
There is a characteristic peak (apparent peak does not occur in upper figure, the peak may be forced very much not have due to the peak of FTO electro-conductive glass), be
(200) crystallographic plane diffraction peak of graphite oxide does not occur sharp graphite (002) crystallographic plane diffraction peak about in collection of illustrative plates at 2 θ=26 °,
This shows that graphite has been fully oxidized.Simultaneously as intercalation effect makes graphite layers, away from widening, graphite-structure is destroyed, and is formed
New crystal structure.After graphene oxide is reduced electrochemically, about there is a wider diffraction maximum in 2 θ=24 °, this
Show that GO loses most oxygen-containing group and interplanar distance is caused to reduce in reduction process.
3.1.3 scanning electron microscope collection of illustrative plates
Fig. 4 a are the scanning electron microscope (SEM) photograph that graphene oxide (GO) drop coating shows in FTO.Since the surface of graphene oxide contains
Oxygen functional group enriches, such as carboxyl, hydroxyl, ester group and ether, although so that the hydrophily of the compound is preferable, intermolecular appearance
Easily form packing phenomenon.Fig. 4 a clearly find out, the aggregation of GO molecules.When drop coating in FTO surfaces GO in PBS buffer solutions
In, when to be reduced to redox graphene be (RGO), i.e., redox graphene is on the basis of GO, is restored again,
Exactly remove part functional group.The greatly reducing due to oxygen-containing group after reduction makes the reduction of RGO ability of aggregation, so as in base
Disperse evenly Fig. 4 b on bottom.
3.2 catalytic activity characterize
3.2.1 electrochemical impedance spectroscopy
In order to further evaluate the GO solution of the different volumes of same concentrations to electrode to I3 -Reduction reaction electro-catalysis
Activity obtains the Nyquist impedance spectrums to electrode using Symmetrical cells of the structure for " to electrode/electrolyte/to electrode "
(EIS), the results are shown in Figure 5, goes out equivalent circuit diagram using Randles models fittings to evaluate the performance parameter to electrode.
In general, Nyquist figures include two semicircles, the semicircle of high frequency region is the charge transfer resistance R to electrode/electrolyte interfacect, it is low
Frequency area semicircle is I inside electrolyte3 -/I-This special diffusion resistance (Z of the energy of electricity pairN).As can be seen from Figure 5：40μL、80μL、
The impedance value R of 120 μ L, 150 μ LctRespectively 800 Ω, 521 Ω, 166 Ω, 60 Ω illustrate in the range of certain drop coating amount,
The FTO of 150 μ LGO is loaded with to electrode to I3 -Reduction reaction electro catalytic activity it is higher.
3.2.2 polarization curve atlas analysis
Test the Tafel polarization curves of Symmetrical cells.In general, Tafel polarization curves are made of three regions.
Low potential area (IUI<200mv) relative to I3 -/I-Limit diffusion in the electrolyte.Intermediate potential area is since electric charge transfer is drawn
It rises, as Tafel regions.Test result is as shown in the figure, quasi- solid-state iodine electrolyte cathode means electricity with anode branch inclined rate
Pole surface has higher current density.(exchange current density, J0).Higher slope further relates to urging
Changing in reaction has higher electro catalytic activity.
In addition, J0Also it can be calculated according to formula (1), wherein R is calibrating gas constant, and T is absolute temperature, RctFor electricity
Lotus transfer resistance, n are the electronics number that electrochemical reaction is related to, and F is Faraday constant.By formula (1) it is found that J0With RctInto anti-
Than, therefore the result that the result of Tafel polarization tests is characterized with EIS is also consistent.
3.3 photoelectric properties are studied
Quasi- solid-state iodine electrolyte phase compares, and liquid iodophor electrolyte has larger charge transport rate.
Fig. 7 a are to be loaded with the J-V curves of the FTO of 150 μ LGO to the DSSCs of electrode assembling.The PCE of the DSSCs of assembling is
3.83% (Voc=673mV, Jsc=8.74mA cm-2, FF=0.65), this shows that RGO can be preferably in catalytic electrolysis matter
I3 -, photovoltaic performance significantly improves.
And it is photoelectric current work spectrum (IPCE and the incident monochromatic wavelength to the DSSCs of electrode assembling to be also tested for RGO
Between relation curve), as a result as shown in Figure 7b.It can be seen that the IPCE of the DSSCs of electrode assembling is reached at about 530nm
To maximum value, the absorption spectrum of this and N719 ruthenium dyes is consistent.It is maximum in the range of the light area that wavelength is 400~700nm
It is 66% to be worth, only because the battery has higher Jsc。
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention for those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the row of protection scope of the present invention.
Claims (10)
1. the method for electrochemical reduction oxidation graphene, which is characterized in that include the following steps：
(1) graphene oxide solution is configured；
(2) by the graphene oxide solution drop coating in step (1) in FTO electro-conductive glass substrates；
(3) redox graphene is prepared with the method for electrochemical reduction.
2. the method for electrochemical reduction oxidation graphene according to claim 1, which is characterized in that in step (1)：With
Assay balance weighs graphene oxide and is dissolved in water, and first ultrasound, sees whether fully dissolved, after fully dissolved, adds in absolute ethyl alcohol,
Obtain graphene oxide solution.
3. the method for electrochemical reduction oxidation graphene according to claim 2, which is characterized in that in step (2)：With
The graphene oxide solution being configured in liquid-transfering gun removing step (1) drips to the square of rubberized fabric in FTO electro-conductive glass substrates
It is interior, after drop is good, dried in infrared lamp；The graphene oxide solution of similary operating method drop coating different volumes respectively is led in FTO
Electric substrate of glass, to prepare the redox graphene of different content.
4. the method for electrochemical reduction oxidation graphene according to claim 3, which is characterized in that in step (3)：It will
Graphene oxide is reduced to redox graphene by the method for the good electrode electrochemical reduction of drop coating in step (2)；Specifically
Method is：Using three-electrode system, working electrode is the FTO conductions that homemade drop coating has graphene oxide solution in step (2)
Substrate of glass, to electrode be Pt electrodes, reference electrode Ag/AgCl；Buffer solution is the 0.1M PBS that pH is 7.4, is specifically matched
Method processed is as follows：5.76g KH2PO4、20.64g Na2HPO4·12H2O and 7.45g KCl are dissolved in 1L secondary waters, and use salt
Acid adjusts pH to 7.4 to obtain the final product；Current potential is set as 0 to -1.4V, sweeps speed as 100mV/s.
5. the method for electrochemical reduction oxidation graphene according to claim 1, which is characterized in that
In step (1)：2.3mg graphene oxides are weighed with assay balance and are dissolved in 6mL water, first ultrasound 30-50min, observation
Whether fully dissolved, after fully dissolved, add in 4mL absolute ethyl alcohols；
In step (2)：It pipettes the graphene oxide solution prepared in 10 μ L steps (1) every time with liquid-transfering gun, drips to FTO conductions
In substrate of glass in the square of rubberized fabric, square size is 0.6cm × 0.6cm, after drop is good, is dried in infrared lamp, together
The graphene oxide solution of sample operating method difference drop coating different volumes prepares going back for different content in FTO electro-conductive glass substrates
Former graphene oxide；
In step (3)：Graphene oxide is reduced to reduction-oxidation by the method for the good electrode electrochemical reduction of (2) drop coating
Graphene；Specific method is：Using three-electrode system, working electrode is that homemade drop coating has the graphene oxide molten in step (2)
The FTO electro-conductive glass substrates of liquid, to electrode be Pt electrodes, reference electrode Ag/AgCl；Buffer solution is the 0.1M that pH is 7.4
PBS, specific preparation method are as follows：5.76g KH2PO4、20.64g Na2HPO4·12H2O and 7.45g KCl are dissolved in 1L bis- times
In water, and with hydrochloric acid tune pH to 7.4 to obtain the final product；Current potential is set as 0 to -1.4V, sweeps speed as 100mV/s.
6. the quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene, which is characterized in that quasi- solid-state
Dye-sensitized solar cells are prepared using following steps：
(1) pretreatment of FTO：FTO is first used into detergent ultrasound 40min in ultrasonic cleaner；Then cleaning solution is poured out,
It is rinsed well again with secondary water after rinsing；Then after the isopropanol saturated solution ultrasound 40min of NaOH, then in a water
Ultrasonic 40min；EtOH Sonicate 20min is finally used, nitrogen dries up, for use；
(2) liquid electrolyte and quasi-solid electrolyte is configured；
(3) light anode is prepared；
(4) it prepares to electrode：Including graphene oxide solution is configured, prepared graphene oxide solution drop coating is in FTO conductions
Redox graphene is prepared in substrate of glass and with the method for electrochemical reduction；
(5) encapsulation of battery.
7. the quasi-solid-state dye sensitized sun electricity according to claim 6 prepared using electrochemical reduction oxidation graphene
Pond, which is characterized in that in step (2)：Using the anhydrous acetonitrile steamed again as solvent, it is a concentration of that LiI is configured in glove box
0.1mol/L、I2The liquid electrolyte of a concentration of 0.5mol/L of a concentration of 0.05mol/L, DMPII a concentration of 0.6mol/L, TBP,
DMPII is 1,2- dimethyl -3- propyl iodate imidazoles, and TBP is 4- tert .-butylpyridines；The preparation method of quasi-solid electrolyte is such as
Under：The vinylidene fluoride hexafluoropropylene copolymer solution of a concentration of 5wt% is added in above-mentioned liquid electrolyte, solvent is 3- first
Base propionitrile.
8. the quasi-solid-state dye sensitized sun electricity according to claim 7 prepared using electrochemical reduction oxidation graphene
Pond, which is characterized in that in step (3)：Thickness is loaded with as 15 μm of TiO2The FTO electro-conductive glass of film immerses a concentration of
The TiCl of 0.05mol/L4In aqueous solution, half an hour in 70 DEG C of baking oven is placed in, is rinsed after taking-up with deionized water, nitrogen is blown
It is dry, it is then placed in Muffle furnace in 450 DEG C of annealing, is cooled to 120 DEG C, puts the electrodes into prepared 1mmol/LN719 rapidly
In ruthenium dye acetonitrile solution, after standing 16h, electrode is taken out, the dyestuff of film surface physical absorption, nitrogen are cleaned with anhydrous acetonitrile
Drying.
9. the quasi-solid-state dye sensitized sun electricity according to claim 8 prepared using electrochemical reduction oxidation graphene
Pond, which is characterized in that in step (4)：On the FTO conducting surfaces of 3M stickers after the pre-treatment, will make its patch into 0.6cm ×
The square of 0.6cm；2.3mg graphene oxides are weighed with assay balance and are dissolved in 6mL water, and first ultrasound 30-50min, observation is
No fully dissolved after fully dissolved, adds in 4mL absolute ethyl alcohols；Pipette the graphene oxide solution of 10 μ L preparations every time with liquid-transfering gun,
It drips in FTO electro-conductive glass substrates in the square of rubberized fabric, after drop is good, is dried in infrared lamp, similary operating method difference
The graphene oxide solution of drop coating different volumes prepares the redox graphene of different content in FTO electro-conductive glass substrates；It adopts
With three-electrode system, working electrode has the FTO electro-conductive glass substrates of graphene oxide solution for above-mentioned homemade drop coating, to electrode
For Pt electrodes, reference electrode Ag/AgCl；Buffer solution is the 0.1M PBS that pH is 7.4, and specific preparation method is as follows：5.76g
KH2PO4、20.64g Na2HPO4·12H2O and 7.45g KCl are dissolved in 1L secondary waters, and with hydrochloric acid tune pH to 7.4 to obtain the final product；
Current potential is set as 0 to -1.4V, sweeps speed as 100mV/s.
10. the quasi-solid-state dye sensitized sun electricity according to claim 9 prepared using electrochemical reduction oxidation graphene
Pond, which is characterized in that in step (5)：The Surlyn films that thickness is 30 μm are placed in the TiO to electrode and dye sensitization2
Between light anode, then in instrument is sealed hot pressing under the conditions of 120 DEG C, cling；It is cooled to room temperature, is added dropwise on the hole to the electrode back side
Quasi-solid electrolyte makes the electrolyte on hole fully enter inside battery, that is, completes cell package.
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| CN111635144A (en) * | 2020-06-30 | 2020-09-08 | 华侨大学 | Preparation method of reduced graphene oxide film capable of enhancing carbon dot fluorescence |
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