CN108172405B - The quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene - Google Patents
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 present invention discloses the method for electrochemical reduction oxidation graphene and the quasi-solid-state dye sensitized solar cell using the preparation of electrochemical reduction oxidation graphene, the method for electrochemical reduction oxidation graphene include the following steps: that (1) configures graphene oxide solution；(2) by the graphene oxide solution drop coating in step (1) in FTO electro-conductive glass substrate；(3) redox graphene is prepared with the method for electrochemical reduction.It is prepared using the quasi-solid-state dye sensitized solar cell of electrochemical reduction oxidation graphene preparation using following steps: (1) configuring liquid electrolyte and quasi-solid electrolyte；(2) light anode is prepared；(3) preparation is to electrode；(4) encapsulation of battery.The J-V curve of battery, which is 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 technique
Traditional carbon material because their inexpensive, high surface area, high conductivity be used as DSSCs to electrode material
Material.Carbon material abundant 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 mixes composition is used as DSSCs for the first time by group
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
Desired sheet resistance can be obtained in the specific surface of electrode in this way, obtains 6.67% photoelectric conversion effect to electrode based on this material
Rate.This work is that the non-Pt of developing low-cost opens road to electrode material.
As a member of carbon simple substance, the unique structure of graphene and property provide for multi-functional nanometer material research
Ideal platform.Xu etc. stablizes the suspension of reduced graphene (RGO) using 1- pyrene butyric acid for the first time, and the membrane electrode of preparation is used as
DSSC to electrode.But DSSCs of electrode is only obtained based on this 2.2% photoelectric efficiency.This explanation, with Pt to electrode
Material is compared, and there are also much need improved space.L.Kavan seminar research discovery I3 -/I–In graphene solution again
Life is better than in traditional organic solvent.In addition, they have found the catalytic activity and edge defect and oxide group of graphene
Concentration is directly proportional.I.Aksay seminar is research shows that the ratio of functionalization graphene C/O also has very strong shadow to its catalytic activity
It rings.By optimize functionalization graphene C/O ratio, as to electrode material obtain 5.0% efficiency (with Pt obtain similar in
Efficiency 5.5%).These conclusions show that the quantity of oxygen functional group and optimization C/O ratio are expected to obtain best catalytic activity.
Graphene oxide is reduced to redox graphene method, and there are commonly chemical methods, usually in graphene oxide
Reducing agent, such as hydrazine hydrate, sodium hydroxide, ethylenediamine or glucose are added in solution, can draw in the solution after reduction in this way
Enter impurity, makes troubles to the processing in later period.
Summary of the invention
Also it is an object of the present invention to provide a kind of method of electrochemical reduction oxidation graphene and using electrochemistry
The quasi-solid-state dye sensitized solar cell of former graphene oxide preparation.
In order to achieve the above objectives, the present invention adopts the following technical solutions:
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 substrate；
(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 to weigh graphene oxide with assay balance
Xie Yushui, first ultrasound, sees whether fully dissolved, after fully dissolved, dehydrated alcohol is added, obtains graphene oxide solution.
The method of above-mentioned electrochemical reduction oxidation graphene, in step (2): with configuration in liquid-transfering gun removing step (1)
Graphene oxide solution, drip in FTO electro-conductive glass substrate in the square of rubberized fabric, after drop is good, dried in infrared lamp；
The graphene oxide solution of same operating method difference drop coating different volumes contains in FTO electro-conductive glass substrate 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；Method particularly includes: use three-electrode system, work
Making electrode is the FTO electro-conductive glass substrate that homemade drop coating has graphene oxide solution in step (2), is Pt electrode 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 is dissolved in 1L secondary water, and with hydrochloric acid tune pH to 7.4 to obtain the final product；Current potential is set
- 1.4V is arrived for 0, sweeping speed is 100mV/s.
The method of above-mentioned electrochemical reduction oxidation graphene, in step (1): weighing 2.3mg oxidation stone with assay balance
Black alkene is dissolved in 6mL water, and first ultrasound 30-50min, sees whether fully dissolved, and after fully dissolved, 4mL dehydrated alcohol is added；
In step (2): pipetting the graphene oxide solution prepared in 10 μ L steps (1) every time with liquid-transfering gun, drip to FTO
In electro-conductive glass substrate in the square of rubberized fabric, square size is that 0.6cm × 0.6cm dries after drop is good in infrared lamp
Dry, the graphene oxide solution of same operating method difference drop coating different volumes prepares different content in FTO electro-conductive glass substrate
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；Method particularly includes: three-electrode system is used, working electrode is that homemade drop coating has graphite oxide in step (2)
The FTO electro-conductive glass substrate of alkene solution is Pt electrode, reference electrode Ag/AgCl to electrode；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 is 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, and sweeping speed is 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) FTO first the pretreatment of FTO: is used to 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, is dried with nitrogen, for use.
(2) liquid electrolyte and quasi-solid electrolyte are configured；
(3) light anode is prepared；
(4) preparation is to electrode: including configuring graphene oxide solution, prepared graphene oxide solution drop coating is in FTO
In electro-conductive glass substrate, and with the method for electrochemical reduction prepare redox graphene；
(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, it is 0.1mol/L, I that LiI concentration is configured in glove box2Concentration be 0.05mol/L,
DMPII concentration is the liquid electrolyte that 0.6mol/L, TBP concentration are 0.5mol/L, DMPII 1,2- dimethyl -3- propyl iodide
Change imidazoles, TBP is 4- tert .-butylpyridine；Quasi-solid electrolyte the preparation method is as follows: being added in above-mentioned liquid electrolyte
Concentration is the vinylidene fluoride hexafluoropropylene copolymer solution of 5wt%, and solvent is 3- methyl propionitrile.
The above-mentioned quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene, in step (3):
It is loaded with a thickness of 15 μm of TiO2The FTO electro-conductive glass of film immerses the TiCl that concentration is 0.05mol/L4In aqueous solution, it is placed in 70
DEG C baking oven in half an hour, after taking-up with deionized water rinse, be dried with nitrogen, be then placed in Muffle furnace 450 DEG C anneal, it is cold
But it to 120 DEG C, puts the electrodes into rapidly in prepared 1mmol/LN719 ruthenium dye acetonitrile solution, after standing 16h, takes out electricity
Pole is cleaned the dyestuff of film surface physical absorption with anhydrous acetonitrile, is dried with nitrogen.
The above-mentioned quasi-solid-state dye sensitized solar cell prepared using electrochemical reduction oxidation graphene, in step (4):
Its patch on the FTO conducting surface of 3M sticker after the pre-treatment, will be made at the square of 0.6cm × 0.6cm；It is weighed with assay balance
2.3mg graphene oxide is dissolved in 6mL water, and first ultrasound 30-50min, sees whether fully dissolved, after fully dissolved, addition 4mL without
Water-ethanol；The graphene oxide solution for pipetting 10 μ L preparation every time with liquid-transfering gun, drips to rubberized fabric in FTO electro-conductive glass substrate
In square, after drop is good, dried in infrared lamp, the graphene oxide solutions of same operating method difference drop coating different volumes in
FTO electro-conductive glass substrate, prepares the redox graphene of different content；Using three-electrode system, working electrode be it is above-mentioned from
The drop coating of system has the FTO electro-conductive glass substrate of graphene oxide solution, is Pt electrode, reference electrode Ag/AgCl to electrode；It is slow
Rushing 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 is dissolved in 1L 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, 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):
Surlyn film with a thickness of 30 μm is placed in the TiO to electrode and dye sensitization2Between light anode, then in heat-sealing instrument
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, keeps the electrolyte on hole whole
Into inside battery, i.e. completion cell package.
Beneficial effects of the present invention are as follows:
In the present invention, electrochemical reducing is directly to use the solution drop coating of graphene oxide to electro-conductive glass substrate
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 curve of battery shows that measuring open-circuit photovoltage based on quasi-solid electrolyte system is
673mV, short-circuit photocurrent are 8.74mA cm-2, fill factor 65%, corresponding photoelectric efficiency is 3.83%.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 a is the cyclic voltammetry curve figure that 40 μ L graphene oxide solution electrochemical reductions are RGO；
Fig. 1 b is the cyclic voltammetry curve figure that 80 μ L graphene oxide solution electrochemical reductions are RGO；
Fig. 1 c is the cyclic voltammetry curve figure that 120 μ L graphene oxide solution electrochemical reductions are RGO；
Fig. 1 d is the cyclic voltammetry curve figure that 150 μ L graphene oxide solution electrochemical reductions are RGO；
Fig. 2 a is the color before electrochemical reduction；
Fig. 2 b is the color after electrochemical reduction；
Fig. 3 is the variation diagram of XRD before and after electrochemical reduction；
Fig. 4 a is the scanning electron microscope (SEM) photograph of GO before electrochemical reduction；
Fig. 4 b is the scanning electron microscope (SEM) photograph of RGO after electrochemical reduction；
Fig. 5 is the identical to electrode assembling of the GO drop coating of same concentrations different volumes (40 μ L, 80 μ L, 120 μ L, 150 μ L)
Battery respectively complete the Nyquist spectrogram (frequency 800KHZ-0.1HZ, bias 0V) after primary CV-EIS test；
Fig. 6 is to be loaded with Tafel polarization curve after 150 μ LGO electrochemical reductions；
Fig. 7 a is that RGO is J-V (a) curve to the DDSCs of electrode；
Fig. 7 b is that RGO is IPCE curve (b) to electrode.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further below with reference to preferred embodiments and drawings
It is bright.Similar component is indicated in attached drawing with identical appended drawing reference.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.
One, the method for electrochemical reduction oxidation graphene
(1) 2.3mg graphene oxide (GO) being weighed with assay balance and being dissolved in 6mL water, first ultrasound 30-50min, observation is
No fully dissolved.After fully dissolved, 4mL dehydrated alcohol is added.
(2) it pipettes the graphene oxide solution prepared in 10 μ L steps (1) every time with liquid-transfering gun, drips to FTO glass rubberizing
In the square of cloth (square size 0.6cm × 0.6cm), after drop is good, dried in infrared lamp, same operating method is dripped respectively
The graphene oxide solution of different volumes is applied in FTO substrate, prepares the redox graphene of different content.
It (3) is RGO (reduction-oxidation graphite by the method reduction GO of the good electrode electrochemical reduction of drop coating in step (2)
Alkene).
The specific method is as follows: using three-electrode system, working electrode is that homemade drop coating has the FTO of GO to lead in step (2)
Electric glass is Pt electrode, reference electrode Ag/AgCl to electrode；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 is dissolved in 1L secondary water, and uses hydrochloric acid
Adjust pH to 7.4 to obtain the final product.Current potential is set as 0 to -1.4V, and sweeping speed is 100mV/s.
Two, following steps system is used using the quasi-solid-state dye sensitized solar cell of electrochemical reduction oxidation graphene preparation
It is standby:
The pretreatment of FTO: FTO is first used to detergent ultrasound 40min in ultrasonic cleaner；Then cleaning solution is fallen
Out, it is 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, is dried with nitrogen, for use.
It (is steamed again) by solvent of anhydrous acetonitrile, it is 0.1mol/L, I that LiI concentration is configured in glove box2Concentration is
0.05mol/L, DMPII concentration are the liquid electrolyte that 0.6mol/L, TBP concentration are 0.5mol/L, DMPII 1,2- diformazan
Base -3- propyl iodate imidazoles, TBP are 4- tert .-butylpyridine；Quasi-solid electrolyte the preparation method is as follows: in above-mentioned liquid electricity
The vinylidene fluoride hexafluoropropylene copolymer solution that concentration is 5wt% is added in Xie Zhizhong, and solvent is 3- methyl propionitrile.
The preparation of light anode: 15 μm of TiO are loaded with2The FTO electro-conductive glass of film immerses the TiCl that concentration is 0.05mol/L4
In aqueous solution, it is placed in half an hour in 70 DEG C of baking oven, rinsed, be dried with nitrogen with deionized water after taking-up, be 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 dye solution.After standing 16h, take
Electrode out cleans the dyestuff of film surface physical absorption with anhydrous acetonitrile, is dried with nitrogen.
Preparation to electrode: on 3M sticker FTO conducting surface after the pre-treatment, will make its patch at 0.6cm × 0.6cm just
It is rectangular；2.3mg graphene oxide, which is weighed, with assay balance is dissolved in 6mL water, first ultrasound 30-50min, sees whether fully dissolved,
After fully dissolved, 4mL dehydrated alcohol is added；The graphene oxide solution for pipetting 10 μ L preparation every time with liquid-transfering gun, drips to FTO and leads
It in electric substrate of glass in the square of rubberized fabric, after drop is good, is dried in infrared lamp, same operating method difference drop coating is not androgynous
Long-pending graphene oxide solution prepares the redox graphene of different content in FTO electro-conductive glass substrate；Using three electrode bodies
System, working electrode are the FTO electro-conductive glass substrate that above-mentioned homemade drop coating has graphene oxide solution, are Pt electrode 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 is dissolved in 1L secondary water, and with hydrochloric acid tune pH to 7.4 to obtain the final product；Current potential is set
- 1.4V is arrived for 0, sweeping speed is 100mV/s.
The encapsulation of battery: the Surlyn film with a thickness of 30 μm is placed in the TiO to electrode and dye sensitization2Light anode it
Between, then heat-sealing instrument (120 DEG C) in 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, i.e., completion cell package.
Three, 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 disadvantages, by the mixed solution drop coating of the second alcohol and water of GO and electro-conductive glass, then we take first
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 having had, therefore we have drop coating in PBS solution
GO is reduced electrochemically as RGO (Fig. 1 a-d).Since RGO is relative to GO after reduction, the oxygen-containing group of molecule is reduced, therefore meeting
There is peak current to gradually decrease, it is finally stable.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 restoring, and color is shallow
Brown.After electrochemical process reduction, color becomes the redox graphene of black, and the variation of this color can intuitively be seen
GO is reduced to the process of RGO out.
3.1.2XRD map
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), is
(200) crystallographic plane diffraction peak of graphite oxide does not occur sharp graphite (002) crystallographic plane diffraction peak about in map 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 map
Fig. 4 a is 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 is abundant, such as carboxyl, hydroxyl, ester group and ether, although making the hydrophily of the compound preferable, intermolecular appearance
Easily form packing phenomenon.Fig. 4 a clearly finds out, the aggregation of GO molecule.When drop coating in the surface FTO GO in PBS buffer solution
In, when to be reduced to redox graphene be (RGO), i.e., redox graphene is restored again on the basis of GO,
Exactly remove part functional group.The greatly reducing due to oxygen-containing group after reduction makes the reduction of RGO ability of aggregation, thus in base
Disperse more evenly Fig. 4 b on bottom.
3.2 catalytic activity characterization
3.2.1 electrochemical impedance spectroscopy
In order to further evaluate same concentrations different volumes GO solution to electrode to I3 -Reduction reaction electro-catalysis
Activity obtains the Nyquist impedance spectrum to electrode using the Symmetrical cells that structure is " to electrode/electrolyte/to electrode "
(EIS), as a result as shown in figure 5, going out equivalent circuit diagram to evaluate the performance parameter to electrode using Randles models fitting.
In general, Nyquist figure includes two semicircles, the semicircle of high frequency region is the charge transfer resistance R to electrode/electrolyte interfacect, 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: 40 μ L, 80 μ L,
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, carry
There is the FTO of 150 μ LGO to electrode to I3 -Reduction reaction electro catalytic activity it is higher.
3.2.2 polarization curve atlas analysis
Test the Tafel polarization curve of Symmetrical cells.In general, what Tafel polarization curve was made of three regions.?
Low potential area (IUI < 200mv) is relative to I3 -/I-Limit diffusion in the electrolyte.Intermediate potential area is since electric charge transfer is drawn
It rises, as the region Tafel.Test result is as shown, quasi- solid-state iodine electrolyte cathode and anode branch inclined rate mean electricity
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, J0It can also 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 RctAt anti-
Than, therefore the result that the result of Tafel polarization test is characterized with EIS is also consistent.
The research of 3.3 photoelectric properties
Quasi- solid-state iodine electrolyte phase compares, and liquid iodophor electrolyte has biggish charge transport rate.
Fig. 7 a is to be loaded with the FTO of 150 μ LGO to the J-V curve of 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 being also tested for RGO is photoelectric current work spectrum (IPCE and the incident monochromatic wavelength to the DSSCs of electrode assembling
Between relation curve), as a result as shown in Figure 7b.It can be seen that being reached at about 530nm to the IPCE of the DSSCs of electrode assembling
To maximum value, the absorption spectrum of this and N719 ruthenium dye is consistent.It is maximum within the scope of the light area that wavelength is 400~700nm
Value is 66%, only because battery J with highersc。
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 may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the scope of protection of the present invention.
Claims (1)
1. preparing quasi-solid-state dye sensitized solar cell using electrochemical reduction oxidation graphene, which is characterized in that quasi- solid-state dye
Material sensitization solar cell is prepared using following steps:
(1) FTO first the pretreatment of FTO: is used to 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, is dried with nitrogen, for use；
(2) liquid electrolyte and quasi-solid electrolyte are configured；
Using the anhydrous acetonitrile steamed again as solvent, it is 0.1mol/L, I that LiI concentration is configured in glove box2Concentration is 0.05mol/
L, DMPII concentration is the liquid electrolyte that 0.6mol/L, TBP concentration are 0.5mol/L, DMPII 1,2- dimethyl -3- propyl
Iodate imidazoles, TBP are 4- tert .-butylpyridine；Quasi-solid electrolyte the preparation method is as follows: in above-mentioned liquid electrolyte plus
Enter the vinylidene fluoride hexafluoropropylene copolymer solution that concentration is 5wt%, solvent is 3- methyl propionitrile；
(3) it prepares light anode: being loaded with a thickness of 15 μm of TiO2The FTO electro-conductive glass of film, immersing concentration is 0.05mol/L's
TiCl4In aqueous solution, it is placed in half an hour in 70 DEG C of baking oven, rinsed, be dried with nitrogen with deionized water after taking-up, be then placed in horse
It not anneals in furnace at 450 DEG C, is cooled to 120 DEG C, puts the electrodes into prepared 1mmol/LN719 ruthenium dye acetonitrile solution rapidly
In, after standing 16h, electrode is taken out, the dyestuff of film surface physical absorption is cleaned with anhydrous acetonitrile, is dried with nitrogen；
(4) preparation is to electrode:
Its patch on the FTO conducting surface of 3M sticker after the pre-treatment, will be made at the square of 0.6cm × 0.6cm；Claimed with assay balance
2.3mg graphene oxide is taken to be dissolved in 6mL water, first ultrasound 30-50min, sees whether fully dissolved, and after fully dissolved, 4mL is added
Dehydrated alcohol；The graphene oxide solution for pipetting 10 μ L preparation every time with liquid-transfering gun, drips to rubberized fabric in FTO electro-conductive glass substrate
Square in, pipette 150 μ L altogether, after drop is good, dried in infrared lamp；Using three-electrode system, working electrode be it is above-mentioned from
The drop coating of system has the FTO electro-conductive glass substrate of graphene oxide solution, is Pt electrode, reference electrode Ag/AgCl to electrode；It is slow
Rushing 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
It is dissolved in 1L secondary water 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；
(5) the Surlyn film with a thickness of 30 μm the encapsulation of battery: is placed in the TiO to electrode and dye sensitization2Light anode it
Between, then seal instrument in 120 DEG C under the conditions of hot pressing, cling；It is cooled to room temperature, quasi- solid-state electricity is added dropwise on the hole to the electrode back side
Xie Zhi makes the electrolyte on hole fully enter inside battery, i.e. completion cell package.
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