CN102543469B - Dye-sensitized solar cell nitrogen-doping graphene counter electrode and preparation method thereof - Google Patents
Dye-sensitized solar cell nitrogen-doping graphene counter electrode and preparation method thereof Download PDFInfo
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- Y02E10/542—Dye sensitized solar cells
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
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- Y02E10/549—Organic PV cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a dye-sensitized solar cell nitrogen-doping graphene counter electrode and a preparation method thereof, and belongs to the technical field of solar cells, in particular to a nitrogen-doping graphene counter electrode applied to a dye-sensitized solar cell and a preparation method of the counter electrode. The counter electrode comprises a substrate, and is characterized in that: a plurality of layers of nitrogen-doping graphene films are uniformly cured on the surface of the substrate by methods of drawing, spinning, dispensing, spraying or printing. The counter electrode is prepared from nitrogen-doping graphene; on one hand, the advantages of high specific surface area, high conductivity, high stability, high intensity and the like of the graphene are utilized; and on the other hand, because nitrogen is doped in the graphene, carbon in a crystal lattice is replaced by nitrogen atoms in different forms, and more defects are formed in the doped graphene. Therefore, the electrocatalytic activity of the counter electrode can be greatly improved, the performance of the prepared counter electrode is improved, the counter electrode is applied to the dye-sensitized solar cell, and the photoelectric conversion efficiency exceeds 6.5 percent.
Description
Technical field
DSSC nitrogen-doping graphene counter electrode and preparation method thereof, belongs to technical field of solar batteries, is specifically related to a kind of nitrogen-doping graphene counter electrode in DSSC and preparation method thereof that is applied to.
Background technology
DSSC is because manufacture craft is simple, cost is low, the high extensive concern that is subject to of conversion efficiency.As the chief component of DSSC, to the Main Function of electrode, be to accept the electronics of external circuit the I in catalytic reduction electrolyte
3 -for I
-.At present DSSC is mainly that platinum is deposited on to the platinum prepared in substrate to electrode to electrode.Although platinum catalytic activity is high, platinum is rare precious metals, and price is too high, and is containing I
-/ I
3 -in the electrolyte of redox couple, stability is bad.In recent years, occurred that employing material with carbon element and conducting polymer replace platinum preparation at a low price to electrode report, but because the catalytic activity of material with carbon element and conducting polymer is lower than platinum, so the photoelectric conversion efficiency of assembled battery is also on the low side.Graphene be a kind of by carbon atom with sp
2hybridized orbit forms the two-dimensional material that hexangle type is honeycomb lattice.Because its special structure makes it have the features such as high specific area, electrical conductance, mechanical strength and stability, the very big concern of therefore having introduced people in fields such as photoelectron, energy storage and conversion, electro-catalysis.The CN101976608A Chinese invention patent of announcing on February 16th, 2011 discloses that a kind of to take Graphene nanostructure, bigger serface be raw material, is coated in and on glass substrate, prepares the method for Graphene to electrode.But experiment showed, adopt Graphene as DSSC to electrode, its catalytic activity is not high.This is mainly that catalytic activity point causes less because the defect of Graphene itself is few.
Summary of the invention
The technical problem to be solved in the present invention is: overcome the deficiencies in the prior art, provide a kind of electro catalytic activity high, good stability, cheap DSSC nitrogen-doping graphene counter electrode and preparation method thereof.
The technical solution adopted for the present invention to solve the technical problems is: this DSSC nitrogen-doping graphene counter electrode, comprise substrate, and it is characterized in that: the film that is evenly solidified with multilayer nitrogen-doped graphene on described substrate surface.
The number of plies of described multilayer nitrogen-doped graphene film is 2～5 layers, and gross thickness is 0.1-15 micron.Can apply the thickness that the number of plies is controlled substrate surface nitrogen-doped graphene film by controlling the concentration of nitrogen-doped graphene in dispersion liquid or increasing.
Described substrate is a kind of in electro-conductive glass sheet, ITO conductive polyester sheet, titanium sheet, transparent polyester sheet or sheet glass.When only applying one deck nitrogen-doped graphene film, can adopt electro-conductive glass sheet, ITO conductive polyester sheet or titanium sheet as substrate.When the concentration of nitrogen-doped graphene is higher or apply the number of plies when more, also can directly adopt nonconducting common glass sheet, polyester sheet etc. as substrate.
Described by nitrogen-doped graphene film be cured to suprabasil method comprise lift, spin coating, drip to be coated with, spraying or printing.
A method of preparing above-mentioned DSSC nitrogen-doping graphene counter electrode, is characterized in that, this preparation method comprises the steps:
1) adopt hydro thermal method to prepare nitrogen-doped graphene;
2) nitrogen-doped graphene preparing is distributed in solvent, by ultrasonic and stirring, forms uniform and stable dispersion liquid; Described solvent is the mixture of a kind of or two kinds of arbitrary proportions in water, ethanol, isopropyl alcohol, n-butanol;
3) substrate is preheated to 45～90 ℃, then by dispersion liquid by lifting, spin coating, drip be coated with, the method for spraying or printing is evenly cured to substrate surface, and be dried 0.5～2 hour under vacuum condition, baking temperature is 50～300 ℃, makes DSSC nitrogen-doping graphene counter electrode.
Step 2), in, in described dispersion liquid, the concentration of nitrogen-doped graphene is 0.1-1.5mg/mL.
Preferably, in described dispersion liquid, the concentration of nitrogen-doped graphene is 0.3-1.2mg/mL.
Step 3), in, described baking temperature is 80～200 ℃.
In addition the concrete steps that hydro thermal method step 1) is prepared nitrogen-doped graphene are:
(1) 30～80mg graphene oxide is distributed in 100mL deionized water, ultrasonic dispersion 0.5～1 hour, adds ammoniacal liquor 1～2ml, regulator solution pH=10～11;
(2) above-mentioned solution is put into the water heating kettle that is lined with polytetrafluoroethylene, at 100～200 ℃, hydro-thermal reaction 8～24 hours;
(3) naturally cool to after room temperature, filter the reactant liquor in water heating kettle, and repeatedly rinse with deionized water and ethanol the product leaching, then dry under 50 ℃ of vacuum, make nitrogen-doped graphene.
Compared with prior art, the beneficial effect that DSSC nitrogen-doping graphene counter electrode of the present invention and preparation method thereof has is: 1, adopt nitrogen-doped graphene to prepare electrode as raw material, utilize Graphene specific area large on the one hand, conductivity is high, good stability, the advantages such as intensity is large, on the other hand due in nitrogen-doped graphene, nitrogen-atoms replaces the carbon in lattice with different forms, in doped graphene, form more defect point, therefore can greatly improve the electro catalytic activity to electrode, improve the prepared performance to electrode, be applied in DSSC, photoelectric conversion efficiency surpasses 6.5%, 2, nitrogen-doped graphene material is easily prepared, and price is relatively low, good stability, mechanical strength is high, and wide material sources, applicable to various electrode basement, the electrode of preparing various shape and size, is conducive to suitability for industrialized production and the practical application of DSSC, 3, preparation technology is simple, does not need special, complicated equipment, can make the manufacturing cost of DSSC further reduce.
Accompanying drawing explanation
Fig. 1 is the nitrogen-doped graphene x-ray photoelectron spectroscopy figure of embodiment 1 preparation.
Fig. 2 is the I-V curve of the DSSC based on DSSC nitrogen-doping graphene counter electrode in embodiment 1.
Below in conjunction with accompanying drawing 1～2, the present invention will be further described, and wherein embodiment 1 is most preferred embodiment:
Embodiment
Experimental technique described in following embodiment, if no special instructions, is conventional method; The synthetic method of following graphene oxide is referring to document (W.Hummers, J.Am.Chem.Soc.1958,80:1339); Reagent and material described in other, if no special instructions, all can obtain from commercial channels.
Embodiment 1
First adopt hydro thermal method to prepare nitrogen-doped graphene:
Get 30mg graphene oxide and be scattered in 100mL deionized water, ultrasonic dispersion 0.5 hour, dissolves graphene oxide completely, generates uniform brown yellow solution, adds ammoniacal liquor 1ml, regulation system pH value=10.The solution that regulates pH value is put into the water heating kettle that is lined with polytetrafluoroethylene, at 150 ℃, hydro-thermal reaction 24 hours.Naturally cool to after room temperature, filter the reactant liquor in water heating kettle, and by deionized water and ethanol wash products repeatedly, then at 50 ℃, vacuum, be dried and obtain nitrogen-doped graphene.Nitrogen-doped graphene characterizes with x-ray photoelectron spectroscopy, as shown in Figure 1, occurs obvious N1S peak in figure.
Nitrogen-doped graphene is cured to conductive glass surface, prepares DSSC nitrogen-doping graphene counter electrode:
Get the nitrogen-doped graphene that 8mg prepares and add in isopropyl alcohol, ultrasonic 2 hours, form even, stable dispersion liquid system, the concentration of the alkene dispersion liquid of nitrogen doped graphite is 0.8mg/mL.Electro-conductive glass is cleaned up, be then preheating to 90 ℃, then by the method for spraying, the dispersion liquid that is dissolved with nitrogen-doped graphene is coated onto in the electro-conductive glass substrate of preheating, form the film of one deck nitrogen-doped graphene, thickness is about 7 microns.The electrode of preparation is put into 80 ℃, vacuum and be dried 1 hour, prepare DSSC nitrogen-doping graphene counter electrode.
Prepare nitrogen-doping graphene counter electrode DSSC:
First electro-conductive glass is carried out to preliminary treatment, then titania slurry is coated on the electro-conductive glass of handling well, after high-temperature process, immerse the work electrode that adsorbs the formation battery that spends the night in dyestuff, on work electrode, cover the nitrogen-doping graphene counter electrode of above-mentioned preparation, two interelectrode gap fillings contain I
-/ I
3 -the electrolyte of redox couple, is prepared into DSSC.
Measure the DSSC electricity conversion of preparation.The photoelectricity I-V curve of battery is as shown in Figure 2.
The test of battery performance be by from battery work electrode with electrode drawn to two wires receive on battery performance test device.The work area of battery is 0.2cm
-2, intensity of illumination is 100mW/cm
2.Fill factor, curve factor (ff) refers to the current/voltage product (I on the point that can obtain peak power output in I-V curve
opt* V
opt) and I
sc* V
oc(I
scfor short-circuit photocurrent, V
ocfor open circuit photovoltage) ratio, its embodies the power output of battery with the change characteristic of load.Photoelectric conversion efficiency (η) is I
opt* V
optluminous power P with input
inratio.
Short-circuit photocurrent, open circuit photovoltage, fill factor, curve factor and the photoelectric conversion efficiency of by Fig. 2, being calculated battery are respectively 14.18mA/cm
2, 0.685V, 0.67 and 6.51%.
Embodiment 2
Get 80mg graphene oxide and add in 100ml deionized water, ultrasonic dispersion 1 hour, dissolves graphene oxide completely, generates uniform brown yellow solution, then adds ammoniacal liquor 1.5ml, makes pH value=11 of solution.The solution that regulates pH value is put into and is lined with teflon-lined water heating kettle, and at 200 ℃, hydro-thermal is 22 hours.Naturally cool to after room temperature, filter the reactant liquor in water heating kettle, with deionized water and ethanol, repeatedly rinse the product leaching, then at 50 ℃, vacuum, be dried, make nitrogen-doped graphene.
Getting the nitrogen-doped graphene that 2mg prepares is distributed in isopropyl alcohol, within ultrasonic 1 hour, form uniform dispersion, the concentration of the alkene dispersion liquid of nitrogen doped graphite is 0.1mg/mL, with spin-coating method, above-mentioned dispersion liquid is cured to the ITO conductive polyester sheet surface that cleans up in advance and be preheated to 45 ℃, the film that forms one deck nitrogen-doped graphene, thickness is about 0.1 micron.By the electrode of preparation under vacuum condition 60 ℃ dry 0.5 hour.Prepare nitrogen-doped graphene electrode.
Embodiment 3
Get 50mg graphene oxide and be scattered in 100mL deionized water, ultrasonic dispersion 45min, dissolves graphene oxide completely, generates uniform brown yellow solution, adds ammoniacal liquor 1.2ml, regulation system pH value=10.5.The solution that regulates pH value is put into the water heating kettle that is lined with polytetrafluoroethylene, at 150 ℃, hydro-thermal reaction 24 hours.Naturally cool to after room temperature, filter the reactant liquor in water heating kettle, and by deionized water and ethanol wash products repeatedly, then at 50 ℃, vacuum, be dried, obtain nitrogen-doped graphene.
Getting the nitrogen-doped graphene that 20mg prepares is distributed in ethanol, within ultrasonic 1 hour, form uniform dispersion, the concentration of the alkene dispersion liquid of nitrogen doped graphite is 1.5mg/mL, with czochralski method, above-mentioned dispersion liquid is cured to the titanium plate surface that cleans up in advance and be preheated to 90 ℃, form one deck nitrogen-doped graphene film, thickness is about 2 microns.By the electrode of preparation under vacuum condition 300 ℃ dry 0.5 hour.Prepare nitrogen-doped graphene electrode.
Embodiment 4
The preparation method of nitrogen-doped graphene is with embodiment 1.
Getting the nitrogen-doped graphene that 20mg prepares is distributed in ethanol, within ultrasonic 1 hour, form uniform dispersion, the concentration of the alkene dispersion liquid of nitrogen doped graphite is 1.5mg/mL, with drop-coating, above-mentioned dispersion liquid is cured to the conductive glass surface that cleans up in advance and be preheated to 70 ℃, form one deck nitrogen-doped graphene film, repeatedly drip and be coated with 2 times, nitrogen-doped graphene film thickness is about 15 microns.By the electrode of preparation under vacuum condition 50 ℃ dry 2 hours.Prepare nitrogen-doped graphene electrode.
Embodiment 5
The preparation method of nitrogen-doped graphene is with embodiment 1.
Getting the nitrogen-doped graphene that 10mg prepares is distributed in deionized water, within ultrasonic 1 hour, form uniform dispersion, the concentration of the alkene dispersion liquid of nitrogen doped graphite is 1mg/mL, with drop-coating, above-mentioned dispersion liquid is cured to the transparent polyester sheet surface that cleans up in advance and be preheated to 45 ℃, form nitrogen-doped graphene film, gross thickness is about 7 microns.Dry 2 hours of lower 50 ℃ of vacuum condition.Prepare nitrogen-doped graphene electrode.
Embodiment 6
The preparation method of nitrogen-doped graphene is with embodiment 1.
Getting the nitrogen-doped graphene that 20mg prepares is distributed in n-butanol, within ultrasonic 1 hour, form uniform dispersion, the concentration of the alkene dispersion liquid of nitrogen doped graphite is 0.5mg/mL, by print process, above-mentioned dispersion liquid is cured to the common glass sheet surface that cleans up in advance and be preheated to 70 ℃, repeatedly print 3 times, form gross thickness and be about 5 microns of nitrogen-doped graphene films.Dry 1 hour of lower 200 ℃ of vacuum condition.Prepare nitrogen-doped graphene electrode.
Embodiment 7
The preparation method of nitrogen-doped graphene is with embodiment 1.
Getting the nitrogen-doped graphene that 15mg prepares is distributed in the mixed solution (volume ratio is 1: 1) of ethanol and isopropyl alcohol, within ultrasonic 1 hour, form uniform dispersion, the concentration of the alkene dispersion liquid of nitrogen doped graphite is that 0.5mg/mL is cured to above-mentioned dispersion liquid by print process the ITO conductive polyester sheet surface that cleans up in advance and be preheated to 45 ℃, form one deck nitrogen-doped graphene film, thickness is about 2 microns.By the electrode of preparation under vacuum condition 60 ℃ dry 1.5 hours.Prepare nitrogen-doped graphene electrode.
Embodiment 8
The preparation method of nitrogen-doped graphene is with embodiment 1.
Get in the mixed solution (volume ratio is 2: 1) that 15mg nitrogen-doped graphene is distributed to n-butanol and water, within ultrasonic 1 hour, form uniform dispersion, the concentration of the alkene dispersion liquid of nitrogen doped graphite is 1mg/mL, with czochralski method, nitrogen-doped graphene is deposited to the electro-conductive glass substrate surface that cleans up in advance and be preheated to 60 ℃, thickness is about 1.5 microns, dry 0.5 hour of lower 300 ℃ of vacuum condition.Prepare nitrogen-doped graphene electrode.
Embodiment 9
The preparation method of nitrogen-doped graphene is with embodiment 1.
Getting the nitrogen-doped graphene that 15mg prepares is distributed in the mixed solution (volume ratio is 1: 2) of n-butanol and isopropyl alcohol, within ultrasonic 1 hour, form uniform dispersion, the concentration of the alkene dispersion liquid of nitrogen doped graphite is that 0.7mg/mL is cured to above-mentioned dispersion liquid with spraying process the ITO conductive polyester sheet surface that cleans up in advance and be preheated to 45 ℃, form one deck nitrogen-doped graphene film, thickness is about 6 microns.By the electrode of preparation under vacuum condition 80 ℃ dry 1.5 hours.Prepare nitrogen-doped graphene electrode.
The above, be only preferred embodiment of the present invention, is not the present invention to be done to the restriction of other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not depart from, any simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection range of technical solution of the present invention.
Claims (6)
1. a DSSC nitrogen-doping graphene counter electrode, comprises substrate, it is characterized in that: on described substrate surface, be evenly solidified with the film of 2 ~ 5 layers of nitrogen-doped graphene, gross thickness is 0.1-15 micron; Described substrate is ITO conductive polyester sheet, titanium sheet or transparent polyester sheet, and described nitrogen-doped graphene adopts hydro thermal method preparation; The concrete steps that described hydro thermal method is prepared nitrogen-doped graphene are:
1) 30 ~ 80mg graphene oxide is distributed in 100mL deionized water, ultrasonic dispersion 0.5 ~ 1 hour, adds ammoniacal liquor 1 ~ 2ml, regulator solution pH=10 ~ 11;
2) above-mentioned solution is put into the water heating kettle that is lined with polytetrafluoroethylene, at 100 ~ 200 ℃, hydro-thermal reaction 8 ~ 24 hours;
3) naturally cool to after room temperature, filter the reactant liquor in water heating kettle, and repeatedly rinse with deionized water and ethanol the product leaching, then dry under 50 ℃ of vacuum, make nitrogen-doped graphene.
2. DSSC nitrogen-doping graphene counter electrode according to claim 1, is characterized in that: described by nitrogen-doped graphene film be cured to suprabasil method comprise lift, spin coating, drip be coated with, spraying or printing.
3. prepare the preparation method of DSSC nitrogen-doping graphene counter electrode as claimed in claim 1 or 2, it is characterized in that, comprise the steps:
3.1 adopt hydro thermal method to prepare nitrogen-doped graphene;
3.2 are distributed to the nitrogen-doped graphene preparing in solvent, by ultrasonic and stirring, form uniform and stable dispersion liquid; Described solvent is the mixture of a kind of or two kinds of arbitrary proportions in water, ethanol, isopropyl alcohol, n-butanol;
3.3 are preheated to 45 ~ 90 ℃ by substrate, then by dispersion liquid by lifting, spin coating, drip be coated with, the method for spraying or printing is evenly cured to substrate surface, and be dried 0.5 ~ 2 hour under vacuum condition, baking temperature is 50 ~ 300 ℃, makes DSSC nitrogen-doping graphene counter electrode;
In step 3.1, the concrete steps that described hydro thermal method is prepared nitrogen-doped graphene are:
1) 30 ~ 80mg graphene oxide is distributed in 100mL deionized water, ultrasonic dispersion 0.5 ~ 1 hour, adds ammoniacal liquor 1 ~ 2ml, regulator solution pH=10 ~ 11;
2) above-mentioned solution is put into the water heating kettle that is lined with polytetrafluoroethylene, at 100 ~ 200 ℃, hydro-thermal reaction 8 ~ 24 hours;
3) naturally cool to after room temperature, filter the reactant liquor in water heating kettle, and repeatedly rinse with deionized water and ethanol the product leaching, then dry under 50 ℃ of vacuum, make nitrogen-doped graphene.
4. the preparation method of DSSC nitrogen-doping graphene counter electrode according to claim 3, is characterized in that: in step 3.2, in described dispersion liquid, the concentration of nitrogen-doped graphene is 0.1-1.5mg/mL.
5. the preparation method of DSSC nitrogen-doping graphene counter electrode according to claim 3, is characterized in that: in step 3.2, in described dispersion liquid, the concentration of nitrogen-doped graphene is 0.3-1.2mg/mL.
6. the preparation method of DSSC nitrogen-doping graphene counter electrode according to claim 3, is characterized in that: in step 3.3, described baking temperature is 80 ~ 200 ℃.
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| CN102764724A (en) * | 2012-07-23 | 2012-11-07 | 贵州新碳高科有限责任公司 | Method for spraying graphene coat, and graphene coat prepared by same |
| CN104058388A (en) * | 2013-03-18 | 2014-09-24 | 海洋王照明科技股份有限公司 | Nitrogen-doped graphene film and preparation method thereof and capacitor |
| CN105006572A (en) * | 2014-04-22 | 2015-10-28 | 中国科学院苏州纳米技术与纳米仿生研究所 | Production method and application of nitrogen doped graphene dispersion film |
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| CN104108705B (en) * | 2014-07-11 | 2016-05-18 | 同济大学 | A kind of preparation method of nitrogen doping oriented graphite alkene |
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| CN104465113A (en) * | 2014-12-13 | 2015-03-25 | 天津理工大学 | Nitrogen-doped graphene counter electrode preparing method and application of nitrogen-doped graphene counter electrode in dye-sensitized solar cell |
| WO2017139983A1 (en) * | 2016-02-19 | 2017-08-24 | 肖丽芳 | Method for preparing positive electrode material having three-dimensional nitrogen-doped structure for use in lithium-sulfur battery |
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| CN110828186B (en) * | 2019-11-18 | 2021-09-28 | 黑龙江科技大学 | CeO (CeO)2Preparation method of modified nitrogen-doped graphene DSSC counter electrode |
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