CN113436898A - Thin film electrode material for dye-sensitized solar cell and preparation method thereof - Google Patents
Thin film electrode material for dye-sensitized solar cell and preparation method thereof Download PDFInfo
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- Y02E10/00—Energy generation through renewable energy sources
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- Y02E10/542—Dye sensitized solar cells
Abstract
The invention relates to the technical field of functional materials, in particular to a thin film electrode material for a dye-sensitized solar cell and a preparation method thereof, wherein the thin film electrode material comprises the following steps: preparation of graphene oxide/Sb2S3Composite material-graphene oxide/Sb2S3And (2) grafting aniline on the composite material to obtain an intermediate, loading the intermediate on ITO conductive glass, and curing to obtain the thin film electrode material for the dye-sensitized solar cell. The method takes the graphene oxide as a core locus to realize the reaction with Sb2S3The polymerization of aniline is realized in the curing process, the thin film electrode material for the dye-sensitized solar cell is taken as a counter electrode, and Sb is added2S3And polyaniline to effect the promotion of the redox of the electrolyte solution.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a thin film electrode material for a dye-sensitized solar cell and a preparation method thereof.
Background
Energy is the driving force of social development, energy supply in the world at present mainly depends on fossil energy such as petroleum, natural gas, coal and the like, however, the problems of the limited fossil fuel energy, resource shortage caused by over exploitation and utilization, environmental pollution, ecological destruction and the like become bottlenecks which restrict the global economic and environmental coordination development. Therefore, development of green, clean and continuously renewable new energy is a common concern of scientists around the world. Among them, solar energy has incomparable advantages as renewable energy with abundant resources. The solar energy collector is clean, safe and efficient, low in utilization cost, free of geographic resource limitation and the like, so that the development and utilization of solar energy are concerned.
In the development process of solar cells, the preparation of new cheap materials and the simplification of the preparation process thereof have been the key points of research of scientists. Dye-sensitized solar cells (DSSCs) are a new generation of photovoltaic devices, having the advantages of clean, green and low cost, and their emergence has attracted much interest. So far, the service life of the dye-sensitized solar cell can reach 10 to 15 years, the dye-sensitized solar cell has good stability, and the photoelectric conversion efficiency of the cell is 13 percent higher, but the manufacturing cost of the dye-sensitized solar cell is only 1/5 to 1/10.
The dye-sensitized solar cell simulates the photosynthesis principle in plants in nature, adopts a nano-porous nanocrystalline film adsorbing dye as a photo-anode, selects a proper oxidation-reduction electrolyte and adopts platinized conductive glass as a counter electrode to realize the photoelectric conversion of the solar cell.
Among the components of DSSCs, the counter electrode is an important component of dye-sensitized solar cells, which accelerates I3 -/I-This reaction process requires that the counter electrode has ultrahigh effective specific surface area, excellent conductivity, high chemical stability, and relatively high catalytic activity for electrolyte redox, and at present, although platinum counter electrodes are widely used in dye-sensitized solar cells due to their excellent conductivity and high catalytic reduction activity, the scarce platinum counter electrodes themselves are very expensive, and some documents report that platinum causes catalyst poisoning in the cells, so it is necessary to prepare a suitable counter electrode material to replace the platinum counter electrodes.
The carbon material has been a research hotspot in this direction, mainly because the carbon counter electrode has the advantages of corrosion resistance, low cost, high catalytic activity and the like, and meanwhile, the carbon material has good conductivity, electrocatalytic activity and dual stability of chemistry and heat, in recent years, graphene has attracted research interest of academic circles, and there are many related reports (ACS Nano,2010,4, 6203; ACS Nano,2011,5,165) in the aspect of DSSCs counter electrodes.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a thin film electrode material for a dye-sensitized solar cell and a preparation method thereof2S3And grafting with aniline and passing Sb2S3And polyaniline to promote the redox of the electrolyte.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a thin film electrode material for a dye-sensitized solar cell comprises the following steps:
(1) cleaning and cutting the ITO conductive glass to obtain standby conductive glass;
(2) preparation of graphene oxide/Sb2S3A composite material;
ultrasonically dispersing graphene oxide in ethylene glycol to obtain a clear solution, and then adding SbCl3Uniformly mixing polyvinylpyrrolidone and thiourea, reacting for 9-12h at the temperature of 100-120 ℃ in a reaction kettle, centrifuging, washing and drying in vacuum to obtain the graphene oxide/Sb2S3A composite material;
wherein, the graphene oxide and SbCl3The mass ratio of (1: 150-); SbCl3The mass ratio of polyvinylpyrrolidone to thiourea was 1: 1-1.5: 3-4;
(3) preparation of an intermediate:
mixing the graphene oxide/Sb obtained in the step (2)2S3After the composite material is mixed with hydrochloric acid solution of aniline, dropwise adding hydrochloric acid solution of ammonium persulfate into the mixture, and stirring the mixture for reaction for 1 to 2 hours at room temperature in argon atmosphere to obtain an intermediate;
wherein, the graphene oxide/Sb2S3The ratio of the mass of the composite material, the volume of the hydrochloric acid solution of aniline to the volume of the hydrochloric acid solution of ammonium persulfate is 0.5 g: 8-10 mL: 10-13 mL;
(4) preparing a thin film electrode material:
s1, preparing a triton aqueous solution with the volume fraction of 20-25%;
s2, grinding the intermediate in the step (3), adding the ground intermediate into the water solution of Triton in the step S1, ultrasonically dispersing the ground intermediate to form a suspension, depositing the suspension on the surface of the ITO conductive glass in the step (1) and forming a film to obtain film-coated conductive glass;
s3, curing the film-coated conductive glass obtained in the step S2 at the temperature of 190-220 ℃ for 2-2.5h in an argon atmosphere to obtain the film electrode material for the dye-sensitized solar cell.
Preferably, the method for cleaning the ITO conductive glass in step (1) comprises: h with the mass fraction of 70 percent is adopted in sequence2SO4And washing the ITO glass for 10-20min by using the solution, deionized water and acetone, and drying.
Preferably, the graphene oxide in the step (2) is prepared by using a modified Hummer's method.
Preferably, the hydrochloric acid solution of aniline in step (3) is prepared from aniline and 25% by volume hydrochloric acid solution, and the volume ratio of aniline to hydrochloric acid solution is 2-3: 100.
preferably, the hydrochloric acid solution of ammonium persulfate in the step (3) is prepared from ammonium persulfate and a hydrochloric acid solution with a volume fraction of 25%, and the mass ratio of the ammonium persulfate to the volume of the hydrochloric acid solution is 4-6 g: 100 mL.
The invention also provides the thin film electrode material for the dye-sensitized solar cell, which is prepared by the preparation method of the thin film electrode material for the dye-sensitized solar cell.
Compared with the prior art, the invention has the beneficial effects that:
1、Sb2S3is an important V-VI type semiconductor material, Sb2S3The invention realizes Sb through the support material-graphene oxide by expanding the spectrum absorption range to the visible light region with obvious absorption coefficient and relatively narrow forbidden bandwidth in the visible light region, thereby being beneficial to the utilization of natural light2S3Compounding with graphene oxide, using graphene oxide as a core site, which is in one aspect with Sb2S3Compounding to prepare the graphene oxide/Sb2S3On the other hand, carboxyl carried by graphene oxide can guide aniline to graft, aniline chains are wrapped on the surface of the graphene oxide in a combined winding manner through pi bonds and amine ester bonds, and then aniline polymerization is realized in the curing process to prepare polyaniline.
2. Compared with the prior art which takes the graphene oxide as the main raw material, the method takes a small amount of the graphene oxide as the core locus to realize Sb2S3The grafting of aniline and the coating of polyaniline, in which case, Sb2S3The material is coated in the polyaniline material, and the defect of opaqueness of a small amount of graphene oxide to the whole film electrode material is improved, and the defect of tight packing caused by using a large amount of graphene oxide is overcome.
Drawings
FIG. 1 is an SEM image of a thin film electrode material prepared in example 1 of the present invention;
FIG. 2 is a IV curve of a dye-sensitized solar cell constructed by a thin film counter electrode prepared in example 1 of the present invention;
fig. 3 is an IV curve of a dye-sensitized solar cell constructed with a platinum counter electrode.
Detailed Description
The following detailed description of specific embodiments of the invention is provided, but it should be understood that the scope of the invention is not limited to the specific embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. The experimental methods described in the examples of the present invention are all conventional methods unless otherwise specified.
Example 1
A preparation method of a thin film electrode material for a dye-sensitized solar cell comprises the following steps:
(1) cleaning ITO conductive glass, cutting to 1cm multiplied by 3cm, and sequentially adopting H with the mass fraction of 70%2SO4Washing the ITO glass with the solution, deionized water and acetone for 10min, and drying to obtain standby conductive glass;
(2) preparation of graphene oxide/Sb2S3A composite material;
ultrasonically dispersing graphene oxide in ethylene glycol to obtain a clear solution, and then adding SbCl3Uniformly mixing polyvinylpyrrolidone and thiourea, reacting for 12h at 100 ℃ in a reaction kettle, centrifuging, washing and drying in vacuum to obtain the graphene oxide/Sb2S3A composite material;
wherein, the graphene oxide and SbCl3The mass ratio of (A) to (B) is 1: 200; SbCl3The mass ratio of polyvinylpyrrolidone to thiourea was 1: 1.2: 3.5;
(3) preparation of an intermediate:
mixing the graphene oxide/Sb obtained in the step (2)2S3After the composite material is mixed with hydrochloric acid solution of aniline, dropwise adding hydrochloric acid solution of ammonium persulfate into the mixture, and stirring the mixture for reaction for 1 hour at room temperature in argon atmosphere to obtain an intermediate;
wherein, the graphene oxide/Sb2S3The ratio of the mass of the composite material, the volume of the hydrochloric acid solution of aniline to the volume of the hydrochloric acid solution of ammonium persulfate is 0.5 g: 8mL of: 11 mL;
the hydrochloric acid solution of aniline is prepared from aniline and hydrochloric acid solution with the volume fraction of 25%, and the volume ratio of aniline to hydrochloric acid solution is 2: 100, respectively;
the hydrochloric acid solution of the ammonium persulfate is prepared from the ammonium persulfate and a hydrochloric acid solution with the volume fraction of 25%, and the mass ratio of the ammonium persulfate to the volume of the hydrochloric acid solution is 6 g: 100 mL;
(4) preparing a thin film electrode material:
s1, preparing a 20 volume percent water solution of Triton;
s2, grinding the intermediate in the step (3), adding the ground intermediate into the water solution of Triton in the step S1, ultrasonically dispersing the ground intermediate to form a suspension, depositing the suspension on the surface of the ITO conductive glass in the step (1) and forming a film to obtain film-coated conductive glass;
and S3, curing the film-coated conductive glass obtained in the step S2 at 190 ℃ for 2.5 hours in an argon atmosphere to obtain the film electrode material for the dye-sensitized solar cell.
The obtained thin film electrode material is used as a counter electrode to assemble a dye-sensitized solar cell, and the short-circuit current, the open-circuit voltage, the filling factor and the conversion efficiency of the dye-sensitized solar cell are respectively 15.07mA/cm20.722V, 0.676 and 7.35%, corresponding IV curves are shown in fig. 2; the conversion efficiency of the dye-sensitized solar cell assembled by the thin-film electrode material counter electrode is slightly higher than that of the dye-sensitized solar cell assembled by the platinum counter electrode under the same condition, and the short-circuit current, the open-circuit voltage, the filling factor and the conversion efficiency of the dye-sensitized solar cell assembled by the platinum counter electrode are 14.45mA/cm respectively20.696V, 0.701 and 7.05%, the corresponding IV curves are shown in fig. 3.
Example 2
A preparation method of a thin film electrode material for a dye-sensitized solar cell comprises the following steps:
(1) cleaning ITO conductive glass, cutting to 2cm multiplied by 2cm, and sequentially adopting 70% H by mass fraction2SO4Washing the ITO glass with the solution, deionized water and acetone for 15min, and drying to obtain standby conductive glass;
(2) preparation of graphene oxide/Sb2S3A composite material;
ultrasonically dispersing graphene oxide in ethylene glycol to obtain a clear solution, and then adding SbCl3Uniformly mixing polyvinylpyrrolidone and thiourea, reacting for 10 hours at 110 ℃ in a reaction kettle, centrifuging, washing and drying in vacuum to obtain the graphene oxide/Sb2S3A composite material;
wherein, the graphene oxide and SbCl3The mass ratio of (A) to (B) is 1: 150; SbCl3The mass ratio of polyvinylpyrrolidone to thiourea was 1: 1.5: 3;
(3) preparation of an intermediate:
mixing the graphene oxide/Sb obtained in the step (2)2S3After the composite material is mixed with hydrochloric acid solution of aniline, dropwise adding hydrochloric acid solution of ammonium persulfate into the mixture, and stirring the mixture for reaction for 1.5 hours at room temperature in argon atmosphere to obtain an intermediate;
wherein, the graphene oxide/Sb2S3The ratio of the mass of the composite material, the volume of the hydrochloric acid solution of aniline to the volume of the hydrochloric acid solution of ammonium persulfate is 0.5 g: 9mL of: 10 mL;
the hydrochloric acid solution of aniline is prepared from aniline and hydrochloric acid solution with the volume fraction of 25%, and the volume ratio of aniline to hydrochloric acid solution is 2.5: 100, respectively;
the hydrochloric acid solution of the ammonium persulfate is prepared from the ammonium persulfate and a hydrochloric acid solution with the volume fraction of 25%, and the mass ratio of the ammonium persulfate to the volume of the hydrochloric acid solution is 5 g: 100 mL;
(4) preparing a thin film electrode material:
s1, preparing a 23% volume fraction of water solution of Triton;
s2, grinding the intermediate in the step (3), adding the ground intermediate into the water solution of Triton in the step S1, ultrasonically dispersing the ground intermediate to form a suspension, depositing the suspension on the surface of the ITO conductive glass in the step (1) and forming a film to obtain film-coated conductive glass;
and S3, curing the film-coated conductive glass obtained in the step S2 at 220 ℃ for 2 hours in an argon atmosphere to obtain the film electrode material for the dye-sensitized solar cell.
Example 3
A preparation method of a thin film electrode material for a dye-sensitized solar cell comprises the following steps:
(1) cleaning ITO conductive glass, cutting to 3cm multiplied by 3cm, and sequentially adopting H with the mass fraction of 70%2SO4ITO glass washed by solution, deionized water and acetoneDrying after 20min to obtain standby conductive glass;
(2) preparation of graphene oxide/Sb2S3A composite material;
ultrasonically dispersing graphene oxide in ethylene glycol to obtain a clear solution, and then adding SbCl3Uniformly mixing polyvinylpyrrolidone and thiourea, reacting for 9 hours at 120 ℃ in a reaction kettle, centrifuging, washing and drying in vacuum to obtain the graphene oxide/Sb2S3A composite material;
wherein, the graphene oxide and SbCl3The mass ratio of (1: 150-); SbCl3The mass ratio of polyvinylpyrrolidone to thiourea was 1: 1: 4;
(3) preparation of an intermediate:
mixing the graphene oxide/Sb obtained in the step (2)2S3After the composite material is mixed with hydrochloric acid solution of aniline, dropwise adding hydrochloric acid solution of ammonium persulfate into the mixture, and stirring the mixture for reaction for 2 hours at room temperature in argon atmosphere to obtain an intermediate;
wherein, the graphene oxide/Sb2S3The ratio of the mass of the composite material, the volume of the hydrochloric acid solution of aniline to the volume of the hydrochloric acid solution of ammonium persulfate is 0.5 g: 10mL of: 13 mL;
the hydrochloric acid solution of aniline is prepared from aniline and hydrochloric acid solution with the volume fraction of 25%, and the volume ratio of aniline to hydrochloric acid solution is 3: 100, respectively;
the hydrochloric acid solution of the ammonium persulfate is prepared from the ammonium persulfate and a hydrochloric acid solution with the volume fraction of 25%, and the mass ratio of the ammonium persulfate to the volume of the hydrochloric acid solution is 4 g: 100 mL;
(4) preparing a thin film electrode material:
s1, preparing a 25% triton water solution by volume fraction;
s2, grinding the intermediate in the step (3), adding the ground intermediate into the water solution of Triton in the step S1, ultrasonically dispersing the ground intermediate to form a suspension, depositing the suspension on the surface of the ITO conductive glass in the step (1) and forming a film to obtain film-coated conductive glass;
and S3, curing the film-coated conductive glass obtained in the step S2 at 200 ℃ for 2.5 hours in an argon atmosphere to obtain the film electrode material for the dye-sensitized solar cell.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (6)
1. A preparation method of a thin film electrode material for a dye-sensitized solar cell is characterized by comprising the following steps:
(1) cleaning and cutting the ITO conductive glass to obtain standby conductive glass;
(2) preparation of graphene oxide/Sb2S3A composite material;
ultrasonically dispersing graphene oxide in ethylene glycol to obtain a clear solution, and then adding SbCl3Uniformly mixing polyvinylpyrrolidone and thiourea, reacting for 9-12h at the temperature of 100-120 ℃ in a reaction kettle, centrifuging, washing and drying in vacuum to obtain the graphene oxide/Sb2S3A composite material;
wherein, the graphene oxide and SbCl3The mass ratio of (1: 150-); SbCl3The mass ratio of polyvinylpyrrolidone to thiourea was 1: 1-1.5: 3-4;
(3) preparation of an intermediate:
mixing the graphene oxide/Sb obtained in the step (2)2S3After the composite material is mixed with hydrochloric acid solution of aniline, dropwise adding hydrochloric acid solution of ammonium persulfate into the mixture, and stirring the mixture for reaction for 1 to 2 hours at room temperature in argon atmosphere to obtain an intermediate;
wherein, the graphene oxide/Sb2S3The ratio of the mass of the composite material, the volume of the hydrochloric acid solution of aniline to the volume of the hydrochloric acid solution of ammonium persulfate is 0.5 g: 8-10 mL: 10-13 mL;
(4) preparing a thin film electrode material:
s1, preparing a triton aqueous solution with the volume fraction of 20-25%;
s2, grinding the intermediate in the step (3), adding the ground intermediate into the water solution of Triton in the step S1, ultrasonically dispersing the ground intermediate to form a suspension, depositing the suspension on the surface of the ITO conductive glass in the step (1) and forming a film to obtain film-coated conductive glass;
s3, curing the film-coated conductive glass obtained in the step S2 at the temperature of 190-220 ℃ for 2-2.5h in an argon atmosphere to obtain the film electrode material for the dye-sensitized solar cell.
2. The method for preparing the thin film electrode material for the dye-sensitized solar cell according to claim 1, wherein the method for cleaning the ITO conductive glass in the step (1) comprises the following steps: h with the mass fraction of 70 percent is adopted in sequence2SO4And washing the ITO glass for 10-20min by using the solution, deionized water and acetone, and drying.
3. The method for preparing the thin film electrode material for the dye-sensitized solar cell according to claim 1, wherein the graphene oxide obtained in the step (2) is prepared by using a modified Hummer's method.
4. The method for preparing a thin film electrode material for a dye-sensitized solar cell according to claim 1, wherein the hydrochloric acid solution of aniline of step (3) is prepared from aniline and 25% by volume hydrochloric acid solution, and the volume ratio of aniline to hydrochloric acid solution is 2-3: 100.
5. the method for preparing the thin-film electrode material for the dye-sensitized solar cell according to claim 1, wherein the hydrochloric acid solution of ammonium persulfate in the step (3) is prepared from ammonium persulfate and a hydrochloric acid solution with a volume fraction of 25%, and the mass ratio of the ammonium persulfate to the volume of the hydrochloric acid solution is 4-6 g: 100 mL.
6. A thin film electrode material for dye-sensitized solar cells, which is prepared by the method for preparing the thin film electrode material for dye-sensitized solar cells according to any one of claims 1 to 5.
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