CN104538190A - Preparation method of natural pigment sensitization titanium oxide and zinc oxide composite film solar cell - Google Patents

Preparation method of natural pigment sensitization titanium oxide and zinc oxide composite film solar cell Download PDF

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CN104538190A
CN104538190A CN201410768619.7A CN201410768619A CN104538190A CN 104538190 A CN104538190 A CN 104538190A CN 201410768619 A CN201410768619 A CN 201410768619A CN 104538190 A CN104538190 A CN 104538190A
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solar cell
tio
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preparation
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季惠明
王鸣婧
赵晓东
叶梦阳
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Tianjin University
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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
    • 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 invention relates to a preparation method of a natural pigment sensitization titanium oxide and zinc oxide composite film solar cell. A TiO2/ZnO composite film is prepared by a sol-gel method; a natural lycium ruthenicum pigment solution of 0.01-0.04 g/mL and a natural HEhuang carthamin yellow solution of 0.01-0.04 g/mL are prepared respectively and then are mixed to a natural pigment solution in an isopyknic mode; the TiO2/ZnO composite film is arranged in the natural pigment solution to be soaked for 6-24 hours, then is taken out, is washed with deionized water and is dried at 30-40 DEG C, and a photo-anode of the pigment sensitization solar cell is formed; the natural pigment sensitization TiO2/ZnO composite film serves as the photo-anode, a Pt sheet serves as a counter electrode, and the photo-anode, the counter electrode and a standard iodine-base electrolyte are assembled to be the pigment sensitization solar cell of a sandwich structure. The natural pigment sensitization titanium oxide and zinc oxide composite film solar cell has higher photovoltaic conversion efficiency of 1.2-3.1%, the synthetic method is simple, the preparation cost is low, and the application prospects are wide.

Description

The preparation method of natural colouring matter sensitization titanium oxide-zinc oxide composite film solar cell
Technical field
The present invention relates to a kind of preparation method of DSSC, particularly natural colouring matter sensitization TiO 2the preparation method of/ZnO laminated film solar cell; Improve the method for solar cell photoelectric conversion efficiency.
Background technology
Along with the development rapidly of economy, the problem of energy shortage becomes increasingly conspicuous.The gross energy that solar energy takes up an area ball exceedes nearly 9%, it is the clean energy resource that a kind of memory space is very abundant, have easy to use, inexhaustible, pollution-free, not by the feature such as regional impact and cheapness, become various countries scientist in recent years and utilized emphatically and one of new forms of energy of exploitation.Solar cell develops the most effective method of solar energy.Although the monocrystaline silicon solar cell of dominate has higher photoelectric conversion efficiency (>20%) in actual applications at present, cost of manufacture remains high, and is difficult to be applied in large-scale industrial production.Be only the 1/5-1/10 of silicon solar cell from the preparation cost of the DSSC (being called for short DSSCs) of the rise nineties in 20th century, and there is higher photoelectric conversion efficiency simultaneously, thus become the focus of research.
DSSC is by the film light anode of sensitization, redox electrolytes matter, form parts such as electrodes, mainly produce electronics by light anode absorb photons, light induced electron is transmitted by external circuit and forms electric current, and the selection of light anode material is to the performance impact of DSSC very large with preparation.TiO 2nano-crystal film is a kind of light anode material the most often used, and it has loose porous structure, is easy to adsorpting dye molecule, but electronics is at TiO 2migration rate in film is low, and electron-hole compound phenomenon easily occurs, and limits the further raising of DSSC photoelectric conversion efficiency.And TiO 2compare, ZnO has electron mobility and longer carrier lifetime faster.Can by ZnO and TiO 2compound, at TiO 2form the barrier layer of core shell structure between nanocrystalline and electrolyte, reduce due to TiO 2the electron-hole compound probability that electronics in film reacts with the redox couple be in the dye molecule of oxidation state and electrolyte solution and causes, thus the photoelectric conversion efficiency improving DSSC.
In addition, selecting of dye sensitizing agent is also very important, and its effect absorbs all band sunlight comprising visible light wave range, produces photoelectron, and by photoelectron transfer on semiconductive thin film conduction band.At present, the Ru-polypyridine organometallic complex dye sensitizing agent performance such as N3 dyestuff, N719 dyestuff and " black dyestuff " is best, but the technics comparing such as its synthesis, purification are complicated, and cost is also just corresponding higher, is unfavorable for that large-scale industrial production is applied.And natural dye distribution is wide, of a great variety, can directly extract from plant, pollution-free, without the need to loaded down with trivial details building-up process, separating-purifying process is relatively simple, be expected the absorption of sensitization realization to sunlight full band range by multiple natural dye, be suitable as the dye sensitizing agent of DSSC.
Summary of the invention
The object of this invention is to provide one natural colouring matter sensitization TiO 2the preparation method of the light anode of/ZnO laminated film solar cell.Concrete technology first adopts sol-gel process to prepare TiO 2/ ZnO laminated film, re-uses natural dye (Assessment of Pigment of Lycium ruthenicum Murr and river the Huangshui River carthamin yellow) and carries out sensitized treatment, be assembled into solar cell in this, as positive electrode.
Prepared DSSC preparation method is simple, preparation cost is cheap, has higher photoelectric conversion efficiency (1.2-3.1%), has a extensive future.
The present invention is achieved by the following technical solutions:
A kind of with natural colouring matter sensitization TiO 2the preparation method of the light anode of/ZnO laminated film solar cell; It is characterized in that first adopting sol-gel process to prepare TiO 2/ ZnO laminated film, re-uses natural dye and carries out sensitized treatment, be assembled into solar cell as positive electrode.
Described natural dye is Assessment of Pigment of Lycium ruthenicum Murr and river the Huangshui River carthamin yellow.
Natural colouring matter sensitization TiO 2the preparation method of the light anode of/ZnO laminated film solar cell, concrete steps are as follows:
(1) sol-gel process is adopted to prepare TiO 2/ ZnO laminated film;
(2) prepare 0.01g/mL-0.04g/mL natural Assessment of Pigment of Lycium ruthenicum Murr solution and natural river the Huangshui River carthamin yellow solution respectively, then equal-volume is mixed into natural colouring matter solution;
(3) by TiO 2/ ZnO laminated film is placed in natural colouring matter solution and soaks 6-24h, after spending deionized water, 30-40 DEG C of oven dry, forms dye-sensitized solar cell anode after getting;
(4) with natural colouring matter sensitization TiO 2/ ZnO laminated film is as light anode, and Pt sheet, as to electrode, is assembled into the DSSC of sandwich structure together with standard iodine-based electrolyte.
Be described as follows below:
TiO 2/ ZnO laminated film can adopt general method preparation, also can adopt with the following method:
(1) preparation of peroxo titanic acid sol:
(1) TiOSO of 0.15-0.25mol/L is prepared 4h 2o solution, the ammonia spirit of preparation 3mol/L, preparation 30wt.%H 2o 2solution;
(2) by Ti 4+with NH 4 +mol ratio is that ammoniacal liquor is instilled TiOSO by the ratio of 1:2-1:3 4h 2mix in O solution, mixture system pH value is controlled between for 6-8, constantly stir simultaneously and reactant is mixed, and generate white precipitate; (3) precipitation suction filtration that will be obtained, after spending deionized water three times, then adds deionized water and stirring and obtains white suspension;
(4) by Ti 4+and H 2o 2mol ratio be that the ratio of 1:3-1:5 is by H 2o 2in solution instillation white suspension, constantly stir after reactant is mixed, still aging 12-36h, obtains peroxo titanic acid sol.
(2) preparation of titania precursor body colloidal sol:
By the peroxo titanic acid sol of preparation, in reflux, in 80-100 DEG C of backflow 4-10h, obtain stable titania precursor body colloidal sol.
(3) preparation of zinc oxide precursor colloidal sol:
(1) ethanolic solution of the Zinc diacetate dihydrate of 0.18mol/L is prepared;
(2) add with zinc acetate equimolar diethanol amine in the solution, after mixing, fully stir in 50-80 DEG C of water-bath and obtain zinc oxide precursor colloidal sol.
(4) TiO 2the preparation of/ZnO laminated film:
(1) by FTO glass cleaning totally and dry, adopt Best-Effort request technique, titania precursor body colloidal sol is formed titanium oxide sol film in FTO substrate of glass;
(2), after titanium oxide sol film being dried at 80-100 DEG C, be warmed up to 450-550 DEG C with the speed of 2-3 DEG C/minute, be incubated 30 minutes, form the TiO of crystallization 2film;
(3) by TiO 2film cleaning totally and dry, adopts Best-Effort request technique, by zinc oxide precursor colloidal sol at TiO 2film is formed zinc oxide dissolved glue film;
(4), after zinc oxide dissolved glue film being dried at 80-100 DEG C, be warmed up to 250-350 DEG C with the speed of 2-3 DEG C/minute, be incubated 30 minutes, form the TiO of crystallization 2/ ZnO composite membrane;
(5) TiO will obtained 2/ ZnO composite membrane is substrate, repeats above (1)-(4) process 2-5 time, finally forms TiO 2/ ZnO laminated film.
(5) preparation of dye-sensitized solar cell anode and the assembling of battery:
(1) prepare 0.01g/mL-0.04g/mL natural Assessment of Pigment of Lycium ruthenicum Murr solution and natural river the Huangshui River carthamin yellow solution respectively, then equal-volume is mixed into natural colouring matter solution;
(2) by TiO 2/ ZnO laminated film is placed in natural colouring matter solution and soaks 6-24h, after spending deionized water 1-2 time, 30-40 DEG C of oven dry, forms dye-sensitized solar cell anode after getting;
(3) with natural colouring matter sensitization TiO 2/ ZnO laminated film is as light anode, and Pt sheet, as to electrode, is assembled into the DSSC of sandwich structure together with standard iodine-based electrolyte;
(5) at simulated solar illumination condition (AM 1.5G, 100mW cm -2) under test the I-V curve of solar cell, then calculate the photoelectric conversion efficiency of battery.
The DSSC prepared by above technology has higher photoelectric conversion efficiency (1.2-3.1%), and synthetic method is simple, preparation cost is cheap, has a extensive future.
Accompanying drawing explanation
Fig. 1: prepare TiO in embodiment 2 2the XRD collection of illustrative plates of/ZnO laminated film;
Fig. 2: prepare TiO in embodiment 2 2the SEM collection of illustrative plates of/ZnO laminated film.
Embodiment
Embodiment 1:
(1) preparation of peroxo titanic acid sol:
(1) 500mL 0.15mol/L TiOSO is prepared 4h 2o solution, the ammonia spirit of preparation 3mol/L, preparation 30wt.%H 2o 2solution;
(2) the ammoniacal liquor instillation TiOSO of 50mL is measured 4h 2mix in O solution, mixture system pH value is controlled between for 6-8, constantly stir simultaneously and reactant is mixed, and generate white precipitate;
(3) precipitation suction filtration that will be obtained, after spending deionized water three times, then adds deionized water and stirring and obtains white suspension;
(4) H of 34mL is measured 2o 2in solution instillation white suspension, constantly stir after reactant is mixed, still aging 12h, obtains peroxo titanic acid sol.
(2) preparation of titania precursor body colloidal sol:
By the peroxo titanic acid sol of preparation, in reflux, in 100 DEG C of backflow 4h, obtain stable titania precursor body colloidal sol
(3) preparation of zinc oxide colloidal sol:
(1) ethanolic solution of the Zinc diacetate dihydrate of 200mL 0.18mol/L is prepared;
(2) add with zinc acetate equimolar diethanol amine in the solution, more abundant stirring obtains zinc oxide precursor colloidal sol in 50 DEG C of water-baths.
(4) TiO 2the preparation of/ZnO laminated film:
(1) by FTO glass cleaning totally and dry, adopt Best-Effort request technique, titania precursor body colloidal sol is formed titanium oxide sol film in FTO substrate of glass;
(2), after titanium oxide sol film being dried at 80 DEG C, be warmed up to 450 DEG C with the speed of 3 DEG C/minute, be incubated 30 minutes, form the TiO of crystallization 2film;
(3) by TiO 2film cleaning totally and dry, adopts Best-Effort request technique, by zinc oxide precursor colloidal sol at TiO 2film is formed zinc oxide dissolved glue film;
(4), after zinc oxide dissolved glue film being dried at 80-100 DEG C, be warmed up to 250 DEG C with the speed of 3 DEG C/minute, be incubated 30 minutes, form the TiO of crystallization 2/ ZnO composite membrane.
(5) TiO will obtained 2/ ZnO composite membrane is substrate, repeats above (1)-(4) process 2 times, finally forms TiO 2/ ZnO laminated film.
(5) preparation of dye-sensitized solar cell anode and the assembling of battery
(1) prepare 0.01g/mL Assessment of Pigment of Lycium ruthenicum Murr solution and river the Huangshui River carthamin yellow solution respectively, then equal-volume is mixed into natural colouring matter solution;
(2) by TiO 2/ ZnO laminated film is placed in natural colouring matter solution and soaks 6h, after spending deionized water 1 time, 30 DEG C of oven dry, forms dye-sensitized solar cell anode after getting;
(3) with natural colouring matter sensitization TiO 2/ ZnO laminated film is as light anode, and Pt sheet, as to electrode, is assembled into the DSSC of sandwich structure together with standard iodine-based electrolyte;
(5) at simulated solar illumination condition (AM 1.5G, 100mW cm -2) under test the I-V curve of solar cell, then calculate the photoelectric conversion efficiency of battery, recording photoelectric conversion efficiency is 1.2%.
Embodiment 2:
(1) preparation of peroxo titanic acid sol:
(1) 500mL 0.2mol/L TiOSO is prepared 4h 2o solution, the ammonia spirit of preparation 3mol/L, preparation 30wt.%H 2o 2solution;
(2) the ammoniacal liquor instillation TiOSO of 67mL is measured 4h 2mix in O solution, mixture system pH value is controlled between for 6-8, constantly stir simultaneously and reactant is mixed, and generate white precipitate;
(3) precipitation suction filtration that will be obtained, after spending deionized water three times, then adds deionized water and stirring and obtains white suspension;
(4) H of 45mL is measured 2o 2in solution instillation white suspension, constantly stir after reactant is mixed, still aging 24h, obtains peroxo titanic acid sol.
(2) preparation of titania precursor body colloidal sol:
By the peroxo titanic acid sol of preparation, in reflux, in 90 DEG C of backflow 8h, obtain stable titania precursor body colloidal sol
(3) preparation of zinc oxide colloidal sol:
(1) ethanolic solution of the Zinc diacetate dihydrate of 200mL 0.18mol/L is prepared;
(2) add with zinc acetate equimolar diethanol amine in the solution, more abundant stirring obtains zinc oxide precursor colloidal sol in 60 DEG C of water-baths.
(4) TiO 2the preparation of/ZnO laminated film:
(1) by FTO glass cleaning totally and dry, adopt Best-Effort request technique, titania precursor body colloidal sol is formed titanium oxide sol film in FTO substrate of glass;
(2), after titanium oxide sol film being dried at 80 DEG C, be warmed up to 500 DEG C with the speed of 2 DEG C/minute, be incubated 30 minutes, form the TiO of crystallization 2film;
(3) by TiO 2film cleaning totally and dry, adopts Best-Effort request technique, by zinc oxide precursor colloidal sol at TiO 2film is formed zinc oxide dissolved glue film;
(4), after zinc oxide dissolved glue film being dried at 100 DEG C, be warmed up to 300 DEG C with the speed of 2 DEG C/minute, be incubated 30 minutes, form the TiO of crystallization 2/ ZnO composite membrane;
(5) TiO will obtained 2/ ZnO composite membrane is substrate, repeats above (1)-(4) process 3 times, finally forms TiO 2/ ZnO laminated film.
(5) preparation of dye-sensitized solar cell anode and the assembling of battery
(1) prepare 0.02g/mL Assessment of Pigment of Lycium ruthenicum Murr solution and river the Huangshui River carthamin yellow solution respectively, then equal-volume is mixed into natural colouring matter solution;
(2) by TiO 2/ ZnO laminated film is placed in natural colouring matter solution and soaks 12h, after spending deionized water 2 times, 40 DEG C of oven dry, forms dye-sensitized solar cell anode after getting;
(3) with natural colouring matter sensitization TiO 2/ ZnO laminated film is as light anode, and Pt sheet, as to electrode, is assembled into the DSSC of sandwich structure together with standard iodine-based electrolyte;
(5) at simulated solar illumination condition (AM 1.5G, 100mW cm -2) under test the I-V curve of solar cell, then calculate the photoelectric conversion efficiency of battery, recording photoelectric conversion efficiency is 3.1%.
Embodiment 3:
(1) preparation of peroxo titanic acid sol:
(1) 500mL 0.25mol/L TiOSO is prepared 4h 2o solution, the ammonia spirit of preparation 3mol/L, preparation 30wt.%H 2o 2solution;
(2) the ammoniacal liquor instillation TiOSO of 83mL is measured 4h 2mix in O solution, mixture system pH value is controlled between for 6-8, constantly stir simultaneously and reactant is mixed, and generate white precipitate;
(3) precipitation suction filtration that will be obtained, after spending deionized water three times, then adds deionized water and stirring and obtains white suspension;
(4) H of 57mL is measured 2o 2in solution instillation white suspension, constantly stir after reactant is mixed, still aging 36h, obtains peroxo titanic acid sol.
(2) preparation of titania precursor body colloidal sol:
By the peroxo titanic acid sol of preparation, in reflux, in 80 DEG C of backflow 10h, obtain stable titania precursor body colloidal sol
(3) preparation of zinc oxide colloidal sol:
(1) ethanolic solution of the Zinc diacetate dihydrate of 200mL 0.18mol/L is prepared;
(2) add with zinc acetate equimolar diethanol amine in the solution, more abundant stirring obtains zinc oxide precursor colloidal sol in 80 DEG C of water-baths.
(4) TiO 2the preparation of/ZnO laminated film:
(1) by FTO glass cleaning totally and dry, adopt Best-Effort request technique, titania precursor body colloidal sol is formed titanium oxide sol film in FTO substrate of glass;
(2), after titanium oxide sol film being dried at 80 DEG C, be warmed up to 550 DEG C with the speed of 3 DEG C/minute, be incubated 30 minutes, form the TiO of crystallization 2film;
(3) by TiO 2film cleaning totally and dry, adopts Best-Effort request technique, by zinc oxide precursor colloidal sol at TiO 2film is formed zinc oxide dissolved glue film;
(4), after zinc oxide dissolved glue film being dried at 100 DEG C, be warmed up to 350 DEG C with the speed of 3 DEG C/minute, be incubated 30 minutes, form the TiO of crystallization 2/ ZnO composite membrane;
(5) TiO will obtained 2/ ZnO composite membrane is substrate, repeats above (1)-(4) process 5 times, finally forms TiO 2/ ZnO laminated film.
(5) preparation of dye-sensitized solar cell anode and the assembling of battery
(1) prepare 0.04g/mL Assessment of Pigment of Lycium ruthenicum Murr solution and river the Huangshui River carthamin yellow solution respectively, then equal-volume is mixed into natural colouring matter solution;
(2) by TiO 2/ ZnO laminated film is placed in natural colouring matter solution and soaks 24h, after spending deionized water 2 times, 30 DEG C of oven dry, forms dye-sensitized solar cell anode after getting;
(3) with natural colouring matter sensitization TiO 2/ ZnO laminated film is as light anode, and Pt sheet, as to electrode, is assembled into the DSSC of sandwich structure together with standard iodine-based electrolyte;
(5) at simulated solar illumination condition (AM 1.5G, 100mW cm -2) under test the I-V curve of solar cell, then calculate the photoelectric conversion efficiency of battery, recording photoelectric conversion efficiency is 2.9%.
Embodiment 4:
(1) sol-gel process is adopted to prepare TiO 2/ ZnO laminated film;
(2) prepare 0.025g/mL natural Assessment of Pigment of Lycium ruthenicum Murr solution and natural river the Huangshui River carthamin yellow solution respectively, then equal-volume is mixed into natural colouring matter solution;
(3) by TiO 2/ ZnO laminated film is placed in natural colouring matter solution and soaks 12h, after spending deionized water 2 times, 340 DEG C of oven dry, forms dye-sensitized solar cell anode after getting;
(4) with natural colouring matter sensitization TiO 2/ ZnO laminated film is as light anode, and Pt sheet, as to electrode, is assembled into the DSSC of sandwich structure together with standard iodine-based electrolyte.
Under simulated solar illumination condition, recording photoelectric conversion efficiency is 2.8%.
Open and all methods that propose of the present invention and technology of preparing, those skilled in the art are by using for reference present disclosure, the links such as appropriate change raw material and process route realize, although method of the present invention and technology of preparing are described by preferred embodiment, person skilled obviously can change Method and Technology route as herein described or reconfigure not departing from content of the present invention, spirit and scope, realizes final technology of preparing.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are deemed to be included in spirit of the present invention, scope and content.

Claims (3)

1. the preparation method with natural colouring matter sensitization titanium oxide-zinc oxide composite film solar cell; It is characterized in that first adopting sol-gel process to prepare TiO 2/ ZnO laminated film, re-uses natural dye and carries out sensitized treatment, be assembled into solar cell as positive electrode.
2. the method for claim 1, is characterized in that described natural dye is Assessment of Pigment of Lycium ruthenicum Murr and river the Huangshui River carthamin yellow.
3. the method for claim 1, is characterized in that concrete steps are as follows:
(1) sol-gel process is adopted to prepare TiO 2/ ZnO laminated film;
(2) prepare 0.01g/mL-0.04g/mL natural Assessment of Pigment of Lycium ruthenicum Murr solution and natural river the Huangshui River carthamin yellow solution respectively, then equal-volume is mixed into natural colouring matter solution;
(3) by TiO 2/ ZnO laminated film is placed in natural colouring matter solution and soaks 6-24h, after spending deionized water, 30-40 DEG C of oven dry, forms dye-sensitized solar cell anode after getting;
(4) with natural colouring matter sensitization TiO 2/ ZnO laminated film is as light anode, and Pt sheet, as to electrode, is assembled into the DSSC of sandwich structure together with standard iodine-based electrolyte.
CN201410768619.7A 2014-12-12 2014-12-12 Preparation method of natural pigment sensitization titanium oxide and zinc oxide composite film solar cell Pending CN104538190A (en)

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