CN102280264B - Titanium/strontium covered nanocrystalline titanium dioxide film for dye-sensitized solar cell and preparation method thereof - Google Patents
Titanium/strontium covered nanocrystalline titanium dioxide film for dye-sensitized solar cell and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a titanium/strontium covered nanocrystalline titanium dioxide film for a dye-sensitized solar cell and a preparation method thereof. The titanium/strontium dual-layer covered nanocrystalline titanium dioxide film is prepared by adding strontium acetate and titanium tetrachloride solution to untreated nanocrystalline titanium dioxide film by way of impregnating. The titanium dioxide film and the preparation method have the following beneficial effects: the semiconductor film effectively prolongs the lives of charges and reduces the probability of charge recombination so that the interfacial charge transfer efficiency is improved; the film is adopted to package the dye-sensitized solar cell and test the performances of the dye-sensitized solar cell; the short-circuit photocurrent, open-circuit photovoltage and energy conversion efficiency of the cell are substantially improved; and the preparation method has obvious advantages compared with the conventional TiCl4 treatment methods.
Description
Technical field
The invention belongs to inorganic field of photovoltaic materials, particularly a kind of preparation method who is used for the titanium/strontium clad nano crystal titanium dioxide film of DSSC.
Background technology
Since professor Grate1 in 1991 introduces dye sensitization broad stopband TiO with the notion of nanoporous
2In the semiconducter research; Obtain the DSSC (Dye-Sensitized Solar Cell of energy conversion efficiency 7.1%; DSSC) since, the DSSC battery has won people's extensive attention with advantages such as its potential low cost, simple relatively manufacture craft and technology, performance are stable.This battery is adsorbed onto nanoporous TiO through the multi-pyridine ligand dyestuff by ruthenium (II)
2On thin film semiconductor's electrode surface, utilize the strong absorption of dyestuff, can semi-conductive spectral response be widened the visual field, thereby obtain desirable energy conversion efficiency visible light.Reached 10% energy conversion efficiency in 1993, and in calendar year 2001 and 2004, battery efficiency reached 10.4% and 11.04%, its conversion efficiency can compare favourably with amorphous silicon solar cell, and manufacturing cost is merely 1/10 ~ 1/5 of solar cell.
The semiconductor of nanostructure through a large amount of monolayer dye molecule of its huge surface area absorption, has improved the collection efficiency of sunlight in solar cell; Nano semiconductor will be transferred to passive electrode from the dye molecule injected electrons simultaneously; Yet the huge surface area of semi-conducting electrode has also increased the charge recombination of electrode surface; Thereby reduce the photoelectric conversion efficiency of solar cell; In order to improve the photovoltaic performance of battery, people have developed multiple physical chemistry modifying technology and have improved nano-TiO
2Characteristic of electrode, these technology comprise TiCl
4Surface treatment, surface coating, doping etc.; Wherein the surface coating is a kind of up-and-coming method; The surface coat to rely on has the semiconductor of higher conduction band position or barrier layer that insulating barrier forms so-called nucleocapsid structure is reduced compound; Can significantly improve injection, transfer efficiency and the transmission performance of nanocrystalline titanium dioxide film, at present the research that titanium/strontium double-coated nanocrystalline titanium dioxide film is used in DSSC also not reported.
Summary of the invention
The technical problem that the present invention will solve provides the preparation method of the nano-crystalline titanium dioxide film of a kind of titanium/strontium coating, uses short-circuit photocurrent, open circuit photovoltage and the ability of this film as the DSSC of electrode material assembling
Parameters and conventional TiCl such as amount transformation efficiency
4Processing method has been compared significantly and has been improved.
For solving the problems of the technologies described above; The technical scheme that the present invention adopts is: the nano-crystalline titanium dioxide film that a kind of titanium/strontium coats; It is characterized in that described nano-crystalline titanium dioxide is a Detitanium-ore-type; Its particle diameter scope is 20～30 nm, and thin-film material is colorless and transparent film or shallow white film.
In addition, the preparation method of the nano-crystalline titanium dioxide film of titanium of the present invention/strontium coating carries out according to following steps:
(1), the preparation of nano-crystalline titanium dioxide film:
Under strong agitation, a certain amount of tetraisopropyl titanate (TTIP) is slowly joined in the appropriate amount of deionized water, continue to stir 1 ~ 4 h, the sediment that obtains is carried out suction filtration and washing; Subsequently sediment is made into the TTIP of certain volume ratio and the mixed solution of TMAH (TMAH); Add the deionized water constant volume; Then powerful stirring reaction 1 ~ 5 h in 100 ~ 150 ℃ of oil baths naturally cools to room temperature, and the white colloid that obtains after reaction is accomplished is transferred in the autoclave and constant volume; Hydrothermal treatment consists 6 ~ 24 h under 150 ~ 300 ℃ condition take out behind the natural cooling and carry out sonicated 20 min, obtain milky TiO 2 sol; On clean conductive glass, form thin film through method for printing screen; Dried film is put into Muffle furnace, and temperature slowly is warming up to 450 ~ 550 ℃, constant temperature 0.5 ~ 10 h; Naturally cool to room temperature, promptly obtain undressed nano-crystalline titanium dioxide film;
(2), the preparation of titanium tetrachloride solution:
A certain amount of titanium tetrachloride is joined in the dropping funel; Be communicated with nitrogen with the glass dropper, insert the dropping funel top, blow 1 ~ 15 min with nitrogen; Under the condition of ice bath titanium tetrachloride after the above-mentioned processing is joined in the deionized water; On magnetic stirring apparatus, fully stir 30 min under the normal temperature, constant volume is to 100 mL then, and promptly obtaining molar concentration is the titanium tetrachloride colourless transparent solution of 0.005 ~ 4 mol/L;
(3), the preparation of strontium acetate solution:
A certain amount of strontium acetate is joined in the appropriate amount of deionized water, on magnetic stirring apparatus, fully stir 30 min under the normal temperature, constant volume is to 100 mL then, and promptly obtaining molar concentration is the strontium acetate colourless transparent solution of 0.001 ~ 2 mol/L;
(4), the preparation of the nanocrystalline titanium dioxide film of titanium/strontium coating:
With the method for the film behind the sintering in the step (1) through dipping, be immersed in the described strontium acetate solution of step (3) the inside earlier, in 30 ~ 90 ℃ of solution, dipping 0.3 ~ 1 h; With nitrogen moisture is blown away subsequently, then film is put into Muffle furnace, slowly be warming up to 400 ~ 550 ℃, constant temperature 0.5 ~ 10 h; Naturally cool to room temperature, and then with the solution the inside of the film immersion that obtains at the described titanium tetrachloride of step (2), in 30 ~ 90 ℃ of solution, dipping 0.3 ~ 1h; With nitrogen moisture is blown away subsequently, then film is put into Muffle furnace, slowly be warming up to 400 ~ 550 ℃; Constant temperature 0.5 ~ 10 h naturally cools to room temperature, promptly obtains handling through strontium acetate earlier; Handle through titanium tetrachloride again, form the internal layer strontium titanates, the duplicature of outer titanium dioxide (being called for short Ti-Sr-Ti) on the nano-crystalline titanium dioxide film surface; Perhaps, be immersed in the described titanium tetrachloride solution of step (2) the inside earlier with the method for the film behind the sintering in the step (1) through dipping, in 30 ~ 90 ℃ of solution, dipping 0.3 ~ 1 h; With nitrogen moisture is blown away subsequently, then film is put into Muffle furnace, slowly be warming up to 400 ~ 550 ℃, constant temperature 0.5 ~ 10 h; Naturally cool to room temperature, and then be immersed in the described strontium acetate solution of step (3) the inside, in 30 ~ 90 ℃ of solution, dipping 0.3 ~ 1 h; With nitrogen moisture is blown away subsequently, then film is put into Muffle furnace, slowly be warming up to 400 ~ 550 ℃; Constant temperature 0.5 ~ 10 h naturally cools to room temperature, promptly obtains handling through titanium tetrachloride earlier; Soak the peracetic acid strontium again and handle, form internal layer titanium dioxide, the duplicature of outer strontium titanates (being called for short Ti-Ti-Sr) on the nano-crystalline titanium dioxide film surface.
Titanium/strontium double-coated the nano-crystalline titanium dioxide film of the present invention preparation as electrode material, according to standard method assembling DSSC, is recorded each performance parameter of DSSC under the AM1.5 simulated solar irradiation.In the prepared cell device, the short-circuit photocurrent of battery, open circuit photovoltage and energy conversion efficiency all have significantly raising, with the TiCl of routine
4Processing method is compared has remarkable advantages; Open circuit photovoltage in the dye-sensitized nanocrystalline titanium dioxide raises; Electron lifetime is significantly improved; Explain that the electron recombination in the nanocrystalline titanium dioxide film has obtained effective inhibition, make the interface charge transfer efficiency be improved, thereby increased substantially the energy conversion efficiency of DSSC.
Description of drawings
Fig. 1 is the nano-crystalline titanium dioxide film X ray of titanium/strontium coating of embodiment of the invention 4-7 preparation
Diffraction spectra;
Fig. 2 is photoelectric current-photovoltage (I-V) collection of illustrative plates of the DSSC assembled among the embodiment of the invention 4-7.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed explanation.
Embodiment 1: without the preparation of the nano-crystalline titanium dioxide film (Ti) of any processing
Under strong agitation, 14 g tetraisopropyl titanates slowly are added drop-wise in the 50 mL deionized waters, continue stirring reaction 2 h, the adularescent deposition generates.The white precipitate that generates is carried out suction filtration and washing, obtain titanium dioxide moist precipitate 24 g, moist precipitate is transferred in the there-necked flask, slowly drip tetramethylammonium hydroxide aqueous solution 3.65 g, it is 40 g that the adding deionized water is adjusted to gross mass.Powerful stirring reaction 3 h naturally cool to room temperature in 120 ℃ of oil baths, will react completion
After the white colloid that obtains be adjusted to 50 mL and be transferred in the 100 mL autoclaves hydrothermal treatment consists 8 h under 220 ℃ condition.Take out behind the natural cooling and carry out sonicated 20 min, obtain milky TiO 2 sol, on clean conductive glass, form one deck sol pellicle through silk screen printing.Dried film is put into Muffle furnace, slowly be warming up to 450 ℃, be incubated 2 h, naturally cool to room temperature, promptly obtain undressed nano-crystalline titanium dioxide film (Ti).
The preparation of the titanium tetrachloride solution of embodiment 2:2 mol/L
Take by weighing 38 g titanium tetrachlorides and add in the dropping funel, be communicated with nitrogen, insert the dropping funel top with the glass dropper; Blow 5 min with nitrogen, titanium tetrachloride dropwise is dissolved in (in the ice bath) in the beaker that fills 50 mL deionized waters, powerful 30 min that stir on magnetic stirring apparatus; Mixed solution is a colourless transparent solution, then solution is transferred in the volumetric flask gradually, adds deionized water; Make cumulative volume reach 100 mL, promptly get the titanium tetrachloride solution that concentration is 2 mol/L.
The preparation of the strontium acetate solution of embodiment 3:1 mol/L
Take by weighing the strontium acetate of 21.47 g, add 70 mL water, normal temperature stirs 30 min down, is transferred to then in the 100 mL volumetric flasks, is settled to 100 mL with deionized water, and promptly getting concentration is the strontium acetate solution of 1 mol/L.
Embodiment 4: the nano-crystalline titanium dioxide film of any special processing (Ti) not
Film among the embodiment 1 is placed surface plate, to wherein adding 20 ml deionized waters, 70 ℃; Take out behind the 30min, dry up with nitrogen and put into Muffle furnace, temperature slowly is warming up to 450 ℃; Be incubated 2 h, naturally cool to room temperature, promptly obtain the nanocrystalline titanium dioxide film of not any processing.Film characterizes through X-ray diffractometer and finds that shown in accompanying drawing 1, prepared titanium dioxide nanocrystalline is an anatase crystal.
Embodiment 5: the preparation of the nano-crystalline titanium dioxide film of handling through titanium tetrachloride (Ti-Ti)
Film among the embodiment 1 is placed surface plate, previous to wherein adding through the liquid among full and uniform 19.5 ml deionized waters and the 0.5 mL embodiment 2,70 ℃; Take out behind 30 min; Dry up with nitrogen and to put into Muffle furnace, temperature slowly is warming up to 450 ℃, is incubated 2 h; Naturally cool to room temperature, promptly obtain the nano-crystalline titanium dioxide film that titanium tetrachloride is handled.Film characterizes through X-ray diffractometer and finds that shown in accompanying drawing 1, prepared nano-crystalline titanium dioxide is an anatase crystal.
Embodiment 6: handle through strontium acetate earlier, the preparation of the nano-crystalline titanium dioxide film (Ti-Sr-Ti) of process titanium tetrachloride processing again
Film among the embodiment 1 is placed surface plate, previous to wherein adding through the liquid among full and uniform 39.5 ml deionized waters and the 0.5 mL embodiment 3,70 ℃; Take out behind 30 min, dry up with nitrogen and put into Muffle furnace, temperature slowly is warming up to 525 ℃; Be incubated 2 h, naturally cool to room temperature, promptly obtain the nano-crystalline titanium dioxide film (Ti-Sr) that strontium acetate is handled; (Ti-Sr) places surface plate with the nano-crystalline titanium dioxide film that obtains, to wherein adding earlier
Preceding through the liquid among full and uniform 19.5 ml deionized waters and the 0.5 mL embodiment 2,70 ℃, take out behind 30 min; Dry up with nitrogen and to put into Muffle furnace; Temperature slowly is warming up to 450 ℃, is incubated 2 h, naturally cools to room temperature; Form internal layer strontium carbonate, the duplicature of outer titanium dioxide at last on the surface.Film characterizes through X-ray diffractometer and finds that shown in accompanying drawing 1, prepared nano-crystalline titanium dioxide is an anatase crystal.
Embodiment 7: handle through titanium tetrachloride earlier, soak the preparation of the titanium dioxide film (Ti-Ti – Sr) of peracetic acid strontium processing again
Film among the embodiment 5 is placed surface plate, previous to wherein adding through the liquid among full and uniform 39.5 ml deionized waters and the 0.5 mL embodiment 3,70 ℃; Take out behind 30 min, dry up with nitrogen and put into Muffle furnace, temperature slowly is warming up to 525 ℃; Be incubated 2 h; Naturally cool to room temperature, promptly obtain forming internal layer titanium dioxide, the duplicature of outer strontium carbonate.Film characterizes through X-ray diffractometer and finds that shown in accompanying drawing 1, prepared titanium dioxide nanocrystalline is an anatase crystal.
The nano-crystalline titanium dioxide film that utilizes embodiment 4～7 preparations is according to existing standard method assembling dye-sensitized solar cells; Wherein dyestuff adopts N719; Electrolyte 0.1 mol/L LiI/0.05 mol/L I2/0.5 mol/L/ is to tert .-butylpyridine/0.6 mol/L iodo 1; The methoxy propyl cyanogen solution of 2-dimethyl-3-n-pro-pyl imidazoles is platinum to electrode, and cell area is 0.2304 cm
2, thickness 4.49 μ m.Under the AM1.5 simulated solar irradiation, record photoelectric current-photovoltage (I-V) curve of DSSC; The performance parameter of battery comprises open circuit photovoltage (Voc), short-circuit photocurrent (Jsc), fill factor, curve factor (FF) and energy conversion efficiency (η), like table 1 and shown in Figure 2.
The parameter measurement table of table 1 DSSC
Claims (1)
1. the preparation method of the nano-crystalline titanium dioxide film that coats of a titanium/strontium is characterized in that this method carries out according to following steps:
(1), the preparation of nano-crystalline titanium dioxide film:
Under strong agitation, a certain amount of tetraisopropyl titanate (TTIP) is slowly joined in the appropriate amount of deionized water, continue to stir 1 ~ 4 h, the sediment that obtains is carried out suction filtration and washing; Subsequently sediment is made into the TTIP of certain volume ratio and the mixed solution of TMAH (TMAH); Add the deionized water constant volume; Then powerful stirring reaction 1 ~ 5 h in 100 ~ 150 ℃ of oil baths naturally cools to room temperature, and the white colloid that obtains after reaction is accomplished is transferred in the autoclave and constant volume; Hydrothermal treatment consists 6 ~ 24 h under 150 ~ 300 ℃ condition take out behind the natural cooling and carry out sonicated 20 min, obtain milky TiO 2 sol; On clean conductive glass, form thin film through method for printing screen; Dried film is put into Muffle furnace, and temperature slowly is warming up to 450 ~ 550 ℃, constant temperature 0.5 ~ 10 h; Naturally cool to room temperature, promptly obtain undressed nano-crystalline titanium dioxide film;
(2), the preparation of titanium tetrachloride solution:
A certain amount of titanium tetrachloride is joined in the dropping funel; Be communicated with nitrogen with the glass dropper, insert the dropping funel top, blow 1 ~ 15 min with nitrogen; Under the condition of ice bath titanium tetrachloride after the above-mentioned processing is joined in the deionized water; On magnetic stirring apparatus, fully stir 30 min under the normal temperature, constant volume is to 100 mL then, and promptly obtaining molar concentration is the titanium tetrachloride colourless transparent solution of 0.005 ~ 4 mol/L;
(3), the preparation of strontium acetate solution:
A certain amount of strontium acetate is joined in the appropriate amount of deionized water, on magnetic stirring apparatus, fully stir 30 min under the normal temperature, constant volume is to 100 mL then, and promptly obtaining molar concentration is the strontium acetate colourless transparent solution of 0.001 ~ 2 mol/L;
(4), the preparation of the nanocrystalline titanium dioxide film of titanium/strontium coating:
With the method for the film behind the sintering in the step (1) through dipping, be immersed in the described strontium acetate solution of step (3) the inside earlier, in 30 ~ 90 ℃ of solution, dipping 0.3 ~ 1 h; With nitrogen moisture is blown away subsequently, then film is put into Muffle furnace, slowly be warming up to 400 ~ 550 ℃, constant temperature 0.5 ~ 10 h; Naturally cool to room temperature, and then with the solution the inside of the film immersion that obtains at the described titanium tetrachloride of step (2), in 30 ~ 90 ℃ of solution, dipping 0.3 ~ 1h; With nitrogen moisture is blown away subsequently, then film is put into Muffle furnace, slowly be warming up to 400 ~ 550 ℃; Constant temperature 0.5 ~ 10 h naturally cools to room temperature, promptly obtains handling through strontium acetate earlier; Handle through titanium tetrachloride again, form the internal layer strontium titanates, the duplicature of outer titanium dioxide (being called for short Ti-Sr-Ti) on the nano-crystalline titanium dioxide film surface; Perhaps, be immersed in the described titanium tetrachloride solution of step (2) the inside earlier with the method for the film behind the sintering in the step (1) through dipping, in 30 ~ 90 ℃ of solution, dipping 0.3 ~ 1 h; With nitrogen moisture is blown away subsequently, then film is put into Muffle furnace, slowly be warming up to 400 ~ 550 ℃, constant temperature 0.5 ~ 10 h; Naturally cool to room temperature, and then be immersed in the described strontium acetate solution of step (3) the inside, in 30 ~ 90 ℃ of solution, dipping 0.3 ~ 1 h; With nitrogen moisture is blown away subsequently, then film is put into Muffle furnace, slowly be warming up to 400 ~ 550 ℃; Constant temperature 0.5 ~ 10 h naturally cools to room temperature, promptly obtains handling through titanium tetrachloride earlier; Soak the peracetic acid strontium again and handle, form internal layer titanium dioxide, the duplicature of outer strontium titanates (being called for short Ti-Ti-Sr) on the nano-crystalline titanium dioxide film surface.
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| CN101022136A (en) * | 2007-03-16 | 2007-08-22 | 南开大学 | Alkaline-earth metal salt decorative nano crystal semiconductor optical anode, producing method and application thereof |
| CN101030607A (en) * | 2007-04-12 | 2007-09-05 | 清华大学 | Sensitized dye solar battery light anode and its production |
| CN101090141A (en) * | 2007-06-26 | 2007-12-19 | 武汉大学 | Preparation method of hybridization electrode of electric insulation salt modulation |
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| CN101022136A (en) * | 2007-03-16 | 2007-08-22 | 南开大学 | Alkaline-earth metal salt decorative nano crystal semiconductor optical anode, producing method and application thereof |
| CN101030607A (en) * | 2007-04-12 | 2007-09-05 | 清华大学 | Sensitized dye solar battery light anode and its production |
| CN101090141A (en) * | 2007-06-26 | 2007-12-19 | 武汉大学 | Preparation method of hybridization electrode of electric insulation salt modulation |
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