CN103762082A - Method for preparing dye sensitization solar cell photo-anode film - Google Patents
Method for preparing dye sensitization solar cell photo-anode film Download PDFInfo
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- CN103762082A CN103762082A CN201410029213.7A CN201410029213A CN103762082A CN 103762082 A CN103762082 A CN 103762082A CN 201410029213 A CN201410029213 A CN 201410029213A CN 103762082 A CN103762082 A CN 103762082A
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- Y02E10/542—Dye sensitized solar cells
Abstract
The invention discloses a method for preparing a dye sensitization solar cell photo-anode film. The method comprises the steps that a solvothermal method is used for preparing titanium dioxide nanosheets; commercial P25 titanium dioxide is used as the source of titanium dioxide nano particles, and a plurality of groups of titanium dioxide slurry with different mass ratios from that of the titanium dioxide nano particles/titanium dioxide nanosheets are prepared; the titanium dioxide slurry is printed on conductive glass to be completely dried through a silk screen print method, and a film of a gradient structure is prepared on the conductive glass; a titanium dioxide film is calcined, and an addition agent in the film is removed; dyes are used for sensitizing the calcined titanium dioxide film, and the dye sensitization solar cell photo-anode film is obtained. The large specific surface area of the nanosheets is beneficial to improving the adsorbing capacity to the dyes, and the nanosheets can promote quick transmission of electrons. In addition the special gradient structure enables incident light to be repeatedly reflected in the film, absorption to the light of the film is effectively enhanced, and therefore the photoelectric conversion efficiency is greatly improved.
Description
Technical field
The present invention relates to a kind of preparation method of dye-sensitized solar cell anode film.
Background technology
Solar energy, as a kind of regenerative resource, has the advantages such as widely distributed and inexhaustible, is a kind of zero clean energy resource polluting.DSSC can change sunlight luminous energy into electric energy, has the advantages such as abundant raw materials, with low cost, technology is relatively simple, can large area suitability for industrialized production.Meanwhile, all raw material and the production technology of preparation DSSC are all nontoxic, pollution-free, and part material can be reclaimed fully, and this has great importance to environmental protection.Through time more than ten years, DSSC research has made great progress at aspects such as electrode, electrolyte, dyestuffs, also has very large development space at aspects such as high efficiency, stability, durability simultaneously.Light anode is the important component part of DSSC.Wherein, compared with high and preparation technology is simple etc., advantage is widely studied titania-based film light anode, transformation efficiency with low cost owing to having.Titanium dioxide is the carrier of dyestuff and the transmission body of electronics, also plays a part to promote that sunlight absorbs simultaneously.Little titania nanoparticles has larger specific area, but is unfavorable for absorption and the electric transmission of light.And large titanium dioxide granule is conducive to absorption and the reflection of light, but fewer to the adsorbance of dyestuff.Traditional titanium dioxide nanocrystalline film often can not be taken into account large reference area, strong light absorption and electric transmission fast.{ titanium dioxide nanoplate of 001} crystal face has large specific area, and nanometer sheet is conducive to transmission and the reflection of light of electronics to contain exposure.The present invention proposes a kind of gradient-structure design of titanium deoxid film, being about to titania nanoparticles and titanium dioxide nanoplate is compounded in and on electro-conductive glass, forms gradient-structure, this gradient-structure is when having guaranteed high Dye Adsorption amount and swift electron transmission, effectively strengthen the absorption to light, thereby greatly improved photoelectric conversion efficiency.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of dye-sensitized solar cell anode film.
The preparation method of a kind of dye-sensitized solar cell anode film provided by the invention the steps include:
(1) adopt solvent-thermal method to prepare titanium dioxide nanoplate;
(2) using commercial P25 titanium dioxide, as titania nanoparticles, originate, configure the titania slurry of some groups of titania nanoparticles/titanium dioxide nanoplate different quality ratios;
(3) by silk screen print method, the titania slurry of different quality ratio is printed on electro-conductive glass and fully and is dried, on electro-conductive glass, be prepared into gradient-structure titanium deoxid film;
(4) by titanium deoxid film calcining, remove the additive in film;
(5) with dyestuff, the titanium deoxid film after calcining is carried out to sensitization, obtain dye-sensitized solar cell anode film.
In described step (1), the method for preparing titanium dioxide nanoplate is: 50 mL butyl titanates are inserted in the polytetrafluoroethyllining lining of 200 mL, then toward wherein adding the hydrofluoric acid that 1～15 mL concentration is 40%; After at room temperature stirring, put into drying box in 180 ℃ of reactions 24 hours; After question response completes, the white precipitate of reaction gained is washed three times with ethanol and distilled water respectively, finally put into vacuum drying chamber and be dried 12 hours in 80 ℃.
The addition of described hydrofluoric acid is preferably 4～10 mL.
In described step (2), the step of configuration titania slurry is: get 0.5 g ethyl cellulose and be dissolved in 6 mL ethanol, then toward the mixed solution that wherein adds 4 g terpinols and 5 mL ethanol to be made into, add again 0.01 mLOP emulsifying agent and 0.3 mL acetylacetone,2,4-pentanedione, finally adding gross mass is the titania powder that 1g is comprised of titania nanoparticles and/or titanium dioxide nanoplate, and mixture is put into 80 ℃ of stirred in water bath until alcohol solvent wherein volatilizees completely; Configure in this way five groups of titania slurries, in every group of titania slurry, the shared mass ratio of titania nanoparticles and titanium dioxide nanoplate is different.
In five groups of titania slurries of described configuration, in every group of slurry, the mass ratio of titania nanoparticles/titanium dioxide nanoplate is a/b, wherein a+b=100.
In described step (3), the number of plies of silk screen printing is 10 layers, often two-layer is one group, in every cluster film, the mass ratio of titania nanoparticles and titanium dioxide nanoplate is all different, from the conducting surface bottom of electro-conductive glass to upper strata, in five groups of titania slurries that use, the mass ratio of titania nanoparticles gradually reduces, the mass ratio of titanium dioxide nanoplate progressively increases, and is prepared into gradient-structure titanium deoxid film on electro-conductive glass; Every printing one deck, at room temperature places film 10 minutes and puts into 80 ℃ of drying boxes dry 10 minutes.
In described step (4), the titanium deoxid film printing is put into tube furnace in 300～500 ℃ of calcinings 20～40 minutes, heating rate is controlled at 2～10 ℃/min.
Described titanium deoxid film is placed in tube furnace in 450 ℃ of calcinings 30 minutes, and heating rate is controlled at 5 ℃/min.
In described step (5), the step of dye sensitization is: will through the titanium deoxid film of 300～500 ℃ of calcinings, be placed in the N719 dyestuff that concentration is 0.3～0.8 mol/L, in darkroom, in 30～70 ℃, soak 10～24 hours, finally with ethanol, wash away the dyestuff of surface attachment and be dried, obtaining dye-sensitized solar cell anode film.
450 ℃ of described calcining heats, the concentration of N719 dyestuff is 0.5 mol/L.
Titania nanoparticles/nanometer sheet gradient structure film light anode is labeled as SPG.
Prepared titania nanoparticles/nanometer sheet gradient film light the anode of the present invention is applied to DSSC, the method of testing of its photoelectric conversion efficiency is: take prepared titanium deoxid film as light anode, platinum electrode is to electrode, electrolyte solution is 0.6 M 1-propyl group-3-methylimidazole salt compounded of iodine, 0.3 M lithium iodide, the acetonitrile solution of 0.05 M iodine and the tertiary yl pyridines of 0.5 M 4-.By platinum is covered on light anode electrode, between two electrodes, form the cavity of approximately 50 μ m, complete the assembling of a sandwich battery.Photoelectric current-photovoltage characteristic curve of DSSC (
i-Vcurve) on Shanghai Chen Hua instrument company electrochemical workstation, to measure, the light source of employing is U.S. Newport company 91160 type solar simulators.Light intensity is 100 mW/cm
2, the illuminating area of electrode is 0.14 cm
2.
Benefit effect of the present invention is:
Titania nanoparticles and nanometer sheet are prepared into gradient structure film on electro-conductive glass, this film has not only improved the adsorbance to dyestuff, and the electronics that nanometer sheet structure is conducive to be excited on dyestuff is transferred to rapidly on electro-conductive glass nanometer sheet, has reduced recombination probability.In addition, nano particle/nanometer sheet gradient-structure makes incident light at the inner multiple reflections that forms of film, has farthest strengthened the absorption to incident light, thereby has effectively improved electricity conversion.
The gradient-structure design of the nanocrystalline titanium dioxide photo anode film of preparing high-photoelectric transformation efficiency that the present invention adopts, can also take into account large reference area, strong light absorption and the gradient structure film of electric transmission fast for the preparation of other.
accompanying drawing explanation
fig. 1gradient-structure design diagram.
fig. 2the low power (a) of titanium dioxide nanoplate and high-resolution (b) transmission electron microscope (TEM) image.
fig. 3the UV-vis DRS abosrption spectrogram of different photo-anode films.
fig. 4the DSSC of anode assembling of not sharing the same light
i-Vcharacteristic curve.
Embodiment
embodiment 1:
Fluorine ion has a great impact the pattern of titanium dioxide.For the impact on titanium dioxide pattern of the addition of checking hydrofluoric acid, the addition of butyl titanate is fixed as 50 mL.Concrete steps are: 50 mL butyl titanates and 1-15 mL hydrofluoric acid (HF, concentration is 40%) are joined in the polytetrafluoroethylene water heating kettle of 200 mL, put into drying box in 180 ℃ of reactions 24 hours after at room temperature stirring.After question response completes, the white precipitate of reaction gained is washed three times with ethanol and distilled water respectively, be finally placed in vacuum drying chamber and be dried 12 hours in 80 ℃.The optimum addition of finding the hydrofluoric acid of preparing titanium dioxide nanoplate in experiment is 4-10 mL.The TEM picture of titanium dioxide nanoplate has confirmed the nano-sheet structure that its border is clearly demarcated, as shown in Figure 2 a.Nanometer sheet is of a size of 30-50 nm, and thickness is about 6.8 nm.Fig. 2 b has provided the high-resolution TEM image of anatase titania nanometer sheet.From high-resolution TEM image, can see lattice fringe clearly, nanometer sheet side and positive interplanar distance, for being respectively 0.235 nm and 0.35 nm, correspond respectively to { 001} and { the 101} crystal face of anatase titania.
embodiment 2:
Using commercial P25 titanium dioxide, as titania nanoparticles, originate.Getting 0.5 g ethyl cellulose is dissolved in 6 mL ethanol, then toward the mixed solution that wherein adds 4 g terpinols and 5 mL ethanol to be made into, add again 0.01 mLOP emulsifying agent and 0.3 mL acetylacetone,2,4-pentanedione, finally add 1 g pure titinium dioxide nano particle, in 80 ℃ of water-baths, stir while heat until alcohol solvent wherein volatilizees completely.
Adopt silk screen print method that slurry is printed on electro-conductive glass.The number of plies of silk screen printing is 10 layers, and every printing one deck is at room temperature placed film 10 minutes and put into 80 ℃ of drying boxes dry 10 minutes.Finally the titanium deoxid film printing is placed in to tube furnace in 450 ℃ of calcinings 30 minutes, heating rate is controlled at 5 ℃/min.
To through the titanium deoxid film of 450 ℃ of calcinings, be placed in the N719 dyestuff that concentration is 0.5 mol/L, in darkroom, in 50 ℃ of immersions 24 hours, finally with ethanol, wash away the dyestuff of surface attachment and be dried, obtain dye-sensitized solar cell anode film.
Film light anode prepared by pure titinium dioxide nano particle is labeled as P100.The UV-vis DRS abosrption spectrogram of P100 as shown in Figure 3.By P100's
i-Vthe photoelectric conversion efficiency that curve (accompanying drawing 4) can calculate P100 is 2.45%.
embodiment 3:
Using butyl titanate as titanium source, 50 mL butyl titanates are placed in to a polytetrafluoroethyllining lining, then toward wherein adding 4-10 mL hydrofluoric acid (concentration is 40%), at room temperature stir rear sealing and be placed in drying box.It is 180 ℃ that reaction temperature is set, and the reaction time is 24 hours.By the white precipitate of reaction gained respectively with ethanol and distilled water washing three times, be finally placed in vacuum drying chamber in 80 ℃ dry 12 hours, obtain titanium dioxide nanoplate powder.Getting 0.5 g ethyl cellulose is dissolved in 6 mL ethanol, then toward the mixed solution that wherein adds 4 g terpinols and 5 mL ethanol to be made into, add again 0.01 mLOP emulsifying agent and 0.3 mL acetylacetone,2,4-pentanedione, finally add 1 g pure titinium dioxide nanometer sheet, in 80 ℃ of water-baths, stir while heat until alcohol solvent wherein volatilizees completely.
Adopt silk screen print method that slurry is printed on electro-conductive glass.The number of plies of silk screen printing is 10 layers, and every printing one deck is at room temperature placed film 10 minutes and put into 80 ℃ of drying boxes dry 10 minutes.Finally the titanium deoxid film printing is placed in to tube furnace in 450 ℃ of calcinings 30 minutes, heating rate is controlled at 5 ℃/min.
To through the titanium deoxid film of 450 ℃ of calcinings, be placed in the N719 dyestuff that concentration is 0.5 mol/L, in darkroom, in 50 ℃ of immersions 24 hours, finally with ethanol, wash away the dyestuff of surface attachment and be dried, obtain dye-sensitized solar cell anode film.Film light anode prepared by pure titinium dioxide nanometer sheet is labeled as S100.The UV-vis DRS abosrption spectrogram of S100 as shown in Figure 3.By S100's
i-Vthe photoelectric conversion efficiency that curve (accompanying drawing 4) can calculate S100 is 5.20%.
embodiment 4:
Using butyl titanate as titanium source, 50 mL butyl titanates are placed in to a polytetrafluoroethyllining lining, then toward wherein adding 4-10 mL hydrofluoric acid (concentration is 40%), at room temperature stir rear sealing and be placed in drying box.It is 180 ℃ that reaction temperature is set, and the reaction time is 24 hours.By the white precipitate of reaction gained respectively with ethanol and distilled water washing three times, be finally placed in vacuum drying chamber in 80 ℃ dry 12 hours, obtain titanium dioxide nanoplate powder.Using commercial P25 titanium dioxide, as titanium dioxide granule, originate.Getting 0.5 g ethyl cellulose is dissolved in 6 mL ethanol, then toward the mixed solution that wherein adds 4 g terpinols and 5 mL ethanol to be made into, add again 0.01 mLOP emulsifying agent and 0.3 mL acetylacetone,2,4-pentanedione, finally add 0.5 g pure titinium dioxide nanometer sheet and 0.5 g pure titinium dioxide nano particle, in 80 ℃ of water-baths, stir while heat until alcohol solvent wherein volatilizees completely.
Adopt silk screen print method that slurry is printed on electro-conductive glass.The number of plies of silk screen printing is 10 layers, and every printing one deck is at room temperature placed film 10 minutes and put into 80 ℃ of drying boxes dry 10 minutes.Finally the titanium deoxid film printing is placed in to tube furnace in 450 ℃ of calcinings 30 minutes, heating rate is controlled at 5 ℃/min.
To through the titanium deoxid film of 450 ℃ of calcinings, be placed in the N719 dyestuff that concentration is 0.5 mol/L, in darkroom, in 50 ℃ of immersions 24 hours, finally with ethanol, wash away the dyestuff of surface attachment and be dried, obtain dye-sensitized solar cell anode film.The film light anode that titania nanoparticles and nanometer sheet are prepared after evenly mixing is labeled as SPH.The UV-vis DRS abosrption spectrogram of SPH as shown in Figure 3.By SPH's
i-Vthe photoelectric conversion efficiency that curve (accompanying drawing 4) can calculate SPH is 4.46%.
embodiment 5:
Using butyl titanate as titanium source, 50 mL butyl titanates are placed in to a polytetrafluoroethyllining lining, then toward wherein adding 4-10 mL hydrofluoric acid (concentration is 40%), at room temperature stir rear sealing and be placed in drying box.It is 180 ℃ that reaction temperature is set, and the reaction time is 24 hours.By the white precipitate of reaction gained respectively with ethanol and distilled water washing three times, be finally placed in vacuum drying chamber in 80 ℃ dry 12 hours, obtain titanium dioxide nanoplate powder.
Using commercial P25 titanium dioxide, as titania nanoparticles, originate.Getting 0.5 g ethyl cellulose is dissolved in 6 mL ethanol, then toward the mixed solution that wherein adds 4 g terpinols and 5 mL ethanol to be made into, add again 0.01 mLOP emulsifying agent and 0.3 mL acetylacetone,2,4-pentanedione, finally adding gross mass is the titania powder of 1g, stirs while heat until alcohol solvent wherein volatilizees completely in 80 ℃ of water-baths.Configure five groups of titania slurries, in every group of slurry, the mass ratio of titania nanoparticles/titanium dioxide nanoplate is respectively: 100/0,75/25,50/50,25/75,0/100.
Adopt silk screen print method that slurry is printed on electro-conductive glass.The number of plies of silk screen printing is 10 layers, and often two-layer is one group, and in every cluster film, the mass ratio of titania nanoparticles and nanometer sheet is all different.From the conducting surface bottom of electro-conductive glass to upper strata, in every cluster film, the mass ratio of titania nanoparticles/titanium dioxide nanoplate is followed successively by: 100/0,75/25,50/50,25/75,0/100.Every printing one deck, at room temperature places film 10 minutes and puts into 80 ℃ of drying boxes dry 10 minutes.Finally the titanium deoxid film printing is placed in to tube furnace in 450 ℃ of calcinings 30 minutes, heating rate is controlled at 5 ℃/min.
To through the titanium deoxid film of 450 ℃ of calcinings, be placed in the N719 dyestuff that concentration is 0.5 mol/L, in darkroom, in 50 ℃ of immersions 24 hours, finally with ethanol, wash away the dyestuff of surface attachment and be dried, obtain dye-sensitized solar cell anode film.Titania nanoparticles/nanometer sheet gradient structure film light anode is labeled as SPG.The UV-vis DRS abosrption spectrogram of SPG as shown in Figure 3.The photoelectric conversion efficiency that can be calculated SPG by the I-V curve (accompanying drawing 4) of SPG is 6.48%.
Claims (10)
1. a preparation method for dye-sensitized solar cell anode film, is characterized in that the steps include:
(1) adopt solvent-thermal method to prepare titanium dioxide nanoplate;
(2) using commercial P25 titanium dioxide, as titania nanoparticles, originate, configure the titania slurry of some groups of titania nanoparticles/titanium dioxide nanoplate different quality ratios;
(3) by silk screen print method, the titania slurry of different quality ratio is printed on electro-conductive glass and fully and is dried, on electro-conductive glass, be prepared into gradient-structure titanium deoxid film;
(4) by titanium deoxid film calcining, remove the additive in film;
(5) with dyestuff, the titanium deoxid film after calcining is carried out to sensitization, obtain dye-sensitized solar cell anode film.
2. preparation method as claimed in claim 1, it is characterized in that: in described step (1), the method of preparing titanium dioxide nanoplate is: 50 mL butyl titanates are inserted in the polytetrafluoroethyllining lining of 200 mL, then toward wherein adding the hydrofluoric acid that 1～15 mL concentration is 40%; After at room temperature stirring, put into drying box in 180 ℃ of reactions 24 hours; After question response completes, the white precipitate of reaction gained is washed three times with ethanol and distilled water respectively, finally put into vacuum drying chamber and be dried 12 hours in 80 ℃.
3. preparation method as claimed in claim 2, is characterized in that: the addition of described hydrofluoric acid is 4～10 mL.
4. preparation method as claimed in claim 1, it is characterized in that: in described step (2), the step of configuration titania slurry is: get 0.5 g ethyl cellulose and be dissolved in 6 mL ethanol, then toward the mixed solution that wherein adds 4 g terpinols and 5 mL ethanol to be made into, add again 0.01 mLOP emulsifying agent and 0.3 mL acetylacetone,2,4-pentanedione, finally adding gross mass is the titania powder that 1g is comprised of titania nanoparticles and/or titanium dioxide nanoplate, and mixture is put into 80 ℃ of stirred in water bath until alcohol solvent wherein volatilizees completely; Configure in this way five groups of titania slurries, in every group of titania slurry, the shared mass ratio of titania nanoparticles and titanium dioxide nanoplate is different.
5. preparation method as claimed in claim 4, is characterized in that: in five groups of titania slurries of described configuration, in every group of slurry, the mass ratio of titania nanoparticles/titanium dioxide nanoplate is a/b, wherein a+b=100.
6. preparation method as claimed in claim 1, it is characterized in that: in described step (3), the number of plies of silk screen printing is 10 layers, often two-layer is one group, in every cluster film, the mass ratio of titania nanoparticles and titanium dioxide nanoplate is all different, from the conducting surface bottom of electro-conductive glass to upper strata, in five groups of titania slurries that use, the mass ratio of titania nanoparticles gradually reduces, the mass ratio of titanium dioxide nanoplate progressively increases, and is prepared into gradient-structure titanium deoxid film on electro-conductive glass; Every printing one deck, at room temperature places film 10 minutes and puts into 80 ℃ of drying boxes dry 10 minutes.
7. preparation method as claimed in claim 1, is characterized in that: in described step (4), the titanium deoxid film printing is put into tube furnace in 300～500 ℃ of calcinings 20～40 minutes, heating rate is controlled at 2～10 ℃/min.
8. preparation method as claimed in claim 7, is characterized in that: described titanium deoxid film is placed in tube furnace in 450 ℃ of calcinings 30 minutes, and heating rate is controlled at 5 ℃/min.
9. preparation method as claimed in claim 1, it is characterized in that: in described step (5), the step of dye sensitization is: will through the titanium deoxid film of 300～500 ℃ of calcinings, be placed in the N719 dyestuff that concentration is 0.3～0.8 mol/L, in darkroom, in 30～70 ℃, soak 10～24 hours, finally with ethanol, wash away the dyestuff of surface attachment and be dried, obtaining dye-sensitized solar cell anode film.
10. preparation method as claimed in claim 9, is characterized in that: 450 ℃ of described calcining heats, the concentration of N719 dyestuff is 0.5 mol/L.
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