CN101140957A - Dye sensitization solar cell based on titanic oxide nano bar light scattering thin film electric pole and its preparing method - Google Patents
Dye sensitization solar cell based on titanic oxide nano bar light scattering thin film electric pole and its preparing method Download PDFInfo
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Abstract
A dye sensitize solar battery based on the light scattering membrane electrode of the titanium dioxide Nano Rods is provided, which belongs to technical field of solar battery manufacturing. The invention comprises light anode, electrolyte solution and counter electrode, which is characterized in that the said light anode includes in turn the first layer closely connected with the conducting fundus and the second layer contacted with the first layer. The first layer is a dense TiO2 thin membrane formed by the TiO2 particles of 2 to 5 nm in grain diameter, while the second layer is a Nano Rods thin membrane formed by the TiO2 tiny particles of 5 to 60 nm in grain diameter and Nano Rods with diameter of 6 to 11 nm and length of 90 to 450. The mirror face diascoptic lighting intensity is obviously weakened while the diffuse transmission light intensity is increased in the infrared band and near infrared band of 600 to 900. The first layer is 50 to 15 nm in thickness while the second layer is 2 to 12 micron in thickness. The dye sensitize solar battery is characterized in high light scattering property, simple preparation method and easy operation.
Description
Technical field
The invention belongs to technical field of solar cell manufacturing, particularly the manufacturing technology of DSSC.
Background technology
DSSC is mainly formed by light anode, electrolyte solution with to electrode three parts.The extinction ability of light anode is the key factor that influences this class solar cell photoelectric conversion efficiency, and its main body is the titanium dioxide (TiO that is interconnected to porous network structure
2) nano-crystal thin-film, because titanium dioxide nanocrystalline can only absorb ultraviolet light and absorptivity has only 30%, therefore titanium dioxide nanocrystalline is carried out sensitization by dyestuff, improve efficiency of light absorption.Present widely used ruthenium dye has efficient absorption to 400～600nm visible light, but (600～900nm) extinction ability wretched insufficiency has limited the raising of photoelectric conversion efficiency at ruddiness and near infrared band.The method that further improves efficiency of light absorption mainly contains three classes:
1) provide efficiency of light absorption higher sensitizing dyestuff.As document " Engineering of efficientpanchromatic sensitizers for nanocrystalline TiO
2-based solar cells " method of the black dyestuff of preparation of report in (J.Am.Chem.Soc.2001,123,1613); the energy of absorption edge of black dyestuff can arrive 920nm; the extinction ability enlarges markedly, but the stability of deceiving dyestuff is not good, can influence the life-span of battery;
2) adsorbance that increases sensitizing dyestuff improves efficiency of light absorption.As document " Single-anddouble-layered mesoporous TiO
2/ P25 TiO
2Electrode for dye-sensitized solar cell " increase thickness of (Sol.Energy Mater.Sol.Cells 2005; 86; 269) middle report and the method that the increase membrane surface area improves the dyestuff adsorbance; its adverse effect is the meeting increase internal resistance of cell, thereby reduces the open circuit photovoltage;
3) utilize light scattering effect to improve efficiency of light absorption.In the light anode, increase the light scattering center, utilize light scattering effect can increase the light path of titanium dioxide nanocrystalline film, increase the efficiency of light absorption of electrode surface dyestuff, particularly strengthen the light absorption of the weak uptake zone of the low light level and organic molecule, thereby improve the photoelectric conversion efficiency of battery;
In the titanium dioxide nanocrystalline film, add nano-bar material as the light scattering center, thereby have remarkable minimizing receive surface state quantity between the crystalline substance, reduce the advantage of the electric transmission speed of the compound probability raising battery of light induced electron and oxidation state electrolyte, be the 3rd) more effective a kind of realization thinking in the class methods.
At document " Photocurrent improvement by incorporation of single-wall carbon nanotubesin TiO
2Film of dye-sensitized solar cells " (Bull.Korean Chem.Soc.2003,24,1501), " Synthesis of TiO
2Nanotubes film and its light scattering property " (Chin.Sci.Bull.2005; 50; 1985); " Sonication-hydrothermal combination technique for thesynthesis of titanate nanotubes from commercially available precursors " (Mater.Res.Bull.2006; 41,237) and " Enhanced charge-collection efficiencies and light scatteringin dye-sensitized solar cells using oriented TiO
2Nanotubes arrays " reported nano-tube material in (Nano Lett.2007,7,69) and with the preparation method of nanotube as the DSSC at light scattering center.These methods are with TiO
2Nanotube or carbon nano-tube and TiO
2The brilliant colloid of receiving mixes by a certain percentage, the preparation DSSC.Its advantage is the specific area that can also increase membrane electrode when increasing light scattering property, improves electric conductivity.But be subjected to nanotube complicated process of preparation up till now, preparation methods' such as length consuming time restriction, the nano-tube material that is fit to caliber, suitable length is not easy to obtain.
At document " Dye-sensitized solar cells based on a single-crystalline TiO
2Nanorod film " (J.Phys.Chem.B 2006,110,2087), " TiO
2Nanorods as additive to TiO
2Filmfor improvement in the performance of dye-sensitized solar cells " reported in (J.Photochem.Photobiol.A; 2006; 180; 184) and " Transient electrical response of dye-sensitized ZnOnanorod solar cells " (J.Phys.Chem.C 2007; 111,8692) and be used for nano-bar material of DSSC and preparation method thereof.
But the TiO that in DSSC, uses at present
2Nanometer rods has two unfavorable aspects, is the restriction that is subjected to the preparation method on the one hand, TiO
2The nanometer rods diameter is bigger, can significantly reduce the specific surface and the dyestuff adsorbance of film, is little at the light absorpting ability of the ruddiness of 600～900 nanometers and near infrared band scope film on the other hand, further improves thereby limited the cell photoelectric transformation efficiency.Document " TiO for example
2Nanorods asadditive to TiO
2Film for improvement in the performance of dye-sensitized solar cells " (J.Photochem.Photobiol.A, 2006,180,184) middle TiO that reports
2The nanometer rods DSSC.The document adopts template and titanium tetrachloride hydrolysis has prepared diameter 180～250 nanometers, length is the TiO of micrometer range
2Nanometer rods is that 15% nanometer rods is mixed the TiO that particle diameter is 25～30 nanometers with mass percent
2Receive in the brilliant colloid, mixing the SnO of fluorine
2Apply colloid on the FTO electro-conductive glass of film, 450 ℃ of heat treatment 30min, make thickness and be 12 microns titanium dioxide photo anode, adopt the Ru-polypyridine dyestuff to carry out sensitization 24h then, experiment shows that the battery electron transmission performance strengthens, and in the visible light wave range scope of 400～500nm certain light scattering enhancement effect (and very little at the light scattering effect of 500～600nm visible light wave range scope and 600～900nm ruddiness and near infrared band) is arranged.This battery has 3 disadvantages: (1) is subjected to the restriction of porous alumina formwork, the TiO of document preparation
2The nanometer rods diameter is bigger, causes the electrode specific surface less, can significantly reduce the dyestuff adsorbance of battery.(2) characteristic of the Ru-polypyridine dyestuff that uses of the document itself just has efficient absorption to 400～600nm visible light, and at the extinction ability wretched insufficiency of ruddiness and near infrared band 600～900nm, therefore, the light absorption of enhancing ruddiness and near infrared band, increase TiO
2The light path of film could produce material impact to the photoelectric conversion efficiency that improves battery.(3) this battery does not add fine and close TiO
2Film, conductive substrates directly with the TiO that is mixed with nanometer rods
2Photo-anode film is connected.Because the adding of nanometer rods causes the hole in the photo-anode film to increase, easier directly the contact with conductive substrates of redox electrolytes matter causes battery short circuit.
Summary of the invention:
The objective of the invention is to overcome the deficiency of above-mentioned prior art, provide that a kind of preparation method is simple, the nanometer rods size is less based on TiO
2DSSC of nano bar light scattering membrane electrode and preparation method thereof utilizes the light scattering effect of ruddiness and near infrared band scope to increase the efficiency of light absorption of battery.
The DSSC that the present invention proposes, comprise light anode, electrolyte solution from top to bottom and to electrode three parts, it is characterized in that: described smooth anode comprises the ground floor that closely contacts with conductive substrates, the second layer that contacts with ground floor successively, and wherein ground floor is by particle diameter 2～5nm TiO
2The fine and close TiO that particulate is formed
2Thin layer, the second layer are the TiO by particle diameter 5～60nm
2The nanometer rods TiO that the nanometer rods of granule and diameter 6～11nm, length 90～450nm is formed
2Thin layer, the thickness of ground floor are that (be preferably 6～9nm), the thickness of the second layer is 2～12 microns (being preferably 4～8 microns) to 5～15nm.
Conductive substrates is the glass of buying on the market that has transparency electrode, and transparency electrode is selected from indium tin oxide films or mixes fluorine SnO
2Film.
The fine and close TiO of ground floor
2Thin layer is by TiO
2Particulate is formed.The fine and close TiO of conductive substrates and ground floor
2Directly contact gear ratio is tightr between the film, can effectively intercept electrolyte on the one hand and contact with conductive substrates, on the other hand near the fine and close TiO conductive substrates
2TiO in the film
2The particle diameter of crystal grain received is very little, can significantly strengthen second layer TiO
2The adhesive force of nano-rod film and conductive substrates.Fine and close TiO
2The integral light-transmitting rate and the planarization of thin layer are good, except the intrinsic in the ultra-violet (UV) band absorbs, at visible region good transmitance are arranged.
Second layer nanometer rods TiO
2Thin layer is by TiO
2Granule and TiO
2Nanometer rods is formed.Granule TiO
2Crystal grain of receiving surrounds the TiO of random distribution
2Nanometer rods, the size and the optical wavelength of nanometer rods are suitable, produce the high light scattering effect, can increase the light path in the thin layer, thereby improve the efficiency of light absorption of battery.When improving light scattering property, the accumulation of nanometer rods also can produce some air gap structure in film, the ions diffusion characteristic can also be improved in this gap, help electrolytical infiltration in the battery, reduce the loss of voltage that concentration polarization that mass transfer causes causes, improve the electricity conversion of battery.
The DSSC that the present invention proposes, its preparation method may further comprise the steps:
(1) the titanium precursor liquid solution evenly is coated on the conductive substrates that cleans up, heated 5～15 minutes down, the fine and close TiO of preparation ground floor on conductive substrates in 100～300 ℃
2Thin layer, described titanium precursor liquid solution are meant that concentration of volume percent is 1～7% tetraisopropyl titanate petroleum ether solution, butyl titanate petroleum ether solution, tetraisopropyl titanate n-butyl ether solution, butyl titanate n-butyl ether solution, tetraisopropyl titanate cyclohexane solution or butyl titanate cyclohexane solution;
(2) at first adopt the using supersonic, water-heating legal system to be equipped with TiO
2Nanotube is then with TiO
2Nanotube is at 500～550 ℃ of heating 0.5～2h, and obtaining diameter is that 6～11nm, length are that 90～450nm, crystal formation are the TiO of monocrystalline Detitanium-ore-type
2Nanometer rods;
Using supersonic, water-heating method reference literature " Sonication-hydrothermal combination technique for thesynthesis of titanate nanotubes from commercially available precursors " (Mater.Res.Bull.2006,41,237), in the preparation process, ultrasonic power is 200～400W, the sonicated time is 0.5～3h, and hydrothermal temperature is 110～130 ℃, and the hydro-thermal time is 24～48h;
(3) with the TiO for preparing in the step (2)
2Nanometer rods and TiO
2The granule colloid is 4～30% by weight percentage, makes TiO after being preferably 20% mixed
2Slurry, wherein TiO
2TiO in the granule colloid
2Short grained particle diameter is 5～60nm, TiO in the colloid
2Solid content be 7～25%;
The titania slurry that different proportion is formed has determined the quantity at light scattering center in the described titanic oxide nano bar light scattering thin film electric pole;
(4) TiO that step (3) is prepared
2Slurry evenly is coated in the fine and close TiO of ground floor that step (1) prepares
2Above the thin layer,, obtain second layer nanometer rods TiO at 450 ℃ of heat treatment 30min
2Thin layer;
Heat treated effect is to make TiO
2Between nanometer rods and the granule, TiO
2Between the granule and TiO
2Combine between granule and the conductive substrates firmly;
(5) repeating step (4) makes second layer nanometer rods TiO
2Thin layer thickness reaches 2～12 microns, makes titanic oxide nano bar light scattering thin film electric pole;
(6) titanic oxide nano bar light scattering thin film electric pole with step (5) preparation is immersed in the dye solution, makes the dye sensitization titanic oxide nano bar light scattering thin film electric pole;
Described dye solution can be 5 * 10
-4M 4, the ethanolic solution of 4 '-dicarboxylic acids bipyridyl ruthenium;
(7) be assembled into solar cell with the dye sensitization titanic oxide nano bar light scattering thin film electric pole that makes in the step (6) and electrolyte with to electrode.
In the step (7), described electrolyte is a pseudo-solid polymer electrolyte, is that the thermal decomposition platinum plating is to electrode to electrode.Pseudo-solid polymer electrolyte and thermal decomposition platinum plating are seen document " BaCO to the preparation method of electrode
3Modification of TiO
2Electrodes in quasi-solid-state dye-sensitized solar cells:performanceimprovement and possible mechanism " (J.Phys.Chem.C; 2007; 111; 8075); " Preparation of nano-Pt-modified electrode and its electrocatalytic activity investigation " (Mater.Chem.Phys.2006; 97,261) and " A novel method for preparing platinizedcounter electrode of nanocrystalline dye-sensitized solar cells " (Chin.Sci.Bull.2005,50,11).
Among the preparation method of DSSC of the present invention, described titanium dioxide granule colloid can adopt any known preparation method acquisition, for example " Synthesis of TiO in this area
2Nanotubes filmand its light scattering property " (Chin.Sci.Bull.2005,50,1985), " The effectof the preparation condition of TiO
2Colloids on their surface structures " (J.Phy s.Chem.B, 2000,104.4130), " pH-dependent redox potential induced in a sensitizing dye byadsorption onto TiO
2" (J.Phys.Chem.B; 1997; 101.55) and " Conversion of lightto electricity by cis-X2bis (2,2 '-bipyridyl-4,4 '-dicarboxylate) ruthenium (II) charge-transfersensitizers (X=Cl-, Br-, l-, CN-, and SCN-) on nanocrystalline TiO
2Electrodes " (J.Am.Chem.Soc, 1993,115.6382) middle reported method, these documents are incorporated herein by reference with it in full at this.
Among the preparation method of DSSC of the present invention, described titanium precursor liquid solution and TiO
2The coating method of slurry: the both sides of the conductive substrates that cleans up are fixed with adhesive tape, it is put into the titanium precursor liquid solution, adopt infusion method that the titanium precursor liquid solution is coated on the conductive substrates equably, promptly on conductive substrates, finished the fine and close TiO of ground floor after the heat treatment
2The preparation of thin layer obtains fine and close TiO
2The membrane electrode semi-finished product; With fine and close TiO
2Reserve the two ends of the blank parts of lead-in wire electrode on the membrane electrode semi-finished product and stick adhesive tape once more, dip in glass bar and get TiO
2Slurry adopts coating process to be dispersed in fine and close TiO
2Above the membrane electrode semi-finished product, obtain TiO
2The elementary semi-finished product of nano bar light scattering membrane electrode.
The method of measurement of DSSC of the present invention is: TiO
2The membrane electrode composition features is observed with FEG-JEM-2011F type transmission electron microscope (TEM), and accelerating voltage is 200kV.TiO
2The membrane electrode transmitted spectrum adopts the HITACHI Model U-3010UV type spectrophotometer that is equipped with the 16cm integrating sphere to record in 300～900nm scope.The DSSC photoelectric properties at room temperature obtain the current-voltage curve of battery by ORIEL 81193 type solar simulators and Kei thley 4200 N-type semiconductor N ability meters, draw open circuit voltage, short circuit current, the fill factor, curve factor of battery then.The light intensity of light source is measured by the FZ-A type irradiance meter of Beijing Normal University photoelectric instrument factory.Intensity of illumination is 30mW/cm
2, effective irradiated area of battery is 0.25cm
2
Any those of skill in the art are easy to improving without departing from the spirit and scope of the present invention and perfect, therefore the present invention only is subjected to the restriction of the content and the scope of claim of the present invention, and its intention contains all and is included in interior alternative or the equivalent of spirit and scope of the invention that claim limits.The present invention will be illustrated by the following examples.But, be to be understood that the present invention is not limited to particular example as described herein and embodiment.The purpose that comprises these particular example and embodiment here is to help those of skill in the art to put into practice the present invention.
DSSC light scattering property height of the present invention, and have preparation method's characteristics simple, easy and simple to handle, be easy to obtain high-quality large area film, be easy to suitability for industrialized production, thereby expanded the application prospect of DSSC.
Description of drawings:
Fig. 1 is the specular transmission curve of spectrum of two kinds of membrane electrodes, and among the figure, curve A is TiO
2Nano bar light scattering membrane electrode, curve B are TiO
2The nano-crystal thin-film electrode.
Fig. 2 is the diffuse transmission curve of spectrum of two kinds of membrane electrodes, and among the figure, curve A is TiO
2Nano bar light scattering membrane electrode, curve B are TiO
2The nano-crystal thin-film electrode.
Fig. 3 is TiO
2The transmission electron microscope of nano-crystal thin-film electrode (TEM) photo.
Fig. 4 is TiO
2The transmission electron microscope of nano bar light scattering membrane electrode (TEM) photo.
Fig. 5 is single TiO
2The high resolution transmission electron microscopy of nanometer rods (HRTEM) photo.
Among Fig. 1, TiO2The nano-crystal thin-film electrode is in long wavelength's scope, and specular transmission is large, and the loss that light passes membrane electrode is large, TiO2Nano bar light scattering membrane electrode specular transmission luminous intensity significantly weakens, and the loss that light passes membrane electrode significantly reduces. Among Fig. 2, TiO2The nano-crystal thin-film electrode is in long wavelength's scope, and diffuse transmission is little, and light path is little, TiO2Nano bar light scattering membrane electrode diffuse transmission luminous intensity increases, and light path enlarges markedly. Fig. 1 and 2 shows, TiO2Nano-crystal thin-film electrode light scattering characteristic is very little, TiO2The nano bar light scattering membrane electrode has strong light scattering effect. Among Fig. 3, TiO2The nano-crystal thin-film electrode be by about 18～35nm to receive brilliant granule molecular. Among Fig. 4, TiO2The nano bar light scattering membrane electrode is by receiving brilliant small-particle and diameter 6～11nm, the TiO of length 90～450nm about 18～35nm2The common composition of nanometer rods. Among Fig. 5, TiO2The high resolution transmission electron microscopy of nanometer rods has the very significantly spacing of lattice of 0.35nm, shows TiO2Nanometer rods is the monocrystalline Detitanium-ore-type.
Embodiment
Embodiment 1
(1) cleans the conductive substrates surface.Use indium tin oxide-coated glass as conductive substrates, adopted the ultrasonic conductive substrates of ethanol/acetone mixed solvent surface 15 minutes, putting into the deionized water for ultrasonic that is added with washing agent again cleaned 15 minutes, after putting into deionized water for ultrasonic rinsing in 15 minutes three times then, conductive substrates is placed in the clean bench, dry with infrared lamp.
(2) preparation titanium precursor liquid solution: the tetraisopropyl titanate of 3mL is dissolved in the benzinum of 100mL, and the dose volume percent concentration is 3% tetraisopropyl titanate petroleum ether solution.
(3) fine and close TiO
2The elementary semi-finished product preparation of membrane electrode.Adhesive tape is sticked on the both sides of cleaning the conductive substrates of oven dry, to reserve the blank parts of lead-in wire electrode.Be immersed in then in 3% the titanium precursor liquid solution, soak after 10 seconds and slowly take out, separate 5min in water in air.
(4) fine and close TiO
2The preparation of membrane electrode semi-finished product.With fine and close TiO
2The elementary semi-finished product of membrane electrode are put into resistance furnace, at 200 ℃ of heat treatment 10min.
(5) titanium dioxide granule colloid for preparing.Press document " Synthesis of TiO
2Nanotubes film and itslightscattering property " (Chin.Sci.Bull.2005,50,1985) and " The effectof the preparation condition of TiO
2Colloids on their surface structures " reported method prepares titanium dioxide granule colloid in (J.Phys.Chem.B, 2000,104.4130):
The aqueous acetic acid of preparation pH=2 in 0 ℃ of ice bath dropwise adds the mixed solution of different third oxygen of 36mL alcohol titanium and 36mL isopropyl alcohol in the 300ml aqueous acetic acid, and at room temperature vigorous stirring is spent the night and obtained clear solution.With this solution in 80 ℃ of stirrings of constant temperature isopropyl alcohol volatilization and obtain light blue clear solution in solution.With light blue clear solution 210 ℃ of hydro-thermal 14h in titanium system autoclave, obtain the TiO of white
2Precipitation.Treat the solution cooling ultrasonic dispersion in back 30 minutes, constantly stir evaporation under 120 ℃ of conditions, the final solid content that obtains the 18nm particle diameter is 10% TiO
2The granule colloid.
(6) titanium dioxide nano-rod preparation.Select for use commodity titanium dioxide nanocrystalline particle P25 as initiation material, adopt the method for using supersonic, water-heating associating to prepare TiO
2Nanometer rods.30ml 10M sodium hydroxide solution and 0.15g titanium dioxide raw material are put into the polytetrafluoroethylene cup, after ultrasonic 2h under the 200W power puts into 110 ℃ of water heating kettle constant temperature 24h, take out water heating kettle and naturally cool to room temperature.Behind the standing sedimentation, the supernatant liquor in the still is poured out, the lower sediment thing uses 0.1M HCl solution, distilled water repeated washing to pH=7 successively, and after the centrifugation, sediment is constant temperature 2h in 500 ℃ of Muffle furnaces, and taking-up naturally cools to room temperature and obtains the nanometer rods product.
(7) titanic oxide nano bar light scattering thin film electric pole preparation.The nanometer rods product is dispersed in the nanometer rods slurry that obtains proper viscosity in the aqueous solution that contains acetylacetone,2,4-pentanedione.According to nanometer rods and the short grained percentage by weight of titanium dioxide is 20%, takes by weighing nanometer rods slurry and TiO
2The granule colloid mixes, and ultrasonic 1h in ultrasonic cleaning machine is put in and grinds 1h in the mortar and mix and make titania slurry.At fine and close TiO
2Reserve the two ends of the blank parts of lead-in wire electrode on the membrane electrode semi-finished product and stick adhesive tape, dip in glass bar and get TiO
2Slurry adopts coating process to be dispersed in fine and close TiO
2Above the membrane electrode semi-finished product, then at 450 ℃ of heat treatment 30min.The fine and close TiO of ground floor wherein
2The thickness of thin layer is 6 nanometers, and it is the TiO by particle diameter 3nm
2Particulate is formed; Second layer nanometer rods TiO
2The thickness of thin layer is 4 microns, and it is the TiO by the titanium dioxide granule of 18nm and diameter 6nm length 100nm
2Nanometer rods is formed.
(8) dye sensitization titanic oxide nano bar light scattering thin film electric pole preparation.With TiO
2The nano bar light scattering membrane electrode heats 0.5h in 110 ℃ Muffle furnace, subsequently it is immersed in 5 * 10
-4M 4, take out behind the 24h in the ethanolic solution of 4 '-dicarboxylic acids bipyridyl ruthenium, with the infrared lamp oven dry of absolute ethyl alcohol flushing back.
(9) pseudo-solid polymer electrolyte preparation.LiI and 0.019g I with 0.100g
2Be dissolved in the mixed solution of 5mL acetonitrile and 5mL propylene carbonate ester, add 0.038g P25 powder then,, add 44 μ L four the tertiary butyl pyridine is ultrasonic and be uniformly dispersed through the ultrasonic polyoxyethylene PEO (molecular weight is 2,000,000) that disperses back adding 0.265g.
(10) the thermal decomposition platinum plating is to electrode preparation.H with 5mmol
2PtCl
6Aqueous isopropanol be added drop-wise to the surface of electro-conductive glass, treat that liquid is sprawled into uniform liquid film fully after, in air, dry, put into 380 ℃ Muffle furnace sintering 15min.
(11) DSSC assembling.On the dye sensitization titanic oxide nano bar light scattering thin film electric pole, add pseudo-solid polymer electrolyte, the thermal decomposition platinum plating faced down to electrodes conduct be attached on the dye sensitization titanic oxide nano bar light scattering thin film electric pole, both sides use clip to fix, and finish the assembling of battery.
Embodiment 2
According to the method among the embodiment 1, except that following step has the change, other step is identical.
During preparation titanium precursor liquid solution, the butyl titanate of 7mL is dissolved in the cyclohexane of 100mL, the dose volume percent concentration is 7% butyl titanate cyclohexane solution.
During titanium dioxide granule colloid for preparing, 230 ℃ of hydro-thermal 14h in titanium system autoclave, the final solid content that obtains the 30nm particle diameter is 20% TiO
2The granule colloid.
When titanium dioxide nano-rod prepared, after putting into 120 ℃ of water heating kettle constant temperature 36h behind the ultrasonic 1h under the 300W power, the lower sediment thing is constant temperature 2h in 550 ℃ of Muffle furnaces.
When titanic oxide nano bar light scattering thin film electric pole prepares, TiO
2The short grained percentage by weight of nanometer rods and titanium dioxide is 20%.The fine and close TiO of ground floor wherein
2The thickness of thin layer is 10 nanometers, and it is made up of particle diameter 5nm titanium dioxide fine particles; Second layer nanometer rods TiO
2The thickness of thin layer is 8 microns, and it is the TiO by the titanium dioxide granule of 30nm and diameter 10nm length 350nm
2Nanometer rods is formed.
Embodiment 3
According to the method among the embodiment 1, except that following step has the change, other step is identical.
During preparation titanium precursor liquid solution, the tetraisopropyl titanate of 1mL is dissolved in the n-butyl ether of 100mL, the dose volume percent concentration is 1% tetraisopropyl titanate n-butyl ether solution.
During titanium dioxide granule colloid for preparing, 230 ℃ of hydro-thermal 12h in titanium system autoclave, the final solid content that obtains the 25nm particle diameter is 15% TiO
2The granule colloid.
When titanium dioxide nano-rod prepared, after putting into 120 ℃ of water heating kettle constant temperature 48h behind the ultrasonic 3h under the 400W power, the lower sediment thing is constant temperature 2h in 500 ℃ of Muffle furnaces.
When titanic oxide nano bar light scattering thin film electric pole prepared, the short grained percentage by weight of nanometer rods and titanium dioxide was 15%.The fine and close TiO of ground floor wherein
2The thickness of thin layer is 5 nanometers, and it is made up of particle diameter 2nm titanium dioxide fine particles; Second layer nanometer rods TiO
2The thickness of thin layer is 4 microns, and it is the TiO by the titanium dioxide granule of 25nm and diameter 11nm length 450nm
2Nanometer rods is formed.
Embodiment 4
According to the method among the embodiment 1, except that following step has the change, other step is identical.
During preparation titanium precursor liquid solution, the tetraisopropyl titanate of 1mL is dissolved in the cyclohexane of 100mL, the dose volume percent concentration is 1% tetraisopropyl titanate cyclohexane solution.
During titanium dioxide granule colloid for preparing, 200 ℃ of hydro-thermal 12h in titanium system autoclave, the final solid content that obtains the 14nm particle diameter is 8% TiO
2The granule colloid.
When titanium dioxide nano-rod prepared, after putting into 120 ℃ of water heating kettle constant temperature 48h behind the ultrasonic 3h under the 400W power, the lower sediment thing is constant temperature 0.5h in 500 ℃ of Muffle furnaces.
When titanic oxide nano bar light scattering thin film electric pole prepared, the short grained percentage by weight of nanometer rods and titanium dioxide was 8%.The fine and close TiO of ground floor wherein
2The thickness of thin layer is 5 nanometers, and it is made up of particle diameter 2nm titanium dioxide fine particles; Second layer nanometer rods TiO
2The thickness of thin layer is 2 microns, and it is the TiO by the titanium dioxide granule of 14nm and diameter 11nm length 450nm
2Nanometer rods is formed.
According to the method among the embodiment 1, except that following step has the change, other step is identical.
During preparation titanium precursor liquid solution, the tetraisopropyl titanate of 4mL is dissolved in the cyclohexane of 100mL, the dose volume percent concentration is 4% tetraisopropyl titanate cyclohexane solution.
During titanium dioxide granule colloid for preparing, 230 ℃ of hydro-thermal 12h in titanium system autoclave, the final solid content that obtains the 25nm particle diameter is 15% TiO
2The granule colloid.
When titanium dioxide nano-rod prepared, after putting into 130 ℃ of water heating kettle constant temperature 36h behind the ultrasonic 3h under the 400W power, the lower sediment thing is constant temperature 0.5h in 550 ℃ of Muffle furnaces.
When titanic oxide nano bar light scattering thin film electric pole prepared, the short grained percentage by weight of nanometer rods and titanium dioxide was 15%.The fine and close TiO of ground floor wherein
2The thickness of thin layer is 8 nanometers, and it is made up of particle diameter 4nm titanium dioxide fine particles; Second layer nanometer rods TiO
2The thickness of thin layer is 12 microns, and it is the TiO by the titanium dioxide granule of 25nm and diameter 10nm length 400nm
2Nanometer rods is formed.
Embodiment 6
According to the method among the embodiment 1, except that following step has the change, other step is identical.
During preparation titanium precursor liquid solution, the tetraisopropyl titanate of 3mL is dissolved in the benzinum of 100mL, the dose volume percent concentration is 3% butyl titanate petroleum ether solution.
During titanium dioxide granule colloid for preparing, 230 ℃ of hydro-thermal 16h in titanium system autoclave, the final solid content that obtains the 35nm particle diameter is 25% TiO
2The granule colloid.
When titanium dioxide nano-rod prepared, after putting into 110 ℃ of water heating kettle constant temperature 36h behind the ultrasonic 0.5h under the 400W power, the lower sediment thing is constant temperature 2h in 500 ℃ of Muffle furnaces.
When titanic oxide nano bar light scattering thin film electric pole prepared, the short grained percentage by weight of nanometer rods and titanium dioxide was 30%.The fine and close TiO of ground floor wherein
2The thickness of thin layer is 9 nanometers, and it is made up of particle diameter 3nm titanium dioxide fine particles; Second layer nanometer rods TiO
2The thickness of thin layer is 8 microns, and it is the TiO by the titanium dioxide granule of 35nm and diameter 9nm length 200nm
2Nanometer rods is formed.
Embodiment 7
According to the method among the embodiment 1, remove TiO
2The granule colloid directly is coated onto above the titanium dioxide dense membrane electrode semi-finished product, obtains beyond the titanium dioxide membrane electrode provided semi-finished product, and other step is identical, obtains titanium dioxide nano-crystal thin-film electrode.Titanium dioxide nano-crystal thin-film electrode is heated 1h in temperature is 100 ℃ Muffle furnace, subsequently it is immersed in 5 * 10
-4M 4, take out behind the 48h in the ethanolic solution of 4 '-dicarboxylic acids bipyridyl ruthenium, make dye sensitization titanium dioxide nanocrystalline membrane electrode with the infrared lamp oven dry of absolute ethyl alcohol flushing back.The fine and close TiO of ground floor wherein
2The thickness of thin layer is 6 nanometers, and it is made up of particle diameter 3nm titanium dioxide fine particles; Second layer TiO
2The thickness of thin layer is 4 microns, and the titanium dioxide granule particle diameter that constitutes this thin layer is 18nm.
Embodiment 8
According to the method among the embodiment 7, except that thickness being changed into 8 microns, other step is identical, makes dye sensitization titanium dioxide nanocrystalline membrane electrode.The fine and close TiO of ground floor wherein
2The thickness of thin layer is 6 nanometers, and it is made up of particle diameter 3nm titanium dioxide fine particles; Second layer TiO
2The thickness of thin layer is 8 microns, and the titanium dioxide granule particle diameter that constitutes this thin layer is 18nm.
Table 1 is to use the DSSC photoelectric properties index based on titanic oxide nano bar light scattering thin film electric pole of embodiment of the invention preparation.
Table 1
| Short-circuit photocurrent Isc (mAcm -2) | Open circuit photovoltage Voc (mV) | Fill factor, curve factor FF | Photoelectric conversion efficiency η (%) | |
| Embodiment 1 embodiment 2 embodiment 3 embodiment 4 |
5.61 6.49 5.21 2.86 5.45 5.96 4.28 5.59 | 0.585 0.575 0.565 0.590 0.555 0.580 0.605 0.585 | 61.0 62.8 66.3 67.4 66.8 62.1 59.2 60.5 | 6.67 7.81 6.51 3.79 6.74 7.15 5.11 6.59 |
Claims (7)
1. DSSC based on titanic oxide nano bar light scattering thin film electric pole, form by light anode, electrolyte solution with to electrode three parts, it is characterized in that: described smooth anode comprises the ground floor that closely contacts with conductive substrates, the second layer that contacts with ground floor successively, and wherein ground floor is by particle diameter 2～5nm TiO
2The fine and close TiO that particulate is formed
2Thin layer, the second layer are the TiO by particle diameter 5～60nm
2The nanometer rods TiO that the nanometer rods of granule and diameter 6～11nm, length 90～450nm is formed
2Thin layer, the thickness of ground floor are 5～15nm, and the thickness of the second layer is 2～12 microns.
2. solar cell according to claim 1 is characterized in that: described conductive substrates is the glass that has transparency electrode, and transparency electrode is selected from indium tin oxide films or mixes fluorine SnO
2Film.
3. solar cell according to claim 1 and 2 is characterized in that: the thickness of ground floor is 6～9nm, and the thickness of the second layer is 4～8 microns.
4. the preparation method according to claim 1 or 2 or 3 described solar cells comprises the steps: successively
(1) the titanium precursor liquid solution evenly is coated on the conductive substrates that cleans up, heated 5～15 minutes down, the fine and close TiO of preparation ground floor on conductive substrates in 100～300 ℃
2Thin layer, described titanium precursor liquid solution are meant that concentration of volume percent is 1～7% tetraisopropyl titanate petroleum ether solution, butyl titanate petroleum ether solution, tetraisopropyl titanate n-butyl ether solution, butyl titanate n-butyl ether solution, tetraisopropyl titanate cyclohexane solution or butyl titanate cyclohexane solution;
(2) adopt the using supersonic, water-heating legal system to be equipped with TiO earlier
2Nanotube is then with TiO
2Nanotube is at 500～550 ℃ of heating 0.5～2h, and obtaining diameter is that 6～11nm, length are that 90～450nm, crystal formation are the TiO of monocrystalline Detitanium-ore-type
2Nanometer rods, in the preparation process, ultrasonic power is 200～400W, and the sonicated time is 0.5～3h, and hydrothermal temperature is 110～130 ℃, and the hydro-thermal time is 24～48h;
(3) with the TiO for preparing in the step (2)
2Nanometer rods and TiO
2Granule is to make TiO after 4～30% mixed by weight percentage
2Slurry, wherein TiO
2TiO in the granule colloid
2Short grained particle diameter is 5～60nm, TiO in the colloid
2Solid content be 7～25%;
(4) TiO that step (3) is prepared
2Slurry evenly is coated in the fine and close TiO of ground floor that step (1) prepares
2Above the thin layer,, obtain second layer nanometer rods TiO at 450 ℃ of heat treatment 30min
2Thin layer;
(5) repeating step (4) 1 times or repeatedly makes second layer nanometer rods TiO
2Thin layer thickness reaches 2～12 microns, makes titanic oxide nano bar light scattering thin film electric pole;
(6) titanic oxide nano bar light scattering thin film electric pole with step (5) preparation is immersed in the dye solution, makes the dye sensitization titanic oxide nano bar light scattering thin film electric pole;
(7) be assembled into solar cell with the dye sensitization titanic oxide nano bar light scattering thin film electric pole that makes in the step (6) and electrolyte with to electrode.
5. preparation method according to claim 4 is characterized in that: the dye solution described in the step (6) is 5 * 10
-4M 4, the ethanolic solution of 4 '-dicarboxylic acids bipyridyl ruthenium.
6. preparation method according to claim 4 is characterized in that: the electrolyte described in the step (7) is a pseudo-solid polymer electrolyte, is that the thermal decomposition platinum plating is to electrode to electrode.
7. preparation method according to claim 4 is characterized in that: the TiO of step (3)
2TiO in the slurry
2Nanometer rods and TiO
2Short grained percentage by weight is 20%.
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