CN102623195A - Method for preparing solar cell through quantum dot and dye synergistic sensitization of TiO2 nanorod array - Google Patents
Method for preparing solar cell through quantum dot and dye synergistic sensitization of TiO2 nanorod array Download PDFInfo
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- CN102623195A CN102623195A CN2012101278566A CN201210127856A CN102623195A CN 102623195 A CN102623195 A CN 102623195A CN 2012101278566 A CN2012101278566 A CN 2012101278566A CN 201210127856 A CN201210127856 A CN 201210127856A CN 102623195 A CN102623195 A CN 102623195A
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Abstract
The invention provides a method for preparing a solar cell through quantum dot and dye synergistic sensitization based on a TiO2 nanorod array electrode. The method comprises the steps of: growing a TiO2 nanorod array on FTO (Fluorinedoped Tin Oxide) glass directly by using a simple hydrothermal method, then, cladding the nanorod array with CdS quantum dots by using a continuous atomic layer adsorption and reaction method or depositing CdSe quantum dots on the nanorod array by using an electrochemical deposition method, and finally soaking a sample in dye N719 for 24 hours. By means of the quantum dot and dye synergistic sensitization, the solar cell is obviously increased in short-circuit current and obviously enhanced in efficiency. The method disclosed by the invention is simple to operate, easy for experiment, low in cost and high in yield.
Description
Technical field
The invention belongs to sensitization nano-array technical field of solar batteries, particularly a kind of TiO in Hydrothermal Preparation
2On the nanometer stick array, utilize chemical method deposition quantum dot, with dyestuff it is carried out the preparation method of the solar cell of cooperated-sensitization again.
Background technology
People are more and more to the research of quantum dot sensitized solar cell in recent years; This mainly is the advantage that self is arranged because of it; (1) can control the shape and the size of quantum dot easily through the preparation method; Have very strong molar extinction coefficient (3) and can produce multiple exciton thereby regulate and control its energy gap (2), the efficient that these advantages make quantum dot sensitized solar cell can reach in theory will be higher than DSSC.The semiconductor that people use quantum size usually is CdS for example, CdSe, and LnP, PbS is adsorbed on TiO
2Do the light anode on the porous membrane.The incident light irradiation is on the light anode, and quantum dot absorbs visible light and produces exciton, and exciton is at quantum dot and TiO
2Separate at the interface, form light induced electron, light induced electron is at TiO
2Transmit between the nano particle, and remaining hole is caught by the oxidation-reduction pair in the electrolyte.The efficient of quantum dot sensitized solar cell is generally at 2-5%, and is more much lower than DSSC (reaching as high as 11.5%).Mainly be the raising that following several reasons has limited its efficient: quantum dot is more limited to absorption of visible light; The transmission rate of hole in quantum dot cell is lower; Light induced electron and electrolyte compound; And by the low fill factor, curve factor that electrode is caused.
The efficient of quantum dot sensitized solar cell is further improved; Enhancing is a practicable method to the absorption of sunlight; Make quantum dot sensitized solar cell reach maximum to absorption of visible light; One of method is exactly to join together two kinds of different extinction materials to use, and realizes synergy.Adsorb the just in time compound this design philosophy of one deck organic dyestuff again in the outside of quantum, and simple.
The TiO of one dimension
2Nanostructure is widely used in the sensitization solar battery because of it can effectively separate photoproduction exciton and excellent charge transmission.Fudan University discloses titanium dioxide nano-rod monocrystalline array film and preparation method thereof; The advantage of this invention is: the one dimension bar structure of titanium dioxide is that electronics provides direct transmission path; Can improve the transport property of electronics; With obtaining the bigger titanium dioxide nano-rod monocrystalline array film of specific area after the acetic acid dilution reduction acidity; Utilize short circuit electricity electric current and the electricity conversion of the DSSC of this array film encapsulation be improved largely (number of patent application 201010608428.6, publication number CN102122577A).But the solar cell that constitutes with this technology has only used conventional dye sensitization.
CdS and CdSe are that the performance that shown is best in these inorganic semiconductor sensitizers, and Peng and his partner have reported the quantum dot sensitized TiO with CdS
2Nano-tube array obtain 4.15% efficient.([1] Sun, WT; Yu, Y; Pan, HY; Gao, XF; Peng, LM, Journal of the American Chemical Society. 2008,130,4:1124.CdS quantum dots sensitized TiO2 nanotube-array photoelectrodes) Diguna reports with CdSe sensitization TiO
2Porous membrane obtains efficient 2.7%.[Diguna,LJ;?Shen,Q;?Kobayashi,J;?Toyoda,T,?Applied?Physics?Letters.?2007,91,2:023116.?High?efficiency?of?CdSe?quantum-dot-sensitized?TiO2?inverse?opal?solar?cells?]
The present invention utilizes TiO
2Nanometer stick array adopts quantum dot (CdS or CdSe) and dyestuff (N719) cooperated-sensitization as the light anode, thereby has further improved the efficient of battery.
Summary of the invention
The purpose of this invention is to provide a kind of quantum dot and dyestuff cooperated-sensitization TiO
2The preparation method of solar battery of nanometer stick array is intended to improve the electricity conversion of battery.
Solar battery structure of the present invention is mainly by clear glass FTO, TiO
2Pt electrode on nanometer stick array, many iodine electrolyte, the FTO electro-conductive glass constitutes, at TiO
2The CdS quantum dot and the N719 dyestuff that have added the ability cooperated-sensitization on the nanometer stick array; Perhaps at TiO
2The CdSe quantum dot and the N719 dyestuff that have added the ability cooperated-sensitization on the nanometer stick array.
Concrete technology with manufacturing solar cells of the present invention is following
1.FTO the surface preparation of electro-conductive glass.
Utilize four step rule that the FTO glass surface is cleaned up, promptly use deionized water successively, acetone, ethanol, deionized water be ultrasonic cleaning 15 min respectively, use drier for use then.
2.TiO
2The growth of nanometer stick array
Measure the deionized water of 8 ml and the concentrated hydrochloric acid of 8 ml (percentage by weight is 36.5%-38%), mix and stir 5 min, add the metatitanic acid four fourth fat of 0.2 ml, continue to stir 5 min.Transfer to mixed solution in the polytetrafluoroethylene jar (20 ml) that is placed with FTO glass (conducting film down), heat 10 h, just can obtain 3.4 μ m, orthotropic TiO at 150 ℃ drying boxes
2Nanometer stick array.In atmosphere to TiO
2Nanometer stick array carries out 500 ℃, the annealing of 2 h.
3. use quantum dot sensitized TiO
2Nanometer stick array
At TiO
2On the nanometer stick array, utilize the continuous atomic layer absorption and the method for reaction to deposit the CdS quantum dot.
TiO is arranged to length
2The substrate of nanometer stick array is immersed in the Cd (AC) of 0.3 M
22 min in the solution take out the back and use deionized water rinsing, put into the Na of 0.3 M again
22 min in the S solution take out the back and use deionized water rinsing, so are an infusion, circulate altogether 40 times.
The method of perhaps utilizing electrochemical deposition is at TiO
2Deposition one deck CdSe on the nanometer stick array.Prepare deposit solution earlier, i.e. 0.0125 M Cd (AC)
2(C
4H
6CdO
42H
2O), 0.0125 M Na
2SeSO
3, 0.025 M NTA (C
6H
6NO
6Na
3).With TiO
2Nanometer rods is a work electrode, and saturated calomel electrode (SCE) is a reference electrode, and the Pt sheet is to electrode, deposition CdSe.Deposition voltage is-1.2 V.
To the sample that makes 1 h that under 350 ℃ temperature, anneals, feed Ar during annealing and protect.
4. absorbing dye N719
Dyestuff N719 solution compound method: 0.035 g ~ 0.1 g dyestuff N719 solid is added in 100-200 ml acetonitrile/tert-butyl alcohol (V:V=1:1) solution, and at room temperature magnetic agitation is until clarification; Then, the quantum dot sensitized TiO of step 3 preparation
2Nanorod electrodes at room temperature is immersed in the above-mentioned dyestuff N719 solution, soaks 24 hours, makes the abundant adsorpting dye molecule of electrode, after the taking-up, dries after rinsing well with acetonitrile.
5. be assembled into battery
Electrolyte solution compound method: with 1.3-2.7 g 1-butyl-3-methyl iodate imidazoles iodine [BMII]; 0.1-0.6 g iodine [I2]; 0.1-0.3 g guanidinium isothiocyanate [GUSCN], 0.6-1.4 g 4-tert .-butylpyridine [TBP] is in 10-20 ml acetonitrile/valeronitrile (V:V=85:15) solution; Then, adopt the Pt/FTO conduct to electrode, the nano-electrode that step 4 was soaked encapsulates with the sarin film, is assembled into sandwich structure, and injects above-mentioned electrolyte.Sealing, 80-100 ℃ of baking 3-10 min.
Advantage of the present invention:
1, the present invention utilizes hydro thermal method directly on the FTO substrate, to grow TiO
2Nanometer stick array.TiO
2Nanometer stick array is that light induced electron provides vertical electron channel, and the specific surface of nanometer rods is bigger, can adsorb more quantum dot.This hydrothermal preparing process is simple, and is with low cost.
2. the present invention utilizes the continuous atomic layer absorption and the method for reaction to deposit the CdS quantum dot or utilize the method for electrochemical deposition to deposit CdSe, and CdSe and CdS are in all inorganic semiconductor sensitizers, and the performance that shows is best.The chemical prepn process of its use is simple, and than being easier to control.
3. utilize quantum dot and dyestuff cooperated-sensitization, dyestuff and quantum dot can absorb visible light simultaneously, have improved absorption of visible light, have increased the photoproduction exciton, thereby have improved efficient.
When with CdS and dyestuff N719 cooperated-sensitization, battery efficiency is 2.0%, all is greatly improved with CdS (0.57%) or independent N719 (0.97%) sensitization with respect to independent.
During with CdSe and dyestuff N719 cooperated-sensitization, battery efficiency is 1.2%, all is greatly improved with CdSe (0.34%) or independent N719 (0.97%) sensitization with respect to independent.
Description of drawings
Fig. 1 is the solar battery structure sketch map of forming with the present invention
Wherein, 1----clear glass, 2----conductive layer FTO, 3----TiO
2Nanometer stick array, 4----CdS quantum dot or CdSe quantum dot, the 5----N719 dyestuff, many iodine of 6----electrolyte, 7----are made in the Pt electrode on the FTO electro-conductive glass;
Fig. 2 is quantum dot sensitized front and back TiO of the present invention
2The ESEM picture of nanometer stick array.
Wherein scheming a is TiO
2The surface topography of nanometer stick array can be found out TiO
2Nanometer rods is vertically grown, and smooth surface, and the nanometer rods diameter is approximately between the 50 nm-100 nm.Figure b is TiO
2The SEM sectional view of nanometer stick array can find out that the length of nanometer rods is approximately 3.4 μ m.Figure c is TiO
2Nanometer rods has deposited the surface topography of nanometer stick array behind the CdS quantum dot, finds surperficial roughening, has explained that the CdS particle is wrapped on the nanometer rods.Figure d is TiO
2Nanometer rods has been wrapped up the surface topography of nanometer stick array behind the CdeS quantum dot.
Fig. 3 is with dyestuff of the present invention and CdS quantum dot cooperated-sensitization TiO
2The J-V curve of nanometer stick array and with independent sensitization properties of sample relatively (under the irradiation of AM 1.5 simulated solar irradiations, light intensity is 100 mW/cm
2).
Wherein scheming a is separately with dyestuff N719 sensitization TiO
2The J-V curve of nanometer rods, electricity conversion η are 0.97%, open circuit voltage V
OcBe 0.67 V, short circuit current I
ScBe 4.0 mA/cm
2Figure b is separately with CdS sensitization TiO
2The J-V curve of nanometer rods, its electricity conversion 0.57%, open circuit voltage V
OcBe 0.62 V, short circuit current I
ScBe 3.1 mA/cm
2, figure c is dyestuff N719 and CdS quantum dot cooperated-sensitization TiO
2The J-V curve of nanometer stick array, its electricity conversion η is 2.0%, open circuit voltage V
OcBe 0.64 V, short circuit current I
ScBe 11.2 mA/cm
2Relatively the J-V curve of three samples can find out that the sample short circuit current of quantum dot CdS and dyestuff cooperated-sensitization and efficient have significantly enhancing.
Fig. 4 is with dyestuff of the present invention and CdSe quantum dot cooperated-sensitization TiO
2The J-V curve of nanometer stick array and with independent sensitization properties of sample relatively (under the irradiation of AM 1.5 simulated solar irradiations, light intensity is 100 mW/cm
2).
Wherein scheming a is separately with dyestuff N719 sensitization TiO
2The J-V curve of nanometer rods, electricity conversion η are 0.97%, open circuit voltage V
OcBe 0.67 V, short circuit current I
ScBe 4.0 mA/cm
2Figure b is separately with CdSe sensitization TiO
2The J-V curve of nanometer rods, its electricity conversion 0.34%, open circuit voltage V
OcBe 0.60 V, short circuit current I
ScBe 2.2 mA/cm
2, figure c is dyestuff N719 and CdSe quantum dot cooperated-sensitization TiO
2The J-V curve of nanometer stick array, its electricity conversion η is 1.20%, open circuit voltage V
OcBe 0.41 V, short circuit current I
ScBe 9.1 mA/cm
2Relatively the J-V curve of three samples can find out that the sample short circuit current of quantum dot CdSe and dyestuff cooperated-sensitization and efficient have significantly enhancing.
Specific embodiments
1.FTO the surface preparation of electro-conductive glass.
Utilize four step rule that the FTO glass surface is cleaned up, promptly use deionized water successively, acetone, ethanol, deionized water be ultrasonic cleaning 15 min respectively, use drier for use then.
2.TiO2 the growth of nanometer stick array
Measure the deionized water of 8 ml and the concentrated hydrochloric acid of 8 ml (percentage by weight is 36.5%-38%), mix and stir 5 min, add the metatitanic acid four fourth fat of 0.2 ml, continue to stir 5 min.Transfer to mixed solution in the polytetrafluoroethylene jar (20 ml) that is placed with FTO glass (conducting film down), heat 10 h, just can obtain 3.4 μ m, orthotropic TiO at 150 ℃ drying boxes
2Nanometer stick array.In atmosphere to TiO
2Nanometer stick array carries out 500 ℃, the annealing of 2 h.
3. wrap up the CdS quantum dot
At TiO
2On the nanometer stick array, utilize the continuous atomic layer absorption and the method for reaction to deposit the CdS quantum dot.
TiO is arranged to length
2The nanometer stick array substrate is immersed in the Cd (AC) of 0.3 M
22 min in the solution take out the back and use deionized water rinsing, put into the Na of 0.3 M again
22 min in the S solution take out the back and use deionized water rinsing, so are an infusion, circulate altogether 40 times.To the sample that makes 1 h that under 350 ℃ temperature, anneals, feed Ar during annealing and protect.
4. absorbing dye N719
Dyestuff N719 solution compound method: 0.035 g ~ 0.1 g dyestuff N719 solid is added in 100-200 ml acetonitrile/tert-butyl alcohol (V:V=1:1) solution, and at room temperature magnetic agitation is until clarification; Then, the CdS sensitization TiO of step 3 preparation
2Nanorod electrodes at room temperature is immersed in the above-mentioned dyestuff N719 solution, soaks 24 hours, makes the abundant adsorpting dye molecule of electrode, after the taking-up, dries after rinsing well with acetonitrile.
5. be assembled into battery
Electrolyte solution compound method: with 1.3-2.7 g 1-butyl-3-methyl iodate imidazoles iodine [BMII]; 0.1-0.6 g iodine [I2]; 0.1-0.3 g guanidinium isothiocyanate [GUSCN], 0.6-1.4 g 4-tert .-butylpyridine [TBP] is in 10-20 ml acetonitrile/valeronitrile (V:V=85:15) solution; Then, adopt the Pt/FTO conduct to electrode, the nano-electrode that step 4 was soaked encapsulates with the sarin film, is assembled into sandwich structure, and injects above-mentioned electrolyte.Sealing, 80-100 ℃ of baking 3-10 min.
1.FTO the surface preparation of electro-conductive glass.
Utilize four step rule that the FTO glass surface is cleaned up, promptly use deionized water successively, acetone, ethanol, deionized water be ultrasonic cleaning 15min respectively, uses drier for use then.
2.TiO
2The growth of nanometer stick array
Measure the deionized water of 8 ml and the concentrated hydrochloric acid of 8 ml (percentage by weight is 36.5%-38%), mix and stir 5 min, add the metatitanic acid four fourth fat of 0.2 ml, continue to stir 5 min.Transfer to mixed solution in the polytetrafluoroethylene jar (20 ml) that is placed with FTO glass (conducting film down), heat 10 h, just can obtain 3.4 μ m, orthotropic TiO at 150 ℃ drying boxes
2Nanometer stick array.In atmosphere to TiO
2Nanometer stick array carries out 500 ℃, the annealing of 2 h.
3. wrap up the CdSe quantum dot
At TiO
2On the nanometer stick array, utilize the method deposition CdSe quantum dot of electrochemical deposition.
Dispose the Na of 0.025 M earlier
2SO
3Solution adds Se (0.0125 M) powder, and 4 h are stirred in 70 ℃ of waters heating, and Se is dissolved fully, obtain Na
2SeSO
3Solution adds C then
4H
6CdO
42H
2O (0.0125 M) adds 0.025 M nitrilotriacetic acid trisodium salt (NTA, C at last
6H
6NO
6Na
3) carry out pH value adjusting with TiO
2Nanometer stick array is a work electrode, and saturated calomel electrode (SCE) is a reference electrode, and the Pt sheet is to electrode, deposition CdSe shell.The deposition electric energy control is at 0.6 C, and deposition voltage is-1.2 V.To the sample that makes 1 h that under 350 ℃ temperature, anneals, feed Ar during annealing and protect.
4. absorbing dye N719
Dyestuff N719 solution compound method: 0.035 g ~ 0.1 g dyestuff N719 solid is added in 100-200 ml acetonitrile/tert-butyl alcohol (V:V=1:1) solution, and at room temperature magnetic agitation is until clarification; Then, at room temperature be immersed in the CdS sensitization TiO2 nanorod electrodes of step 3 preparation in the above-mentioned dyestuff N719 solution, soaked 24 hours, make the abundant adsorpting dye molecule of electrode, after the taking-up, dry after rinsing well with acetonitrile.
5. be assembled into battery
Electrolyte solution compound method: with 1.3-2.7 g 1-butyl-3-methyl iodate imidazoles iodine [BMII]; 0.1-0.6 g iodine [I2]; 0.1-0.3 g guanidinium isothiocyanate [GUSCN], 0.6-1.4 g 4-tert .-butylpyridine [TBP] is in 10-2 ml acetonitrile/valeronitrile (V:V=85:15) solution; Then, adopt the Pt/FTO conduct to electrode, the nano-electrode that step 4 was soaked encapsulates with the sarin film, is assembled into sandwich structure, and injects above-mentioned electrolyte.Sealing, 80-100 ℃ was toasted 3-10 minute.
Claims (3)
1. the TiO of quantum dot and dyestuff cooperated-sensitization
2The nanometer stick array solar cell, mainly by
Clear glass FTO (1), conducting film (2), TiO
2Pt electrode (7) on nanometer stick array (3), many iodine electrolyte (6), the FTO electro-conductive glass (2) constitutes, and it is characterized in that at TiO
2The CdS quantum dot (4) and the N719 dyestuff (5) that have added the ability cooperated-sensitization on the nanometer stick array (3); Perhaps at TiO
2The CdSe quantum dot and the N719 dyestuff (5) that have added the ability cooperated-sensitization on the nanometer stick array (3).
2. the TiO of quantum dot and dyestuff cooperated-sensitization
2The nanometer stick array preparation method of solar battery is characterized in that step is:
1)The surface preparation of FTO electro-conductive glass
Utilize four step rule that the FTO glass surface is cleaned up, promptly use deionized water successively, acetone, ethanol, deionized water be ultrasonic cleaning 15 min respectively, use drier for use then;
2) TiO
2The growth of nanometer stick array
The deionized water and the 8 ml percentage by weights of measuring 8 ml are the concentrated hydrochloric acid of 36.5%-38%; Mix and stir 5 min; The metatitanic acid four fourth fat that add 0.2 ml continue to stir 5 min, transfer to mixed solution in the polytetrafluoroethylene jar that is placed with FTO glass (conducting film down); Drying box heating 10～24 h at 150～200 ℃ obtain the orthotropic TiO of 3.4～5 μ m
2Nanometer stick array; In atmosphere to TiO
2Nanometer stick array carries out 500 ℃, the annealing of 2 h;
3) use quantum dot sensitized TiO
2Nanometer stick array
TiO is arranged to growth
2The substrate of nanometer stick array is immersed in the Cd (AC) of 0.3 M
22 min in the solution take out the back and use deionized water rinsing, put into the Na of 0.3 M again
22 min in the S solution take out the back and use deionized water rinsing, so are an infusion, circulate altogether 40 times;
To the sample that makes 1 h that under 350 ℃ temperature, anneals, feed Ar during annealing and protect;
4) absorbing dye N719
The preparation of dyestuff N719 solution is added to 0.035 g ~ 0.1 g dyestuff N719 solid in the acetonitrile/t-butanol solution of 100-200 ml by V:V=1:1, and at room temperature magnetic agitation is until clarification; Then, the quantum dot sensitized TiO of step 3 preparation
2Nanorod electrodes at room temperature is immersed in the above-mentioned dyestuff N719 solution, soaks 24 hours, makes the abundant adsorpting dye molecule of electrode, after the taking-up, rinses well and dries with acetonitrile;
5) be assembled into battery
Electrolyte solution compound method: with 1.3-2.7 g 1-butyl-3-methyl iodate imidazoles iodine [BMII]; 0.1-0.6 g iodine [I2]; 0.1-0.3 g guanidinium isothiocyanate [GUSCN], 0.6-1.4 g 4-tert .-butylpyridine [TBP] is in acetonitrile/valeronitrile solution of 10-20 ml V:V=85:15; Then, adopt the Pt/FTO conduct to electrode, the nano-electrode that step 4 was soaked encapsulates with the sarin film, is assembled into sandwich structure, and injects above-mentioned electrolyte, sealing, 80-100 ℃ of baking 3-10 min.
3. the TiO of a kind of quantum dot according to claim 2 and dyestuff cooperated-sensitization
2The nanometer stick array preparation method of solar battery is characterized in that step 3) is to utilize the method for electrochemical deposition at TiO
2Deposition one deck CdSe on the nanometer stick array is with TiO
2Nanometer rods is a work electrode, and saturated calomel electrode (SCE) is a reference electrode, and the Pt sheet is to electrode, deposition CdSe; Deposition voltage is-1.2 V; The preparation of deposit solution, i.e. 0.0125 M Cd (AC)
2(C
4H
6CdO
42H2O), 0.0125 M Na
2SeSO
3, 0.025 M NTA (C
6H
6NO
6Na
3); To the sample that makes 1 h that under 350 ℃ temperature, anneals, feed Ar during annealing and protect.
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