CN104752063A - Porous TiO2 nanocrystalline thin film with three-dimensional nanorod film chip structure, preparation method and application - Google Patents
Porous TiO2 nanocrystalline thin film with three-dimensional nanorod film chip structure, preparation method and application Download PDFInfo
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- CN104752063A CN104752063A CN201510169979.XA CN201510169979A CN104752063A CN 104752063 A CN104752063 A CN 104752063A CN 201510169979 A CN201510169979 A CN 201510169979A CN 104752063 A CN104752063 A CN 104752063A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
Abstract
The invention provides a porous TiO2 nanocrystalline thin film with a three-dimensional nanorod film chip structure, a preparation method and an application of the porous TiO2 nanocrystalline thin film serving as a dye-sensitized solar cell photo-anode, and belongs to the technical field of dye-sensitized solar cells. A dye-sensitized solar cell consists of anode conductive glass FTO, a photo-anode, electrolyte solution (I-/I3-) and a Pt counter electrode; and the electrolyte solution is injected in the cell through a vacuum backfilling method. The structure of the dye-sensitized solar cell is shown in a figure I. The porous TiO2 nanocrystalline thin film is characterized in that the material of the photo-anode is the porous TiO2 nanocrystalline thin film with the novel three-dimensional nanorod film chip structure, the porous TiO2 nanocrystalline thin film has a high light scattering effect, the utilization rate of incident light can be improved, a nanorod array and a nanochip structure on the bottom layer provide an efficient conduction path for electrons, and the photo electron collecting efficiency of the photo-anode is improved. The photoelectric conversion efficiency of the TiO2 nanocrystalline thin film is 8.41% and is higher than that of a battery of which the photo-anode is made of P25 by 51.8%.
Description
Technical field
The invention belongs to DSSC technical field, be specifically related to a kind of porous TiO of novel three-dimensional nanometer rods sheet floral structure
2nano-crystal film, preparation method and as the application in dye-sensitized solar cell anode.
Background technology
Along with the continuous aggravation of energy crisis, solar energy is more and more subject to the extensive concern in the whole world as most important a kind of green energy resource.In effective utilization of solar energy, solar cell is research field with fastest developing speed, most active at present.DSSC (DSSCs) be a kind ofly have that manufacture craft is simple, with low cost, the solar cell of new generation of good stability and efficiency high, by the Michael of Lausanne, SUI engineering college
professor etc. utilizes bipyridyl ruthenium (II) Complex dyes and porous TiO
2nano-crystal film was successfully prepared first in 1991.Its photoelectric conversion efficiency under the solar light irradiation of AM1.5 reaches 7.1% breakthroughly.Through the research of twenties years, the photoelectric conversion efficiency of DSSC brought up to more than 11% further, thus substantially increased the confidence of people to DSSC industrialized development.
In a typical DSSCs, the light anode material of dye sensitization by absorbing sunlight, and produces free electron.Therefore light anode material choose the capture rate thus the photovoltaic performance of decision battery that directly affects sunlight.N type semiconductor oxide TiO
2nano-crystal film carries the task such as scattering of the absorption of dyestuff, the transmission of electronics and incident light as the most important smooth anode material of DSSC.Owing to changing TiO at nano-scale
2pattern effectively can improve TiO
2the electron transfer rate of nano-crystal film, the characteristics such as incident light utilization ratio and Dye Adsorption amount, so at present for the porous TiO with special appearance
2the research of nano-crystal film becomes one of Main way of DSSC research.There is the three-dimensional TiO of bigger serface
2nanostructure, such as nanosphere, nano flower etc., its Dye Adsorption ability is strong, and has well light scattering, but owing to having complicated grain boundary structure between three-dimensional nanometer material, its electron transfer rate is generally poor than the nanostructure of one dimension.Therefore, design and synthesis has the novel three-dimensional TiO of high electron transfer rate and bigger serface
2nano material becomes the object that dye-sensitized solar cell anode material is pursued, and has far-reaching Research Significance and application prospect widely.
Summary of the invention
The object of this invention is to provide a kind of porous TiO with novel three-dimensional nanometer rods sheet floral structure
2nano-crystal film, its preparation method and this material are as the application in dye-sensitized solar cell anode.The porous TiO that the method is obtained
2nano-crystal film can also be widely used in the other fields such as photocatalysis, photochemistry, lithium battery.
DSSC of the present invention, by FTO electro-conductive glass, electrolyte solution (I
-/ I
3 -), the porous TiO of three-dimensional manometer rod sheet floral structure
2nano-crystal film and Pt form electrode, the porous TiO of three-dimensional manometer rod sheet floral structure
2nano-crystal film growth is on the FTO conducting film of FTO electro-conductive glass, and electrolyte solution is (by 0.3M DMPII, 0.05M I
2, 0.5M LiI, 0.5M 4-TBP be dissolved in acetontrile and form) method that backfilled by vacuum is injected in the closed area be made up of electrode FTO conducting film and Pt.The porous TiO of this novel three-dimensional nanometer rods sheet floral structure
2nano-crystal film has special loose structure, by effectively absorbing incident light to the Multiple Scattering effect of light, thus can increase substantially the utilance of incident light, reaching the object improving photoelectric conversion efficiency.
A kind of porous TiO with novel three-dimensional nanometer rods sheet floral structure of the present invention
2the preparation method of nano-crystal film, its step is as follows:
(1) measure 2 ~ 6mL hydrochloric acid (concentration 30 ~ 40wt.%) (Beijing fine chemistry Co., Ltd), join in 6mL deionized water, magnetic agitation 20 ~ 30min;
(2) measure 0.2 ~ 0.4mL butyl titanate (Beijing fine chemistry Co., Ltd), join in the solution that step (1) obtains, magnetic agitation 30 ~ 60min;
(3) pouring the mixed solution that step (2) obtains into liner is in the autoclave of polytetrafluoroethylene, the FTO electro-conductive glass (NHTechno company) cleaned is immersed in this mixed solution, and the FTO conducting film of FTO electro-conductive glass is lain at the bottom of still upward; React 2 ~ 5h at 160 ~ 200 DEG C after, treat that it naturally cools to room temperature, can grow on FTO electro-conductive glass and obtain the TiO that one deck thickness is 16 ~ 30 μm
2nano-crystal film;
(4) by TiO
2nano-crystal film respectively rinses 3 ~ 5 times with deionized water and ethanol respectively, then washed product is dried 4 ~ 8h under the vacuum condition of 60 ~ 80 DEG C, finally at 450 ~ 500 DEG C, calcines 1 ~ 2h;
(5) the product film one that step (4) obtains is faced up in the autoclave being immersed in containing 20 ~ 30mL, 6 ~ 10mol/L NaOH solution, react after 2 ~ 4 hours at 160 ~ 200 DEG C, naturally cool to room temperature;
(6) product step (5) obtained immerses 30 ~ 50mL, 0.2 ~ 0.3mol/L HNO
330 ~ 60min in solution, takes out rear deionized water and ethanol respectively rinses 3 ~ 5 times, and dries 4 ~ 8 hours under the vacuum condition of 60 ~ 80 DEG C; Finally at 450 ~ 500 DEG C, calcine 1 ~ 2h, the porous TiO with novel three-dimensional nanometer rods sheet floral structure of the present invention after taking-up, can be obtained on FTO
2nano-crystal film.
The invention provides a kind of porous TiO
2nano-crystal film, it prepares gained by said method.In its XRD phenogram (Fig. 3), 2 θ have obvious diffraction maximum at 27.44,36.04,39.28,41.36,44.16,54.40,56.52,62.77,69.02 and 69.90 places respectively, and known from standard card is rutile structure (JCPDS no.21-1276).
The porous TiO of novel three-dimensional nanometer rods sheet floral structure of the present invention
2nano-crystal film is made up of three kinds of nanostructures: monodimension nano stick array, two-dimensional nano sheet and three-dimensional manometer flower.The nanometer stick array that length is about 3 ~ 5 μm is grown directly upon FTO surface, effectively can improve TiO
2the electron transfer rate of nano-crystal film.Nano flower diameter is about 6 ~ 8 μm, is made up of many nanometer rods, and it is formed in reaction solution, is deposited on gradually on nanometer stick array under high temperature and high pressure environment.Nanometer sheet is reacted by the NaOH solution of nano flower and high concentration and is grown by the mode of recrystallization and forms, the final graduate three-dimensional manometer rod sheet floral structure formed as shown in Figure 2.The unique texture of this nano flower has loose porous characteristic, is conducive to the Dye Adsorption amount increasing light anode, and strengthens the scattering process to light, thus effectively improve the capture rate of light.The flaky nanometer structure generated by nano flower, has with the nanometer stick array of nano flower and bottom and is cross-linked closely, can provide how efficient conducting path for electronics, contributes to the collection efficiency improving light induced electron.Based on above advantage, with this porous TiO
2nano-crystal film is that light anode will improve the photoelectric conversion efficiency of battery greatly.
Advantage of the present invention: this preparation method has the advantage that experimental technique is simple, cost is low and the cycle is short.The TiO of preparation
2material can be applied to DSSC as light anode, is assembled into the photoelectric conversion efficiency (PCE) that battery obtains and can reaches 8.41%, than with commercial TiO
2(P25) battery prepared for light anode material improves 51.8%.
Accompanying drawing explanation
Fig. 1: DSSC structural representation of the present invention; As shown in Figure 1, each component names is: ammeter 1, has the porous TiO of novel three-dimensional nanometer rods sheet floral structure
2nano-crystal film 2, Pt to electrode 3, electrolyte solution (I
-/ I
3 -) 4, FTO electro-conductive glass 5 (its FTO conducting film upward).
Fig. 2: porous TiO prepared by the embodiment of the present invention 1
2the scanning electron microscopic picture of nano-crystal film; Wherein Fig. 2 (a) is end view, and Fig. 2 (b) is vertical view, and illustration is partial enlarged drawing.
Fig. 3: porous TiO prepared by the embodiment of the present invention 1
2the XRD figure of nano-crystal film; From standard card, this material known is rutile structure (JCPDS no.21-1276).The crystallinity of its height contributes to the conduction efficiency improving electronics.
Fig. 4: commercial TiO
2(P25) and the embodiment of the present invention 1 prepare TiO
2(TNRSF) light absorption spectrogram; In visible wavelength range (400 ~ 800nm), the absorptivity of TNRSF is apparently higher than P25, and this mainly has stronger scattering process due to TNRSF to light, and can adsorb more dyestuff.
Fig. 5: commercial TiO
2(P25) and the embodiment of the present invention 1 prepare TiO
2(TNRSF) electrochemical impedance spectrogram (EIS); Wherein Fig. 5 (a) is Nyquist diagram, and Fig. 5 (b) is Bode diagram.In Fig. 5 (a), illustration is the equivalent circuit diagram that impedance spectrogram is corresponding.Can find out that from Fig. 5 (a) every bar curve has two semicircular, the wherein transfer impedance of the corresponding electronics of small semicircle between counter electrode of battery and electrolyte, the corresponding electronics of large semicircle is in battery light anode, transfer impedance between dyestuff and electrolyte.Semicircle radius larger expression transfer impedance is larger, and namely electric transmission is slower.Therefore can infer that electronics transmits in TNRSF photo-anode film faster.Simultaneously corresponding according to first peak value of curve in Fig. 5 (b) frequency values, can be similar to the life-span (τ obtaining electronics
e=1/2 π f
max).The f that TNRSF and P25 is corresponding
maxbe 5.6Hz and 11.2Hz respectively, namely their electron lifetime is 28.4ms and 14.2ms respectively, illustrates that electronics transmits in TNRSF film farther, is more conducive to the collection of light anode to electronics, thus significantly improves photoelectric current.
Fig. 6: with commercial TiO
2(P25) and the embodiment of the present invention 1 prepare TiO
2(TNRSF) the J-V figure of the battery prepared as light anode; As shown in the figure, TNRSF and P25 battery has almost identical open circuit voltage (V
oc), but the short circuit current (J of TNRSF battery
sc) then by 13.56mA/cm
2(P25) 16.95mA/cm is brought up to
2.
Embodiment
Embodiment 1: with the porous TiO of two-step hydrothermal route legal system for novel three-dimensional nanometer rods sheet floral structure
2nano-crystal film, detailed process is as follows
(1) measure 4mL hydrochloric acid (concentration 36wt.%) (Beijing fine chemistry Co., Ltd), join in 6mL deionized water, magnetic agitation 20min;
(2) measure 0.3mL butyl titanate (Beijing fine chemistry Co., Ltd), join in mixed solution described in step (1), magnetic agitation 60min is until solution clarification;
(3) mixed solution in step (2) being poured into liner is in the 45mL autoclave of polytetrafluoroethylene, and by clean FTO electro-conductive glass (the specification 2.2mm after a slice priority acetone and deionized water each ultrasonic cleaning 30min, resistance 14 Europe, light transmittance 90%, NHTechno company) be immersed in this mixed solution, conducting surface lies at the bottom of still upward.React 3 hours at 180 DEG C, treat that it naturally cools to room temperature, can grow on FTO electro-conductive glass and obtain the TiO that one deck thickness is about 28 μm
2nano-crystal film;
(4) by TiO
2nano-crystal film respectively rinses 3 times with deionized water and ethanol respectively, then washed product is dried 6h under the vacuum condition of 80 DEG C, finally at 500 DEG C, calcines 1h.
(5) faced up by the product film one that step (4) obtains in the 45mL autoclave being placed on containing 30mL, 10mol/LNaOH solution, react after 4 hours at 180 DEG C, it naturally cools to room temperature.
(6) product step (5) obtained immerses 45mL, 0.2mol/L HNO
345min in solution, takes out rear deionized water and ethanol respectively rinses 3 times, and dries 6 hours under the vacuum condition of 80 DEG C.Finally at 500 DEG C, calcine 2h, the porous TiO with novel three-dimensional nanometer rods sheet floral structure of the present invention after taking-up, can be obtained on FTO
2nano-crystal film.
Table 1: the EIS fitting parameter contrast of the two kinds of DSSC prepared for light anode with P25 and TNRSF respectively.
What list in table 1 is the fit parameter values of EIS spectrogram equivalent electric circuit, wherein R
1the series resistance of battery, R
2the transfer impedance between electrolyte-Pt electrode-electro-conductive glass FTO, R
3tiO
2transferring charge impedance between-dyestuff-electrolyte, τ
ebe electron lifetime, they have reacted the electron transport property of battery.Be that the battery table of light anode material reveals better charge-conduction ability as can be seen from Table 1 with TNRSF, be conducive to the collection efficiency improving battery light induced electron.
Table 2: every battery performance contrast of the two kinds of DSSC prepared for light anode with P25 and TNRSF respectively.
List respectively with P25 with take TNRSF as the performance parameter of battery of light anode material in table 2, wherein J
scshort circuit current, V
ocbe open circuit voltage, FF is fill factor, curve factor, and η is photoelectric conversion efficiency; Dyeadsorption is the amount of dye of light anode absorption in dye sensitization process.Use TNRSF as light anode material as can be seen from Table 2, effectively can improve the photovoltaic property of battery, thus improve the photoelectric conversion efficiency of battery.
Claims (3)
1. the porous TiO of a three-dimensional manometer rod sheet floral structure
2the preparation method of nano-crystal film, its step is as follows:
(1) measure the hydrochloric acid of 2 ~ 6mL, concentration 30 ~ 40wt.%, join in 6mL deionized water, magnetic agitation 20 ~ 30min;
(2) measure 0.2 ~ 0.4mL butyl titanate, join in the solution that step (1) obtains, magnetic agitation 30 ~ 60min;
(3) mixed solution that step (2) obtains is poured in autoclave, clean FTO electro-conductive glass is immersed in this mixed solution, and the FTO conducting film of FTO electro-conductive glass is lain at the bottom of still upward; React 2 ~ 5h at 160 ~ 200 DEG C after, treat that it naturally cools to room temperature, can grow on FTO electro-conductive glass and obtain the TiO that one deck thickness is 16 ~ 30 μm
2nano-crystal film;
(4) by TiO
2nano-crystal film respectively rinses 3 ~ 5 times with deionized water and ethanol respectively, then washed product is dried 4 ~ 8h under the vacuum condition of 60 ~ 80 DEG C, finally at 450 ~ 500 DEG C, calcines 1 ~ 2h;
(5) the product film one that step (4) obtains is faced up in the autoclave being immersed in containing 20 ~ 30mL, 6 ~ 10mol/L NaOH solution, react after 2 ~ 4 hours at 160 ~ 200 DEG C, naturally cool to room temperature;
(6) product step (5) obtained immerses 30 ~ 50mL, 0.2 ~ 0.3mol/L HNO
330 ~ 60min in solution, takes out rear deionized water and ethanol respectively rinses 3 ~ 5 times, and dries 4 ~ 8 hours under the vacuum condition of 60 ~ 80 DEG C; Finally at 450 ~ 500 DEG C, calcine 1 ~ 2h, the porous TiO with novel three-dimensional nanometer rods sheet floral structure of the present invention after taking-up, can be obtained on FTO
2nano-crystal film.
2. a poriferous titanium dioxide nano-crystal film for three-dimensional manometer rod sheet floral structure, is characterized in that: prepared by method according to claim 1.
3. the poriferous titanium dioxide nano-crystal film of a kind of three-dimensional manometer rod sheet floral structure according to claim 2 is as the application in dye-sensitized solar cell anode.
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Cited By (4)
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| CN105702472A (en) * | 2016-01-25 | 2016-06-22 | 北京大学深圳研究院 | Solar cell electrode, preparation method therefor, and solar cell |
| CN106587282A (en) * | 2016-12-08 | 2017-04-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Difunctional multi-template molecularly imprinted type photoelectric anode material and preparation method and application |
| CN108840579A (en) * | 2018-08-02 | 2018-11-20 | 合肥工业大学 | A kind of superfine Ti O2Nano crystal array and preparation method thereof |
| CN112079576A (en) * | 2020-09-15 | 2020-12-15 | 闽江学院 | Carbon nitride material, in-situ preparation method thereof and application of carbon nitride material in perovskite solar cell |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105702472A (en) * | 2016-01-25 | 2016-06-22 | 北京大学深圳研究院 | Solar cell electrode, preparation method therefor, and solar cell |
| CN106587282A (en) * | 2016-12-08 | 2017-04-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Difunctional multi-template molecularly imprinted type photoelectric anode material and preparation method and application |
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| CN112079576A (en) * | 2020-09-15 | 2020-12-15 | 闽江学院 | Carbon nitride material, in-situ preparation method thereof and application of carbon nitride material in perovskite solar cell |
| CN112079576B (en) * | 2020-09-15 | 2022-04-01 | 闽江学院 | Carbon nitride material, in-situ preparation method thereof and application of carbon nitride material in perovskite solar cell |
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Application publication date: 20150701 |