CN101944439A - Preparation method for TiO2 nanometer rod array of dye sensitized solar cell - Google Patents

Preparation method for TiO2 nanometer rod array of dye sensitized solar cell Download PDF

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CN101944439A
CN101944439A CN2009101578751A CN200910157875A CN101944439A CN 101944439 A CN101944439 A CN 101944439A CN 2009101578751 A CN2009101578751 A CN 2009101578751A CN 200910157875 A CN200910157875 A CN 200910157875A CN 101944439 A CN101944439 A CN 101944439A
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gas
preparation
pressure
substrate
tio
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李�灿
孟立建
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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
    • Y02E10/549—Organic PV cells
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention relates to a preparation method for a TiO2 nanometer rod array of a dye sensitized solar cell. The TiO2 nanometer rod array of the dye sensitized solar cell is prepared by a DC reaction magnetron sputtering method. The method comprises the following steps of: putting a substrate surface into a DC reaction magnetron sputtering device and vacuumizing until the pressure is less than 1*10<3>Pa, wherein Ar gas is taken as sputtering gas and O2 gas is taken as reaction gas; and controlling the pressure of the reaction gas at 0.09 to 1P, the pressure of the sputtering gas at 1 to 5Pa, the sputtering power at 200 to 250w, and the distance from a target to the substrate at 40 to 80mm. The method prepares the TiO2 nanometer rod array by controlling the technological conditions such as the gas pressure, the substrate temperature, the sputtering power and the distance from the target to the substrate. The TiO2 nanometer rod prepared by the method has high preferred orientation along 220, and a highest photovoltaic conversion efficiency of 5.24 percent when applied to the dye sensitized solar cell.

Description

The TiO that is used for DSSC 2The method for making of nanometer stick array
Technical field
The invention belongs to DSSC material preparation and application, relate to a kind of TiO of DSSC particularly 2The preparation method of nanometer stick array.
Background technology
1991, Switzerland scientist Gratzel nanoporous Ti O2 films have prepared a kind of novel solar battery as optoelectronic pole, are called DSSC, and the efficient that is obtained reaches 7%, and the efficient of present this battery has surpassed 11%.In the last few years, nanocrystalline TiO 2Be applied in widely on DSSC (DSSC) device as electrode material.The energy conversion efficiency of DSSC and TiO 2The character of thin-film material has very big association, and it comprises specific area, porosity, the scattering of light performance of film and the TiO that constitutes the nanometer crystal film material 2Crystal formation, particle diameter etc.Titanium dioxide has three kinds of common crystal formations, i.e. anatase, brockite and rutile.Battery with anatase structured titanium dioxide nanocrystalline material preparation has photoelectric conversion efficiency preferably.But TiO for a long time 2The preparation of film depends on sol-gel method, to TiO 2The controllability imperfection of film, repeatability bad, the preparation nanocrystalline TiO 2Also be unordered, all these is unfavorable for the raising of DSSC efficient.The TiO of chemical method preparation 2Nanometer rods and nano-tube array also have been used on the DSSC, and its advantage is that nanometer rods or nano-tube array have bigger surface area, helps the absorption of dyestuff.In addition, the TiO of these one-dimensional nano structures 2Also help improving electron transport property and then improving photoelectric conversion efficiency.Yet these chemical methodes are difficult to be used for preparing the repeatable uniformly TiO of large tracts of land 2Nanometer stick array.
The reaction magnetocontrol sputtering technology is a kind of industrial technology that is fit to, and magnetron sputtering is a kind of low-temperature physics film technique, can be under cryogenic conditions the dynamic process of deposition ion by having certain energy form TiO 2Film, thereby can in film forming, not have residual organic impurities because of chemical method.Advantage such as have in addition that the film forming area is big, film and base material adhesion height, film forming are even, can produce continuously.In addition, this film formation at low temp technology can also be used to deposition of titanium oxide film on organic flexible substrate.Yet there are no any relevant report for preparing titanic oxide nanorod array with sputtering technology up till now.
Summary of the invention
The purpose of this invention is to provide the simple DSSC TiO of a kind of technology 2The preparation method of nanometer stick array.
The present invention utilizes the direct current reaction magnetron sputtering technology to prepare TiO 2The method of nanometer stick array is also used it for DSSC, can carry out according to following technical proposals:
Earlier clean substrate (glass, ITO electro-conductive glass or FTO electro-conductive glass) is put into the vacuum chamber of direct current reaction magnetron sputtering device, vacuum chamber is evacuated to less than 1 * 10 -3Pa, sputter gas and reaction gas pressure independently control respectively (with Ar gas as sputter gas, O 2Gas is as reacting gas).O 2Reacting gas is incorporated into substrate surface by an extra pipeline, and is 0.09-1Pa at oxygen pressure, and sputter pressure is 1-5Pa, and sputtering power is 200-250W, and target carries out direct current reaction magnetron sputtering growth TiO during for 40-80mm to the distance of substrate 2Nanometer stick array.
Advantage of the present invention is:
1) equipment is simple, and is easy to operate.
2) favorable repeatability.
3) adopt the direct current reaction magnetron sputtering method, TiO can large tracts of land evenly grows 2Nanometer stick array.
4) use metal targets easy to prepare.
5) TiO of the inventive method preparation 2Nanometer rods has very strong (220) preferred orientation.
Description of drawings
Fig. 1 is the TiO with the inventive method preparation 2The field emission scanning electron microscope photo of nanometer stick array.
Fig. 2 is the TiO for preparing with the inventive method on the ITO electro-conductive glass 2The X-ray diffractogram of nanometer stick array, X axis are the angle of diffraction (2 θ), and Y-axis is intensity (a.u.).
Fig. 3 is the TiO for preparing with the inventive method when distance is for 40mm between the target substrate 2The field emission scanning electron microscope photo of nanometer stick array.
Fig. 4 is the TiO for preparing with the inventive method when distance is for 80mm between the target substrate 2The field emission scanning electron microscope photo of nanometer stick array.
Fig. 5 is pressure TiO with the inventive method preparation when being 5Pa 2The field emission scanning electron microscope photo of nanometer stick array.
Fig. 6 is pressure TiO with the inventive method preparation when being 1Pa 2The field emission scanning electron microscope photo of nanometer stick array.
Fig. 7 is the TiO with the preparation in 6 hours of the inventive method deposition 2The field emission scanning electron microscope photo of nanometer stick array (nanometer rods length is about 3 microns).
Fig. 8 is the TiO with the preparation in 15 hours of the inventive method deposition 2The field emission scanning electron microscope photo of nanometer stick array (nanometer rods length is about 8 microns).
Embodiment
In order to further specify the present invention, enumerate following embodiment.
Embodiment 1: the preparation method with (220) preferred orientation anatase titania nanometer rods
Clean ITO Conducting Glass is placed the 70mm place, top of vacuum chamber sputtering target, and the control base vacuum is less than 1 * 10 -3Pa does not additionally heat substrate.
Reconcile various splash-proofing sputtering process parameters and carry out sputter, before formal deposition, pre-sputter 20 minutes, concrete technological parameter is:
Reacting gas O 2Air pressure be by force 2.5 * 10 -1Pa, the air pressure of sputter gas Ar are by force 2Pa, sputtering current 0.56A, and sputtering power 235W, sputtering time is 14 hours, obtains the TiO that thickness is about 2 microns 2Nanometer stick array, as shown in Figure 1.Nanometer stick array has very strong anatase (220) orientation, as shown in Figure 2.
Embodiment 2: the preparation method of the titanic oxide nanorod array of different-diameter
The distance that changes target and substrate is from 40mm to 80mm, and other deposition parameter obtains the TiO of different-diameter with embodiment 1 2Nanometer stick array.Fig. 3 and Fig. 4 are respectively the surface topography photo of the nanometer stick array for preparing when distance is for 40mm and 80mm between the target substrate.According to present embodiment as can be seen, the diameter of nanometer rods arrives the shortening of substrate distance along with target and increases to some extent, thereby a kind of method that can control the nanometer rods diameter is provided.
Embodiment 3: one of preparation method of the titanic oxide nanorod array of different-shape
Keep O 2Air pressure is by force 3.1 * 10 -1Pa, sputtering current 0.52A, target and substrate distance are 50mm, the pressure that changes sputtering pressure will obtain the TiO of different-shape and different-diameter from 1Pa to 5Pa 2Nanometer stick array.Fig. 5 and Fig. 6 are respectively the surface topography of the nanometer stick array for preparing when sputter pressure is 5Pa and 1Pa.
Embodiment 4: the preparation method of the nanometer stick array of different length
Keep O 2Air pressure is by force 2.5 * 10 -1Pa, sputtering current 0.56A, target and substrate distance are 40mm, sputter pressure 2Pa changes sedimentation time, obtains the TiO of different length 2Nanometer stick array.Fig. 7 and Fig. 8 are respectively the sectional view that sedimentation time is the nanometer stick array of 6 hours (nanometer rods length is about 3 microns) and 15 hours (nanometer rods length is about 8 microns) preparation.
Embodiment 5: the preparation DSSC
Nanometer stick array baking under 80 degree of embodiment 1 preparation was immersed in then in the N719 dyestuff of 0.5mM the room temperature sensitization in 30 minutes 24 hours, above-mentioned electrode and Pt are assembled into DSSC to the acetonitrile solution of electrode, LiI and I2, and maximum light conversion efficiency reaches 5.24%.

Claims (5)

1. one kind prepares the TiO that is used for DSSC 2The method of nanometer stick array utilizes the direct current reaction magnetron sputtering method to be prepared, and key step is as follows:
Substrate surface is put into the direct current reaction magnetron sputtering device, be evacuated to less than 1 * 10 -3Pa, sputter gas and reaction gas pressure are controlled respectively; The pressure of reacting gas is 0.09-1P, and the pressure of sputter gas is 1-5Pa, and sputtering power is 200-250W, and target is 40-80mm to the distance of substrate.
2. preparation method according to claim 1, wherein, substrate is ITO electro-conductive glass, FTO electro-conductive glass or glass.
3. preparation method according to claim 1, wherein, sputter gas is Ar, reacting gas is O 2
4. preparation method according to claim 1, wherein, the material of target is a purity greater than 99.9% Ti metal.
5. preparation method according to claim 1, wherein, reacting gas and sputter gas are controlled by mass flowmenter respectively.
CN2009101578751A 2009-07-09 2009-07-09 Preparation method for TiO2 nanometer rod array of dye sensitized solar cell Pending CN101944439A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103325577A (en) * 2013-06-21 2013-09-25 南开大学 Cheap transparent dye-sensitized solar cell counter electrode and preparation method thereof
CN103668089A (en) * 2013-12-04 2014-03-26 上海纳米技术及应用国家工程研究中心有限公司 Preparation method for sputtering titanium dioxide nanorod arrays on flexible substrate
CN105624626A (en) * 2016-03-14 2016-06-01 合肥工业大学 Preparation method of three-dimensional photonic crystal based on biological template

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103325577A (en) * 2013-06-21 2013-09-25 南开大学 Cheap transparent dye-sensitized solar cell counter electrode and preparation method thereof
CN103325577B (en) * 2013-06-21 2016-03-02 南开大学 Cheap transparency dye sensitization solar battery is to electrode and preparation method thereof
CN103668089A (en) * 2013-12-04 2014-03-26 上海纳米技术及应用国家工程研究中心有限公司 Preparation method for sputtering titanium dioxide nanorod arrays on flexible substrate
CN103668089B (en) * 2013-12-04 2016-08-17 上海纳米技术及应用国家工程研究中心有限公司 The preparation method of titanic oxide nanorod array is sputtered in flexible substrates
CN105624626A (en) * 2016-03-14 2016-06-01 合肥工业大学 Preparation method of three-dimensional photonic crystal based on biological template
CN105624626B (en) * 2016-03-14 2018-03-09 合肥工业大学 A kind of preparation method of the three-D photon crystal based on biological template

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Application publication date: 20110112