CN102290248B - Method for preparing efficient compound light anode of dye sensitized solar cell - Google Patents

Method for preparing efficient compound light anode of dye sensitized solar cell Download PDF

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CN102290248B
CN102290248B CN 201110154688 CN201110154688A CN102290248B CN 102290248 B CN102290248 B CN 102290248B CN 201110154688 CN201110154688 CN 201110154688 CN 201110154688 A CN201110154688 A CN 201110154688A CN 102290248 B CN102290248 B CN 102290248B
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zno
light anode
nano
tio
film
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CN102290248A (en
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李京波
李庆跃
李凯
王美丽
池旭明
夏建白
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East crystal electronic Jinhua Co., Ltd.
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DONGJING ELECTRONIC Co Ltd ZHEJIANG
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/20—Light-sensitive devices
    • H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
    • H01G9/2036—Light-sensitive devices comprising an oxide semiconductor electrode comprising mixed oxides, e.g. ZnO covered TiO2 particles
    • 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

Abstract

The invention relates to the field of development and utilization research of new energy resources, and in particular relates to a method for preparing an efficient compound light anode of a dye sensitized solar cell. The method comprises the following steps: firstly depositing a ZnO thin film doped with In on a transparent substrate by utilizing a magnetic control sputtering technology; then growing a ZnO nanowire array on the ZnO thin film doped with In by adopting a hydrothermal chemistry reaction method; and finally coating a layer of TiO2 nano particle dispersion solution on the surface of the ZnO nanowire array through a silk screen printing technology, and heating the dispersion solution to enable an organic solvent in the dispersion solution to volatilize, thus obtaining a hole-shaped TiO2 nano crystalline porous membrane/ZnO nanowire array compound light anode structure. Each TiO2 nano particle mainly comprises small particles with the diameter about 10 nanometers, and simultaneously a small quantity of large particles with the diameter about 200 nanometers are dispersed; and the compound light anode can be used for not only improving the photosensitive dye absorption capacity and the light capture efficiency, but also improving the transport capability of photoproduction electrons, and improving the photoelectric conversion efficiency of the dye sensitized solar cell.

Description

The preparation method of the efficient complex light anode of a kind of DSSC
Technical field
The present invention relates to the development and utilization research field of new forms of energy, be specifically related to the preparation method of the efficient complex light anode of a kind of DSSC.
Background technology
The light anode is as the DSSC core component of (Dye-sensitized solar cell is called for short DSSC), to the raising decisive role of battery performance.If improve the photoelectric conversion efficiency of DSSC, the light anode must satisfy two conditions: one, produce a large amount of light induced electrons; Two, light induced electron is by exciting dyestuff to be transferred to external circuit fast through the light anode.TiO 2Nanocrystalline porous film and One-Dimensional ZnO nano-wire array are the two kinds of positive electrode structures the most widely of research at present.TiO 2Nanocrystalline porous film helps the more absorption of polychromatophilia material for the light anode provides big specific area, but wherein has a large amount of crystal boundaries, makes electron diffusion coefficient little, and recombination rate is high, has restricted the further raising of DSSC photoelectric conversion efficiency; Though and the One-Dimensional ZnO nano-wire array can provide the path of straight line transmission, improve electron diffusion length, reduce electron recombination, increase electron lifetime, its adsorbance to dyestuff is limited, makes that the photoelectric conversion efficiency of this type of battery is also undesirable.
Summary of the invention
The objective of the invention is deficiency to prior art; The preparation method of the efficient complex light anode of a kind of DSSC is provided; This complex light anode has not only improved light-sensitive coloring agent adsorbance and light capture rate, has ensured the generation rate of light induced electron, and has improved the transport capability of light induced electron; Reduce the recombination process of electronics, thereby improve the electricity conversion of DSSC.
The preparation method of the efficient complex light anode of DSSC provided by the invention is characterized in that: utilize magnetron sputtering technique at first on transparent substrate, to deposit the ZnO film of mixing In; Adopt the hydrothermal chemical reaction method mixing growing ZnO nano-wire array on the ZnO film of In then; At last through the surface coated one deck TiO of screen printing technique at the ZnO nano-wire array 2The dispersion soln of nano particle, heating make the organic solvent volatilization in the dispersion soln, obtain poroid TiO 2Nanocrystalline porous film/ZnO nano-wire array laminated film is with TiO 2Nanocrystalline porous film/ZnO nano-wire array laminated film soaks in dye solution, takes out the dye solution of back flush away remained on surface, dries, and obtains dye sensitization TiO 2Nanocrystalline porous film/ZnO nano-wire array laminated film light anode.
The present invention deposits the ZnO film of mixing In on transparent substrate be the method that adopts magnetron sputtering, and the thickness of mixing the ZnO film of In is 100-300nm.
ZnO nano-wire array of the present invention is directly being mixed epitaxial growth on the ZnO film of In, need not mix deposit seed on the ZnO film of In.
TiO of the present invention 2Nanocrystalline porous film is made up of about 10 nanometers of diameter and two kinds of particles of about 200 nanometers of diameter, and diameter is that 10 nano particles and diameter are that the volume ratio of 200 nano particles is 90:10-95:5; Surface printing TiO at the ZnO nano-wire array 2Behind the slurry, it 500 ℃ of sintering 30 minutes, is taken out when temperature is reduced to 80 ℃, the ruthenium complex N719 dyestuff absolute ethyl alcohol of putting into 0.3mM/L immediately soaked 24 hours; Take out the dyestuff of back, dry up, obtain the dye sensitization complex light anode with absolute ethyl alcohol flush away remained on surface.
The present invention has optimized the growth conditions and the TiO of ZnO nano-wire array 2The micro-structural of nanocrystalline porous film, promptly on transparent substrate directly deposition mix the ZnO film of In, need be on conductive film deposit seed again, directly mix epitaxial growth of ZnO nano-wire array on the ZnO film of In at this, accelerate the transmission and the collection of electronics; At TiO 2In the slurry, except the particle of 10 traditional nanometers, also introduced the particle of about 200 nanometers of diameter, large-sized nano particle can play scattering and irreflexive effect to the sunlight of incident, improves the utilance of sunlight and increases the chance that dyestuff is excited.In addition, the present invention is with ZnO nano-wire array and TiO 2The advantages of nanocrystalline porous film gets up to form complex light anode, can significantly improve the photoelectric conversion efficiency of battery.
Beneficial effect of the present invention is:
The present invention has optimized the growth conditions of ZnO nano-wire array, is substituted in the SnO that F mixes 2Deposition ZnO crystal seed layer regrowth ZnO nano-wire array directly deposits the ZnO film of mixing In on the conductive substrate on transparent substrate, and this film both can be used as conductive layer, also can be used as crystal seed layer simultaneously, had reduced the obstruction of electric transmission and had simplified processing step.
The present invention has optimized TiO 2The micro-structural of nanocrystalline porous film changes traditional perforated membrane of being made up of single nano particle, in perforated membrane, introduces large-sized TiO 2Nano particle improves the light capture rate of battery as scattering center.
The present invention is with TiO 2Nanocrystalline porous film and ZnO nano-wire array combined electrode structure are as the light anode of DSSC; Guarantee electrode fully absorbing dye, improved the transport capability of light induced electron when having higher light capture rate; Reduce the recombination rate of light induced electron, thereby improved the electricity conversion of DSSC.
Description of drawings
Fig. 1 is TiO of the present invention 2The structural representation of nanocrystalline porous film/ZnO nano-wire array complex light anode.
Fig. 2 is ZnO nano-wire array DSSC of the present invention (a) and TiO 2Current density-voltage curve figure of nanocrystalline porous film/ZnO nano-wire array DSSC (b).
Among Fig. 1,1---transparent substrate; 2---mix the ZnO film of In; 3---the ZnO nano-wire array; 4---TiO 2Nanocrystalline porous film.
Embodiment
As shown in Figure 1, the present invention provides the preparation method of the efficient complex light anode of a kind of DSSC, comprises following step:
Step 1: get a transparent substrate 1, transparent substrate 1 is substrate of glass or flexible plastic substrates, at first transparent substrate 1 is cleaned fully, and it respectively acetone, ethanol and deionized water for ultrasonic 20 minutes, and is dried up with nitrogen, and is for use;
Step 2: deposition is mixed the ZnO film 2 of In on transparent substrate 1, and the described ZnO film 2 that deposition is mixed In on transparent substrate 1 is the methods that adopt magnetron sputtering, and sputtering condition is: mix the ZnO target of In, back of the body end vacuum 4 * 10 -4Pa, sputtering pressure 0.6Pa, Ar gas flow 20SCCM, sputtering power 100W, 300 ℃ of underlayer temperatures, sputtering time 10-30 minute, the thickness of mixing the ZnO film 2 of In was the 100-300 nanometer; This ZnO film 2 of mixing In both can be used as transparency conducting layer, also can be used as the crystal seed layer of growing ZnO nano-wire array 3 simultaneously, had replaced and had mixed the SnO of F 2Deposition ZnO crystal seed layer has reduced the obstruction of electric transmission and has simplified processing step on the conductive substrate;
Step 3: adopt the hydrothermal chemical reaction method, epitaxial growth of ZnO nano-wire array 3 on the ZnO film of mixing In 2 is wherein during epitaxial growth of ZnO nano-wire array 3; The zinc source of adopting is zinc nitrate or zinc acetate solution, and the concentration of this zinc nitrate or zinc acetate solution is 10mM-100mM, through in this zinc nitrate or zinc acetate solution, adding alkaline matters such as ammoniacal liquor, carbonic hydroammonium, NaOH or hexa; Make the pH value of hydro-thermal reaction solution be 9.6-10.6, the solution for preparing is put into band teflon-lined autoclave, envelope still; The hydrothermal temperature that adopts is 90-120 ℃; Reaction time is 3-12 hour, and reaction naturally cools to room temperature with autoclave after finishing; Take out the transparent substrate 1 that deposition is mixed the ZnO film 2 of In; Wash earlier the surface of the ZnO film 2 of mixing In repeatedly, with the ZnO film of mixing In 2 after this hydro-thermal reaction in 80 ℃ of thermostatic drying chambers dry 12 hours, obtain ZnO nano-wire array 3 then with deionized water.This ZnO nano-wire array 3 has reduced the transmission time and the path of light induced electron for the approach that light induced electron provides straight line to transmit, and has reduced the reverse compound probability of light induced electron;
Step 4: adopt the surface printing TiO of screen printing technique at ZnO nano-wire array 3 2Slurry; Heating makes TiO 2Organic solvent volatilization in the slurry obtains TiO 2Nanocrystalline porous film 4 forms TiO 2Nanocrystalline porous film 4/ZnO nano-wire array 3 laminated films, wherein TiO 2Nanocrystalline porous film 4 is made up of about 10 nanometers of diameter and two kinds of particles of about 200 nanometers of diameter; The volume ratio of 10 nano particles and 200 nano particles is 90:10-95:5; Undersized nano particle can provide big specific area for electrode; Increase the dyestuff adsorbance of electrode, large-sized nano particle carries out scattering and diffuse scattering as scattering center to the sunlight of incident, improves the light capture rate of battery.Surface printing TiO at ZnO nano-wire array 3 2Behind the slurry, it 500 ℃ of sintering 30 minutes, is fully vapored away TiO 2Organic substance in the slurry makes TiO 2Space between the nano particle becomes mesoporous, obtains TiO 2Nanocrystalline porous film 4.When sintering temperature is reduced to 80 ℃, take out, the ruthenium complex N719 dyestuff absolute ethyl alcohol of putting into 0.3mM/L immediately soaked 24 hours, and temperature is reduced to TiO after the room temperature 2Have a large amount of gases in nanocrystalline porous film 4 mesoporous and get into, hinder the infiltration and the absorption of dyestuff; Take out the dyestuff of back, dry up, obtain the dye sensitization complex light anode with absolute ethyl alcohol flush away remained on surface;
Step 5: the assembling of DSSC and photoelectric properties test; [(proportioning is: 1.0M 1,3-dimethylimidazolium iodide, 0.05M LiI on the light anode after the sensitization, to drip redox electrolytes matter; 0.1M guanidinium thiocyanate, 0.03M I 2, and 0.5Mtert-butylpyridine) and solvent is the mixed solution (volume ratio is 85:15) of acetonitrile and valeronitrile], add a cover Pt electrode is assembled into DSSC.Under the irradiation of 500W simulated solar radiant xenon lamp, radiation intensity is 100W/cm 2, battery receives illuminating area 0.25cm 2As shown in Figure 2, the battery performance parameter of ZnO nano-wire array DSSC is: open circuit voltage V OcBe 588mV, short-circuit current density J ScBe 2.70mA/cm 2, fill factor, curve factor FF is 0.57, photoelectric conversion efficiency is 0.90%; TiO 2The photoelectric properties parameter of nanocrystalline porous film/ZnO nano-wire array DSSC is: open circuit voltage V OcBe 711mV, short-circuit current density J ScBe 10.69mA/cm 2, fill factor, curve factor FF is 0.62, photoelectric conversion efficiency is 4.68%.Compare TiO with ZnO nano-wire array battery 2Open circuit voltage and the short-circuit current density of nanocrystalline porous film/ZnO nano-wire array DSSC all are greatly enhanced, and photoelectric conversion efficiency obtains the lifting greater than 5 times.

Claims (6)

1. the preparation method of the efficient complex light anode of DSSC is characterized in that: on transparent substrate, deposit the ZnO film of mixing In; Adopt the hydrothermal chemical reaction method mixing growing ZnO nano-wire array on the ZnO film of In then; At last through the surface coated one deck TiO of screen printing technique at the ZnO nano-wire array 2The dispersion soln of nano particle, heating make the organic solvent volatilization in the dispersion soln, obtain poroid TiO 2Nanocrystalline porous film/ZnO nano-wire array laminated film is with TiO 2Nanocrystalline porous film/ZnO nano-wire array laminated film soaks in dye solution, takes out the dye solution of back flush away remained on surface, dries, and obtains dye sensitization TiO 2Nanocrystalline porous film/ZnO nano-wire array laminated film light anode.
2. the preparation method of the efficient complex light anode of DSSC according to claim 1; It is characterized in that: the said ZnO film that deposition is mixed In on transparent substrate is the method that adopts magnetron sputtering, and the thickness of mixing the ZnO film of In is 100-300nm.
3. the preparation method of the efficient complex light anode of DSSC according to claim 1 and 2; It is characterized in that: during said growing ZnO nano-wire array; The ZnO nano-wire array is directly being mixed epitaxial growth on the ZnO film of In, need not mix deposit seed on the ZnO film of In.
4. the preparation method of the efficient complex light anode of DSSC according to claim 1 is characterized in that: at TiO 2In the nanocrystalline porous film, TiO 2Nano particle is that 10 nanometers and diameter are that two kinds of particles of 200 nanometers are formed by diameter, and diameter is that 10 nano particles and diameter are that the volume ratio of 200 nano particles is 90:10-95:5.
5. according to the preparation method of claim 1 or the efficient complex light anode of 4 described DSSCs, it is characterized in that: said surface coated one deck TiO at the ZnO nano-wire array 2Behind the dispersion soln of nano particle, it 500 ℃ of sintering 30 minutes, is taken out when temperature is reduced to 80 ℃, the ruthenium complex N719 dyestuff absolute ethyl alcohol of putting into 0.3mM/L immediately soaked 24 hours; Take out the dyestuff of back, dry up, obtain the dye sensitization complex light anode with absolute ethyl alcohol flush away remained on surface.
6. the preparation method of the efficient complex light anode of DSSC according to claim 1 is characterized in that: said transparent substrate is substrate of glass or flexible plastic substrates.
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CN102637532B (en) * 2012-04-19 2014-07-09 陕西师范大学 Nanocable-containing DSC (dye-sensitized solar cell) photo-anode and preparation method thereof
CN103268825B (en) * 2013-05-08 2016-05-25 上海纳米技术及应用国家工程研究中心有限公司 A kind of compound structured light anode material of solar cell and preparation method
CN103346017B (en) * 2013-07-17 2016-11-16 重庆大学 A kind of dye-sensitized solar cell anode and preparation method thereof
CN103578775B (en) * 2013-11-22 2016-04-27 长沙理工大学 Based on the dye-sensitized solar cells and preparation method thereof of ZnO transparent conductive nanowire array electrode
CN106328721B (en) * 2015-07-06 2018-10-02 南京理工大学 A kind of mesoporous titanium dioxide layer and preparation method thereof of double sized nanostructures networks
CN104966617B (en) * 2015-07-22 2017-06-27 陕西理工学院 For the complex light anode and preparation method of quantum dot sensitized solar cell
CN106847648B (en) * 2017-03-01 2019-01-08 杭州电子科技大学 A kind of preparation method of use for field emission graphene/zinc oxide/graphene sandwich structure composite cathode material
CN109935733B (en) * 2017-12-15 2021-11-23 深圳Tcl工业研究院有限公司 N-type ZnO film, preparation method thereof and QLED device
CN111116232A (en) * 2019-12-13 2020-05-08 苏州麦茂思传感技术有限公司 Synthesis method of formaldehyde gas sensor sensitive material
CN114807882B (en) * 2022-05-06 2023-07-14 广东省科学院半导体研究所 Magnetron sputtering target material, preparation method and application thereof

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CN101814376A (en) * 2010-03-17 2010-08-25 武汉大学 ZnO composite electrode of dye-sensitized solar battery and preparation method thereof

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