CN101916670B - Titanium dioxide nanoflower film photoanode and preparation method thereof - Google Patents

Titanium dioxide nanoflower film photoanode and preparation method thereof Download PDF

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CN101916670B
CN101916670B CN 201010263908 CN201010263908A CN101916670B CN 101916670 B CN101916670 B CN 101916670B CN 201010263908 CN201010263908 CN 201010263908 CN 201010263908 A CN201010263908 A CN 201010263908A CN 101916670 B CN101916670 B CN 101916670B
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tio
deionized water
toluene
hydrochloric acid
nanometer flower
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CN101916670A (en
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魏爱香
葛增娴
赵旺
刘俊
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Guangdong University of Technology
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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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    • 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
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E10/549—Organic PV cells

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Abstract

The invention discloses a titanium dioxide (TiO2) nanoflower film photoanode and a preparation method thereof. The photoandoe consists of common glass, a fluorine (F) doped tin dioxide (SnO2) transparent conductive film and a TiO2 nanoflower film. The preparation method comprises the following step of: directly synthesizing the TiO2 nanoflower film serving as the photoanode of a dye-sensitized solar cell on a FTO glass substrate by taking a mixture of concentrated hydrochloric acid, deionized water, toluene and butyl titanate as a reaction precursor and by hydro-thermal synthesis technology, wherein the shape of nanoflowers and the diameter and the length of nanorods consisting of the nanoflowers can be controlled by changing the ratio of the concentrated hydrochloric acid to the deionized water to the toluene and the concentration of the butyl titanate in the reaction precursor. By using higher light utilization efficiency and excellent electron transfer characteristic of TiO2 nanowires, the photoanode has the advantages of ensuring higher light trapping efficiency of electrodes, improving the transportation capacity of photon-generated carriers, reducing the recombination process of the photon-generated carriers, and consequently improving the photoelectric conversion efficiency of the dye-sensitized solar cells.

Description

A kind of TiO 2Nanometer flower film light anode and preparation method thereof
Technical field
The present invention is specifically related to a kind of TiO 2Nanometer flower film light anode and preparation method thereof.
Background technology
TiO 2Nano structural material has a wide range of applications at aspects such as DSSC, opto-electronic device, photochemical catalyst, transducers; Be that social development has the research object of material impact to the future economy in the current nano materials research field, it carried out controlledly synthesis have profound significance.Along with going deep into of research work; People more and more stress controllability to the research of nano material, and this not only requires to prepare has desirable crystal structure, chemical composition, pattern and size, and can various nanostructures organically be assembled; The controlled construction package that is built into various complicacies; Make it have nano material unique machinery, electricity, optics and chemical property, have only and to realize better controlled, could be nano-TiO some particular configuration or character 2Some peculiar performance finally reach industrialization and provide safeguard.
Dye-sensitized solar cells (Dye-Sensitized Solar Cell, be called for short DSSC) is a kind of photoelectrochemical solar cell, and it mainly constitutes by nano crystal semiconductor optical anode, dye sensitizing agent, electrolyte with to electrode four parts.Wherein the light anode is the core component of DSSC battery, and its structure and composition affect the photovoltaic performance, particularly conversion efficiency of battery strongly.The light anode of traditional DSSC generally adopts nano-TiO 2Porous membrane, TiO 2Though porous membrane is absorbing dye fully; But there are a large amount of crystal boundaries; Cause light induced electron in transmission course, to receive the influence that discharges with heat of capturing of particle surface defect state energy level; Make electron diffusion coefficient little, recombination rate increases, and has restricted the raising of DSSC photoelectric conversion efficiency.And one-dimensional nano structure such as nano wire, nanotube, nanometerization etc. can provide the path of direct light induced electron, improve electron diffusion length, reduce the compound of electronics, increase electron lifetime, and then improve the efficient of the opto-electronic conversion of battery.Therefore, the direct (SnO that mixes F that is coated with on glass on the transparent conducting glass substrate 2Conductive film is called for short FTO) synthetic TiO 2Nanometer flower film is to realize that it is applied to the key technology of DSSC.
Summary of the invention
The invention provides a kind of TiO 2Nanometer flower film light anode and preparation method thereof.
A kind of TiO provided by the invention 2Nanometer flower film light anode, its structure by simple glass, mix the SnO of F 2Nesa coating (FTO), TiO 2Nanometer flower film is formed; The 1st layer is simple glass, and the 2nd layer for mixing the SnO of F 2Nesa coating (being called for short FTO), the 3rd layer of TiO with rutile structure on the FTO glass substrate, growing 2Nanometer flower film.
TiO provided by the invention 2The preparation method of nanometer flower film light anode, its preparation method mainly may further comprise the steps:
1) hydro-thermal synthetic technology directly synthetic TiO on the FTO glass substrate 2Nanometer flower film;
2) the TiO for preparing 2Nanometer flower film is put into the Muffle furnace sintering, is (n-2Bu at its structural formula of ruthenium complex N719 dyestuff then 4N) 2-cis-Ru (L 1) 2(NCS) 2Ethanol solution in soak 24h, take out the dyestuff of back flush away remained on surface, dry, just obtain TiO 2Nanometer flower film light anode.
Above-mentioned steps 1) on the FTO glass substrate, prepares TiO in 2The method of nanometer flower film is: concentrated hydrochloric acid, deionized water, toluene are mixed according to the volume ratio of concentrated hydrochloric acid 20mL, deionized water 20mL, toluene 0mL or concentrated hydrochloric acid 5mL, deionized water 5mL, toluene 15mL or concentrated hydrochloric acid 10mL, deionized water 5mL, toluene 15mL or concentrated hydrochloric acid 15mL, deionized water 25mL, toluene 0mL; Magnetic stirrer 5 minutes; Splash into the butyl titanate of 0.3～0.8mL again, stirred 7 minutes; It is the autoclave of 100mL that the solution for preparing is put into band teflon-lined volume, keeps the FTO glass substrate that cleans up conducting film to lie in a horizontal plane in the agitated reactor up, the envelope still; Put into drying box to agitated reactor then and be heated to 120～180 ℃ and react, the reaction time is 4～20 hours; After reaction finishes, naturally cool to room temperature, take out FTO glass, with deionized water rinsing repeatedly, natural airing in air then.
Above-mentioned steps 2) in the TiO for preparing 2Nanometer flower film is put into 450 ℃ of sintering 30min of Muffle furnace, cools to then about 80 ℃ and takes out, and putting into concentration immediately is 5.0 * 10 -4Soak 24h in the ruthenium complex N719 dyestuff ethanol solution of mol/L; Take out the dyestuff of back, dry, obtain TiO with ethanol flush away remained on surface 2Nanometer flower film light anode.
The invention has the beneficial effects as follows:
The TiO that on the FTO glass substrate, synthesizes 2Nanometer flower film can be directly as dye-sensitized solar cell anode, and this nanometer flower is that the nanometer rods by the square column structure constitutes these TiO 2Nanometer rods has ensured that electrode has higher light capture rate, has improved the transport capability of photo-generated carrier, has reduced the recombination process of photo-generated carrier, thereby improves the electricity conversion of DSSC.
Through changing hydrochloric acid, water and the ratio of toluene, concentration, reaction time and the reaction temperature of butyl titanate in the pre-reaction material, may command is formed the diameter and the length of the nanometer rods of nanometer flower, realizes TiO 2The controllable growth of nanometer flower.
Description of drawings
Fig. 1 is TiO 2The structural representation of nanometer flower film light anode.The 1st layer is simple glass, and the 2nd layer for mixing the SnO of F 2Nesa coating (FTO), the 3rd layer is TiO 2Nanometer flower film.
Fig. 2, Fig. 3, Fig. 4 and Fig. 6 are the TiO that on the FTO glass substrate, grows under the different technology conditions 2Nanometer flower film amplifies 10,000 times SEM figure, and Fig. 7 is the local SEM figure that amplifies 30,000 times among Fig. 6.5,000 times of the multiplication factors of Fig. 5.
The TiO of Fig. 2 2The synthesis condition of nanometer flower film is toluene 0mL, water 20mL, hydrochloric acid 20mL, butyl titanate 0.3mL, 150 ℃ of synthesis temperatures, generated time 20h.
The TiO of Fig. 3 2The synthesis condition of nanometer flower film is toluene 0mL, water 20mL, hydrochloric acid 20mL, butyl titanate 0.6mL, 150 ℃ of synthesis temperatures, generated time 20h.
The TiO of Fig. 4 2The synthesis condition of nanometer flower film is toluene 15mL, water 5mL, hydrochloric acid 5mL, butyl titanate 0.5mL, 150 ℃ of synthesis temperatures, generated time 16h.
The TiO of Fig. 5 2The synthesis condition of nanometer flower film is toluene 15mL, water 5mL, hydrochloric acid 10mL, butyl titanate 0.5mL, 150 ℃ of synthesis temperatures, generated time 20h.
The synthesis condition of Fig. 6 and Fig. 7 is at growth TiO 2Before the nanometer flower film, in concentration the TiCl of 0.1mol/L FTO glass 4After soaking 30min under 80 ℃ in the aqueous solution, the fine and close TiO of the one deck of can on FTO, growing 2Film, and then carry out hydro-thermal reaction and prepare TiO 2The nanometer flower, its synthesis condition is: toluene 0mL, water 25mL, hydrochloric acid 15mL, butyl titanate 0.5mL, 150 ℃ of synthesis temperatures, generated time 20h.
Embodiment
1. on the FTO glass substrate, prepare TiO 2Nanometer flower film.
Adopt the hydro-thermal synthetic technology of low temperature low energy consumption on the FTO glass substrate, to prepare TiO 2Nanometer flower film.Concentrated hydrochloric acid, deionized water, toluene are mixed according to concentrated hydrochloric acid 20mL, deionized water 20mL, toluene 0mL or concentrated hydrochloric acid 5mL, deionized water 5mL, toluene 15mL or concentrated hydrochloric acid 10mL, deionized water 5mL, toluene 15mL or concentrated hydrochloric acid 15mL, deionized water 25mL, toluene 0mL volume ratio; Magnetic stirrer 5 minutes; Splash into the butyl titanate of 0.3～0.8mL again, stirred 7 minutes.It is the autoclave of 100mL that the solution for preparing is put into band teflon-lined volume, keeps the FTO glass substrate that cleans up conducting film to lie in a horizontal plane in the agitated reactor up, the envelope still.Put into drying box to agitated reactor then and be heated to 120～180 ℃ and react, the reaction time is 4～20 hours.After reaction finishes, naturally cool to room temperature, take out FTO glass, with deionized water rinsing repeatedly, natural airing in air then.
2.TiO 2The controllable growth of nanometer flower film.
Through changing concentrated hydrochloric acid, deionized water, the ratio of toluene and the concentration of butyl titanate in the reaction precursor body, can control the pattern of nanometer flower and the diameter and the length of the nanometer rods of forming the nanometer flower, thereby realize TiO 2The controlledly synthesis of nanometer flower.
When (1) ratio of concentrated hydrochloric acid, deionized water, toluene and cumulative volume remained unchanged in the reaction precursor body, the amount of butyl titanate was increased to 0.8mL gradually from 0.3mL, all can on the FTO substrate, grow TiO 2Nanometer flower film, nanometer flower are that the nanometer rods by the square column structure constitutes, and the diameter of nanometer rods increases and chap with the amount of butyl titanate.
(2) pattern of TiO2 nanometer flower is relevant with the concentration of butyl titanate in the pre-reaction material; When the concentration of butyl titanate was hanged down, the nanometer flower was comparatively loose, when butyl titanate concentration is higher; The nanometer rods that constitutes the nanometer flower flocks together very closely, and the shape of nanometer flower is similar to " cauliflower ".
When (3) amount of butyl titanate immobilized in the pre-reaction material, the ratio of hydrochloric acid was big more, and the diameter of the nanometer rods of composition nanometer flower is thin more.
(4) before the hydro-thermal reaction, in concentration the TiCl of 0.1mol/L FTO glass 4After soaking 30min under 80 ℃ in the aqueous solution, the fine and close TiO of the one deck of can on FTO, growing 2Film, and then carry out hydro-thermal reaction and prepare TiO 2The nanometer flower, under the same conditions, TiO 2Nanometer is spent can grow thinner.TiCl 4The compound method of the aqueous solution is to put 100ml water earlier to be put into and to form ice cube in the refrigerator, and then splashes into an amount of TiCl 4Making its concentration is 0.1mol/L, then ice-out, puts into FTO solution and under 80 ℃ of constant temperature, soaks 30min.
3.TiO 2The assembling of nanometer flower film light anode and DSSC.
The TiO for preparing 2Nanometer flower film is put into 450 ℃ of sintering 30min of Muffle furnace, cools to then about 80 ℃ and takes out, and putting into concentration immediately is 5.0 * 10 -4(structural formula is (n-2Bu to the ruthenium complex N719 dyestuff of mol/L 4N) 2-cis-Ru (L 1) 2(NCS) 2] ethanol solution in soak 24h, take out the dyestuff of back with ethanol flush away remained on surface, dry, be exactly prepared light anode.Then with the FTO glass that is coated with the Pt film to electrode, KI/I 2Solution be electrolyte [0.5mol/L KI+0.05mol/L I 2Solvent: acetonitrile (volume integral 80)+isopropyl alcohol (volume fraction 20)], be assembled into battery.

Claims (2)

1. TiO 2The preparation method of nanometer flower film light anode is characterized in that may further comprise the steps:
1) concentrated hydrochloric acid, deionized water, toluene are mixed according to the volume ratio of concentrated hydrochloric acid 20mL, deionized water 20mL, toluene 0mL or concentrated hydrochloric acid 5mL, deionized water 5mL, toluene 15mL or concentrated hydrochloric acid 10mL, deionized water 5mL, toluene 15mL or concentrated hydrochloric acid 15mL, deionized water 25mL, toluene 0mL; Magnetic stirrer 5 minutes; Splash into the butyl titanate of 0.3～0.8mL again, stirred 7 minutes; It is the autoclave of 100mL that the solution for preparing is put into band teflon-lined volume, keeps the FTO glass substrate that cleans up conducting film to lie in a horizontal plane in the agitated reactor up, the envelope still; Put into drying box to agitated reactor then and be heated to 120～180 ℃ and react, the reaction time is 4～20 hours; Reaction naturally cools to room temperature after finishing, and takes out FTO glass, and with deionized water rinsing repeatedly, natural airing in air is accomplished directly synthetic TiO on the FTO glass substrate then 2Nanometer flower film;
2) the TiO for preparing 2Nanometer flower film is put into the Muffle furnace sintering, is (n-2Bu at its structural formula of ruthenium complex N719 dyestuff then 4N) 2-cis-Ru (L 1) 2(NCS) 2Ethanol solution in soak 24h, take out the dyestuff of back flush away remained on surface, dry, just obtain TiO 2Nanometer flower film light anode.
2. preparation method according to claim 1 is characterized in that: above-mentioned steps 2) with the TiO for preparing 2Nanometer flower film is put into 450 ℃ of sintering 30min of Muffle furnace, cools to then about 80 ℃ and takes out, and putting into concentration immediately is 5.0 * 10 -4Soak 24h in the ruthenium complex N719 dyestuff ethanol solution of mol/L; Take out the dyestuff of back, dry, obtain TiO with ethanol flush away remained on surface 2Nanometer flower film light anode.
CN 201010263908 2010-08-25 2010-08-25 Titanium dioxide nanoflower film photoanode and preparation method thereof Expired - Fee Related CN101916670B (en)

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CN102701275B (en) * 2012-06-01 2014-01-15 华北电力大学 Method for preparing TiO2 nano laces
CN103936066A (en) * 2014-05-05 2014-07-23 浙江大学 Method for preparing rutile titanium dioxide nanometer flower array thin film
CN104310794A (en) * 2014-09-28 2015-01-28 吉林大学 Porous TiO2 nanocrystalline thin film having three-dimensional nanorod floral structure as well as preparation method and application of porous TiO2 nanocrystalline thin film
CN105819501A (en) * 2015-01-05 2016-08-03 广东工业大学 Double-layer rutile titanium dioxide nano-structure and preparation method thereof
CN105428070B (en) * 2015-12-18 2017-11-14 哈尔滨工业大学 Based on flower-shaped TiO2The preparation method of the dye-sensitized solar cell anode of powder and blue-green fluorescent C quantum dots
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CN106006825A (en) * 2016-05-23 2016-10-12 无锡市嘉邦电力管道厂 TiO2 film electrode and manufacturing method thereof
CN107254690B (en) * 2017-06-20 2019-01-11 中国科学院新疆理化技术研究所 TiO with three-dimensional hierarchical structure2Nano wire/micro-flowers light anode preparation method
CN107680815B (en) * 2017-09-18 2019-02-01 哈尔滨工业大学 A kind of preparation method and applications of homogeneity barrier layer/skeleton titania structure
CN112505115A (en) * 2020-12-17 2021-03-16 东北农业大学 Preparation and detection method of three-dimensional photosensitive electrode for detecting phospholipids in crude oil

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