CN102768904B - Method for preparing working electrode of TiO2 nanotube array - Google Patents

Method for preparing working electrode of TiO2 nanotube array Download PDF

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Publication number
CN102768904B
CN102768904B CN201110115960.9A CN201110115960A CN102768904B CN 102768904 B CN102768904 B CN 102768904B CN 201110115960 A CN201110115960 A CN 201110115960A CN 102768904 B CN102768904 B CN 102768904B
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tio
nano
tube array
etching
electrode
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CN102768904A (en
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王尚华
林原
周晓文
张敬波
肖绪瑞
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Institute of Chemistry of CAS
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/542Dye sensitized solar cells
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/549Organic PV cells

Abstract

The invention belongs to the field of preparation of working electrodes in dye-sensitized solar cells, and particularly relates to a method for preparing a working electrode of a TiO2 nanotube array. The method for preparing the working electrode of the TiO2 nanotube array employs the TiO2 nanotube array as a starting point, and includes the steps: firstly, depositing TiO2 nanoparticles on the surface of the TiO2 nanotube array by an electrophoretic deposition method to increase the surface area of the TiO2 nanotube array providing the working electrode for a dye-sensitized solar cell; and secondly, preparing the corrugated TiO2 nanotube array by rectangular waves for voltage etching to increase the surface area of the TiO2 nanotube array providing the working electrode for the dye-sensitized solar cell. The prepared working electrode of the TiO2 nanotube array is used for the dye-sensitized solar cell, so that the photoelectric conversion efficiency of the dye-sensitized solar cell is greatly improved.

Description

TiO 2the preparation method of nano-tube array work electrode
Technical field
The invention belongs to the preparation field of the work electrode in DSSC, particularly TiO 2the preparation method of nano-tube array work electrode.
Background technology
DSSC is paid close attention to its high-performance and low-cost widely as third generation thin-film solar cells, and in development, preparation technology is simple, and with low cost, high efficiency clear energy sources aspect is significant.
Work electrode, as the important component part in DSSC, has important impact to the performance of DSSC.The nano-tube array of high-sequential has many advantages: (1) porous nanotube array has large surface area, and larger surface area can be provided for carried dye.(2) rising structure of high-sequential enables electronics along tube wall axially transmission, reduces the transmission path of electronics between interface.(3) nano-tube array structure can improve light scattering property, increases the absorption to light.(4) structure of high-sequential makes the defect on its surface less, and electron recombination center is less, can suppress electron recombination.But, use ungroomed nano-tube array as work electrode, cell photoelectric transformation efficiency lower than traditional with TiO 2the film of nano particle composition is the DSSC of work electrode.Its electricity conversion reason on the low side is caused to have two: (one) TiO 2the surface area of nano-tube array is less than TiO 2the surface area of film of nano particle composition, the dyestuff therefore adsorbed is few, and cause the photon that absorbs during illumination few, the photoelectric current of generation is little.(2) light is to electrode direction incident mode, and electrolyte can absorb a part of near ultraviolet band light, also can absorb and antireflection part light electrode simultaneously.The result finally caused is that the light intensity arriving work electrode is less than light intensity when irradiating from work electrode direction.
Summary of the invention
The object of this invention is to provide the TiO that surface area increases 2the preparation method of nano-tube array work electrode, by gained TiO 2during the work electrode of nano-tube array work electrode as DSSC, electricity conversion can be improved.
The present invention is with TiO 2nano-tube array is starting point, and its method comprises: (one) utilizes electrophoretic deposition at TiO 2the surface deposition TiO of nano-tube array 2nano particle, to increase the TiO as dye-sensitized solar cell working electrode 2the surface area of nano-tube array; (2) square-wave voltage etching preparation corrugated TiO is used 2nano-tube array, to increase the TiO as dye-sensitized solar cell working electrode 2the surface area of nano-tube array 2these two kinds of methods can both increase TiO significantly 2the surface area of nano-tube array.
TiO of the present invention 2the preparation method of nano-tube array work electrode: TiO is contained on surface 2the titanium sheet of nano-tube array is dipped in TiO 2electrophoretic deposition TiO is carried out in suspension-turbid liquid 2nano particle, electrophoretic deposition TiO 2during nano particle with platinized platinum as anode, described titanium sheet is as negative electrode; During electrophoretic deposition, direct voltage used is 5V ~ 30V, at TiO 2tiO on the surface deposition of nano-tube array 2nano particle, obtains the TiO that surface area increases 2nano-tube array work electrode; Or
Titanium sheet is dipped in electrolyte and carries out anode polarization etching TiO 2nano-tube array; The NH consisting of 0.5wt% of electrolyte used during etching 4the H of F, 1wt% 2the ethylene glycol of O and 98.5wt%; Adopt two electrode systems when carrying out anode polarization etching, work electrode is described titanium sheet, is platinized platinum to electrode, and the etching voltage of use etches voltage for square wave, obtains corrugated TiO 2nano-tube array, this corrugated TiO 2nano-tube array increases TiO 2the surface area of nano-tube array work electrode.
TiO is contained on surface used in the present invention 2the titanium sheet of nano-tube array take titanium sheet as substrate, prepared in containing the electrolyte of fluorine ion by anode polarization etching method; The NH consisting of 0.5wt% of electrolyte used during etching 4the H of F, 1wt% 2the ethylene glycol of O and 98.5wt%; Adopt two electrode systems when carrying out anode polarization etching, work electrode is described titanium sheet, is platinized platinum to electrode.
Described TiO 2suspension-turbid liquid is prepared by following methods: under the condition stirred, by TiO 2colloid drops is added in absolute ethyl alcohol, makes in absolute ethyl alcohol containing TiO 2the mass fraction of nano particle is 2% ~ 10%, stirs and obtains TiO 2suspension-turbid liquid; TiO 2the particle diameter of nano particle is 10 ~ 20 nanometers.
The time of described electrophoretic deposition is 10 seconds to 2 minutes.
It is first etch with high voltage, and then etch by low-voltage that described use square wave etching voltage carries out etching.
Described when etching with high voltage, the time stopped under high voltages is 100 milliseconds ~ 3000 milliseconds; Described when etching by low-voltage, the time stopped at lower voltages is 25 milliseconds ~ 1000 milliseconds.
The time that described use square wave etching voltage carries out etching is 10 hours ~ 60 hours (comprise high voltage carry out etching and low-voltage etches).
Described high voltage is 60 ~ 120V, and described low-voltage is 10 ~ 50V.
Distance between described anode and negative electrode is preferably 3 centimetres; Described work electrode and 3 centimetres are preferably to the distance between electrode.
The invention provides above-mentioned two kinds and prepare high surface area TiO 2the method of nano-tube array work electrode, by the TiO prepared 2nano-tube array work electrode can improve electricity conversion as the work electrode of DSSC, can obtain the electricity conversion up to 7.36%.And the method for this preparation work electrode is simple, easily operates, favorable reproducibility.Can be used as flexible dye-sensitized solar battery.
Accompanying drawing explanation
Fig. 1. one provided by the invention prepares TiO 2the device schematic diagram of nano-tube array.
Fig. 2. the oscillogram of the square wave etching voltage described in the present invention.
Fig. 3. the TiO during embodiment of the present invention 1 ~ 6 non-depositing colloidal 2the shape appearance figure of nano-tube array.
Fig. 4. TiO after the embodiment of the present invention 1 ~ 6 electrophoretic deposition colloid 2the shape appearance figure of nano-tube array.
Fig. 5. the embodiment of the present invention 7 ~ 10 corrugated TiO 2the shape appearance figure of nano-tube array.
Embodiment
The experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
Processing mode and the concrete preparation method of titanium sheet used in following embodiment are as follows:
(1) titanium sheet is cut into the small pieces of 1cm × 3cm, be then 400,500 by fineness successively, the sand paper of 800,1000,1500 carries out sanding and polishing, obtains a bright surface;
(2) titanium sheet that step (1) has been polished is used distilled water, acetone, isopropyl alcohol, absolute methanol, distilled water ultrasonic cleaning 5 minutes successively; Cleaned titanium sheet is dried up for subsequent use in nitrogen stream;
(3) utilize the device shown in Fig. 1, the titanium sheet that step (2) dries up is dipped in electrolyte and carries out anode polarization etching preparation TiO 2nano-tube array; The NH consisting of 0.5wt% of electrolyte used during etching 4the H of F, 1wt% 2the ethylene glycol of O and 98.5wt%; Adopt two electrode systems when carrying out anode polarization etching, work electrode is the titanium sheet that step (2) obtains, and is platinized platinum to electrode, and the distance between two electrodes is 3 centimetres; The etching voltage used is direct current 60V; Etch period is 10 ~ 60 hours;
(4) titanium sheet that step (3) etches through anode polarization is taken out from electrolyte, then clean with distilled water and absolute ethyl alcohol successively, dry;
(5) titanium sheet after step (4) being dried is dipped in TiO 2electrophoretic deposition TiO is carried out in suspension-turbid liquid 2nano particle; Electrophoretic deposition TiO 2during nano particle with platinized platinum as anode, the titanium sheet that step (4) obtains is as negative electrode; During electrophoretic deposition, applied voltage scope is 5V ~ 30V, and the time range of electrophoretic deposition is 10 seconds to 2 minutes; Described TiO 2suspension-turbid liquid is prepared by following methods: under the condition stirred, by TiO 2colloid drops is added in absolute ethyl alcohol, makes in absolute ethyl alcohol containing TiO 2the mass fraction of nano particle is 2% ~ 10%, TiO 2the particle diameter of nano particle is 10 ~ 20 nanometers; Then continue stirring 30 minutes, make TiO 2nanoparticulate dispersed is even, forms TiO 2suspension-turbid liquid;
(6) corrugated TiO 2the preparation of nano-tube array: the titanium sheet that step (2) dries up is dipped in electrolyte and carries out anode polarization etching TiO 2nano-tube array; The NH consisting of 0.5wt% of electrolyte used during etching 4the H of F, 1wt% 2the ethylene glycol of O and 98.5wt%; Adopt two electrode systems when carrying out anode polarization etching, work electrode is the titanium sheet that step (2) obtains, and is platinized platinum to electrode, and the distance between two electrodes is 3 centimetres; The etching voltage used etches voltage for square wave, and when using square wave etching voltage to etch, the time stopped under high voltages is 100 milliseconds ~ 3000 milliseconds; The time stopped at lower voltages is 25 milliseconds ~ 1000 milliseconds; Described high voltage is 60 ~ 120V, and described low-voltage is 10 ~ 50V; Etch 10 hours ~ 60 hours altogether;
(7) titanium sheet that step (6) prepares is taken out, and rinses with absolute ethyl alcohol, dries;
(8) titanium sheet after step (7) being dried is placed in Muffle furnace and sinters 2 hours at 500 DEG C, and programming rate is 5 DEG C/min, then naturally cools to room temperature.
The method of DSSC prepared by following embodiment is carried out according to the following steps: the TiO following embodiment prepared 2nano-tube array heats taking-up after a hour at 80 DEG C, immerses 5 × 10 immediately -4molL -1n3 (in the ethanol solution of two (N, N '-2,2 '-bipyridine-4, the 4 '-dioctyl phthalate) ruthenium dye of CIS-bis-thiocyano-, adsorbs 24 hours; Afterwards by TiO 2nano-tube array takes out and rinses well with absolute ethyl alcohol, dry rear as work electrode, electrolyte is added drop-wise to Nano tube array of titanium dioxide working electrode surface, is pressed in above above-mentioned electrolyte as to electrode to sputter platinum, is prepared into DSSC.Consisting of containing 0.5M methylhexyl imidazoles iodine, 0.05M iodine, 0.1M lithium iodide of electrolyte, and the acetonitrile solution of 0.5M 4-tertiary butyl pyridine.
The photoelectric properties of the DSSC in following embodiment adopt electrochemical workstation (Model 273, EG & G) to test at ambient temperature.Light source adopts solar simulator (Newport69911) and corrects with standard silicon battery, and illuminating area is 0.2cm -2.Fill factor, curve factor (ff) refers to that (Isc is short-circuit photocurrent to the current/voltage product (Iopt*Vopt) that can to obtain in I-V curve on the point of peak power output with Isc*Voc, Voc is open-circuit photovoltage) ratio, its embodies the power output of battery with the variation characteristic of load.Photoelectric conversion efficiency (η) is then Iopt*Vopt and the ratio of the luminous power Pin of input.
Embodiment 1.
By carry out in the electrolytic solution anode polarization etch within 10 hours, prepare containing TiO 2the titanium sheet of nano-tube array (shape appearance figure as shown in Figure 3) is dipped in containing TiO 2nano particle (TiO 2nano particle footpath is 10 nanometers) mass fraction is the TiO of 2% 2in suspension-turbid liquid, electrophoretic deposition TiO 2during nano particle, direct voltage used is 5V, and the electrophoretic deposition time is 1O second, then takes out, and cleans, dry with ethanol, obtains the TiO that surface area increases 2nano-tube array work electrode (shape appearance figure as shown in Figure 4); Be soaked in N3 dyestuff after sintering, as the work electrode of DSSC.The photoelectric parameter recording this battery the results are shown in Table 1.
Embodiment 2.
By carry out in the electrolytic solution anode polarization etch within 20 hours, prepare containing TiO 2the titanium sheet of nano-tube array (shape appearance figure as shown in Figure 3) is dipped in containing TiO 2nano particle (TiO 2nano particle diameter is 12 nanometers) mass fraction is the TiO of 5% 2in suspension-turbid liquid, electrophoretic deposition TiO 2during nano particle, direct voltage used is 10V, and the electrophoretic deposition time is 30 seconds, then takes out, and cleans, dry with ethanol, obtains the TiO that surface area increases 2nano-tube array work electrode (shape appearance figure as shown in Figure 4); Be soaked in N3 dyestuff after sintering, as the work electrode of DSSC.The photoelectric parameter recording this battery the results are shown in Table 1.
Embodiment 3.
By carry out in the electrolytic solution anode polarization etch within 30 hours, prepare containing TiO 2the titanium sheet of nano-tube array (shape appearance figure as shown in Figure 3) is dipped in containing TiO 2nano particle (TiO 2nano particle diameter is 15 nanometers) mass fraction is the TiO of 5% 2in suspension-turbid liquid, electrophoretic deposition TiO 2during nano particle, direct voltage used is 15V, and the electrophoretic deposition time is 40 seconds, then takes out, and cleans, dry with ethanol, obtains the TiO that surface area increases 2nano-tube array work electrode (shape appearance figure as shown in Figure 4); Be soaked in N3 dyestuff after sintering, as the work electrode of DSSC.The photoelectric parameter recording this battery the results are shown in Table 1.
Embodiment 4.
By carry out in the electrolytic solution anode polarization etch within 40 hours, prepare containing TiO 2the titanium sheet of nano-tube array (shape appearance figure as shown in Figure 3) is dipped in containing TiO 2nano particle (TiO 2nano particle diameter is 15 nanometers) mass fraction is the TiO of 6% 2in suspension-turbid liquid, electrophoretic deposition TiO 2during nano particle, direct voltage used is 20V, and the electrophoretic deposition time is 60 seconds, then takes out, and cleans, dry with ethanol, obtains the TiO that surface area increases 2nano-tube array work electrode (shape appearance figure as shown in Figure 4); Be soaked in N3 dyestuff after sintering, as the work electrode of DSSC.The photoelectric parameter recording this battery the results are shown in Table 1.
Embodiment 5.
By carry out in the electrolytic solution anode polarization etch within 50 hours, prepare containing TiO 2the titanium sheet of nano-tube array (shape appearance figure as shown in Figure 3) is dipped in containing TiO 2nano particle (TiO 2nano particle diameter is 18 nanometers) mass fraction is the TiO of 8% 2in suspension-turbid liquid, electrophoretic deposition TiO 2during nano particle, direct voltage used is 25V, and the electrophoretic deposition time is 80 seconds, then takes out, and cleans, dry with ethanol, obtains the TiO that surface area increases 2nano-tube array work electrode (shape appearance figure as shown in Figure 4); Be soaked in N3 dyestuff after sintering, as the work electrode of DSSC.The photoelectric parameter recording this battery the results are shown in Table 1.
Embodiment 6.
By carry out in the electrolytic solution anode polarization etch within 60 hours, prepare containing TiO 2the titanium sheet of nano-tube array (shape appearance figure as shown in Figure 3) is dipped in containing TiO 2nano particle (TiO 2nano particle diameter is 20 nanometers) mass fraction is the TiO of 10% 2in suspension-turbid liquid, electrophoretic deposition TiO 2during nano particle, direct voltage used is 30V, and the electrophoretic deposition time is 120 seconds, then takes out, and cleans, dry with ethanol, obtains the TiO that surface area increases 2nano-tube array work electrode (shape appearance figure as shown in Figure 4); Be soaked in N3 dyestuff after sintering, as the work electrode of DSSC.The photoelectric parameter recording this battery the results are shown in Table 1.
Embodiment 7.
Titanium sheet is dipped in electrolyte and carries out anode polarization etching TiO 2nano-tube array, the etching voltage of use etches voltage for square wave, and voltage waveform is as shown in Figure 2; When using square wave etching voltage to etch, the time stopped under 60V is 100 milliseconds; The time stopped under 25V is 25 milliseconds, etches 10 hours altogether; Etch rear taking-up, cleaned with ethanol, dry, obtain corrugated TiO 2nano-tube array, this corrugated TiO 2nano-tube array increases TiO 2the surface area (shape appearance figure as shown in Figure 5) of nano-tube array work electrode, is soaked in N3 dyestuff, as the work electrode of DSSC after sintering.The photoelectric parameter recording this battery the results are shown in Table 1.
Embodiment 8.
Titanium sheet is dipped in electrolyte and carries out anode polarization etching TiO 2nano-tube array, the etching voltage of use etches voltage for square wave, and voltage waveform is as shown in Figure 2; When using square wave etching voltage to etch, the time stopped under 80V is 250 milliseconds; The time stopped under 10V is 100 milliseconds, etches 20 hours altogether; Etch rear taking-up, cleaned with ethanol, dry, obtain corrugated TiO 2nano-tube array, this corrugated TiO 2nano-tube array increases TiO 2the surface area (shape appearance figure as shown in Figure 5) of nano-tube array work electrode, is soaked in N3 dyestuff, as the work electrode of DSSC after sintering.The photoelectric parameter recording this battery the results are shown in Table 1.
Embodiment 9.
Titanium sheet is dipped in electrolyte and carries out anode polarization etching TiO 2nano-tube array, the etching voltage of use etches voltage for square wave, and voltage waveform is as shown in Figure 2; When using square wave etching voltage to etch, the time stopped under 80V is 500 milliseconds; The time stopped under 35V is 200 milliseconds, etches 60 hours altogether; Etch rear taking-up, cleaned with ethanol, dry, obtain corrugated TiO 2nano-tube array, this corrugated TiO 2nano-tube array increases TiO 2the surface area (shape appearance figure as shown in Figure 5) of nano-tube array work electrode, is soaked in N3 dyestuff, as the work electrode of DSSC after sintering.The photoelectric parameter recording this battery the results are shown in Table 1.
Embodiment 10.
Titanium sheet is dipped in electrolyte and carries out anode polarization etching TiO 2nano-tube array, the etching voltage of use etches voltage for square wave, and voltage waveform is as shown in Figure 2; When using square wave etching voltage to etch, the time stopped under 120V is 3000 milliseconds; The time stopped under 50V is 1000 milliseconds, etches 40 hours altogether; Etch rear taking-up, cleaned with ethanol, dry, obtain corrugated TiO 2nano-tube array, this corrugated TiO 2nano-tube array increases TiO 2the surface area (shape appearance figure as shown in Figure 5) of nano-tube array work electrode, is soaked in N3 dyestuff, as the work electrode of DSSC after sintering.The photoelectric parameter recording this battery the results are shown in Table 1.
TiO prepared by table 1 embodiment 1-10 2the photoelectric properties of the DSSC that nano-tube array is assembled into
Data from table 1 are known, electrophoretic deposition TiO 2tiO after nano particle 2nano-tube array and undulatory TiO 2the surface area of nano-tube array increases, therefore, it is possible to adsorb more polychromatophilia material, can produce larger photoelectric current during illumination, therefore, it is possible to improve the electricity conversion of DSSC.The highest electricity conversion reaches 7.36%.

Claims (4)

1. a TiO 2the preparation method of nano-tube array work electrode, is characterized in that: TiO is contained on surface 2the titanium sheet of nano-tube array is dipped in TiO 2electrophoretic deposition TiO is carried out in suspension-turbid liquid 2nano particle, electrophoretic deposition TiO 2during nano particle with platinized platinum as anode, described titanium sheet is as negative electrode; During electrophoretic deposition, direct voltage used is 5V ~ 30V, at TiO 2tiO on the surface deposition of nano-tube array 2nano particle, obtains the TiO that surface area increases 2nano-tube array work electrode.
2. method according to claim 1, is characterized in that: TiO is contained on described surface 2the titanium sheet of nano-tube array take titanium sheet as substrate, prepared in containing the electrolyte of fluorine ion by anode polarization etching method; The NH consisting of 0.5wt% of electrolyte used during etching 4the H of F, 1wt% 2the ethylene glycol of O and 98.5wt%; Adopt two electrode systems when carrying out anode polarization etching, work electrode is described titanium sheet, is platinized platinum to electrode.
3. method according to claim 1, is characterized in that: described TiO 2suspension-turbid liquid is prepared by following methods: under the condition stirred, by TiO 2colloid drops is added in absolute ethyl alcohol, makes in absolute ethyl alcohol containing TiO 2the mass fraction of nano particle is 2% ~ 10%, stirs and obtains TiO 2suspension-turbid liquid; TiO 2the particle diameter of nano particle is 10 ~ 20 nanometers.
4. method according to claim 1, is characterized in that: the time of described electrophoretic deposition is 10 seconds to 2 minutes.
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