CN1905215A - Process for preparing TiO2 nanocrystal porous film electrode by low-temp. electrophoresis sedimentation - Google Patents
Process for preparing TiO2 nanocrystal porous film electrode by low-temp. electrophoresis sedimentation Download PDFInfo
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- CN1905215A CN1905215A CNA2005100122546A CN200510012254A CN1905215A CN 1905215 A CN1905215 A CN 1905215A CN A2005100122546 A CNA2005100122546 A CN A2005100122546A CN 200510012254 A CN200510012254 A CN 200510012254A CN 1905215 A CN1905215 A CN 1905215A
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Abstract
The invention belongs to the manufacturing technical field of dye sensibilized TiO2 nanocrystalline porous thin film electrode and photo- catalyzed electrode, especially relating to a method for preparing TiO2 nanocrystalline porous thin film electrode at low temperature by electrophoretic deposition, mixing alcohol solution containing Ti salt or not with TiO2 grains, making TiO2 colloidal solution by supersonic diffusion, depositing TiO2 colloidal solution on clean conducting substrate by electrophoretic deposition to make TiO2 thin film electrode; and preparing TiO2 nanocrystalline porous thin film electrode at low temperature by postprocessing. And the preparing method is easy to operate, saving energy sources, low-cost, fast to form film, and especially applied to low temperature preparation of flexible TiO2 nanocrystalline porous thin film electrode.
Description
Technical field
The invention belongs to dye sensitization TiO
2The manufacturing technology field of nano-crystal porous film electrode and photochemical catalyst electrode particularly contains titanium salt or does not contain the alcoholic solution and the TiO of titanium salt
2Particle mixing and the TiO that forms through ultrasonic dispersion
2Colloidal solution prepares TiO at low temperatures by electrophoretic deposition and reprocessing
2The method of nano-crystal porous film electrode.
Background technology
At dye sensitization TiO
2In the Na crystal porous membrane solar cell, dye sensitization TiO
2Nano-crystal porous film electrode is being born the effect of absorbing dye, separated charge and transmission light induced electron.In this battery, TiO
2Na crystal porous membrane has bigger serface and high porosity.This not only helps the absorption of a large amount of dye molecules, thereby can improve the luminous energy absorption efficiency of battery, also helps the transmission of electronics in nano-crystal thin-film and then the photoelectric conversion efficiency of raising battery simultaneously.Traditional TiO
2The preparation method of nano-crystal porous film electrode is with TiO
2Colloid is coated on the conductive substrates, makes TiO through 400 ℃～450 ℃ high temperature sinterings again
2Between the particle and TiO
2Combine between particle and the conductive substrates and firmly form good electrical contact, and can remove organic residue, thereby improve TiO
2The stability of electron transport speed and electrode is [as document " Nanocrystalline titanium oxide electrodes for photovoltaicapplications " Journal of the American Ceramic Society in the Na crystal porous membrane, 80 (1997), 3157～3171 is disclosed].The conductive substrates of extensive use now is electro-conductive glass and flexible conducting material.In DSSC, substitute the electro-conductive glass base material with flexible conducting material and be a kind of inevitable trend, heavy because it not only can overcome electro-conductive glass, frangible, shortcoming such as freely deformable can not realize TiO simultaneously
2The spool industrialization of nano-crystal porous film electrode is produced continuously [as document " Performance and stability of TiO
2/ dye solar cells assembled withflexible electrodes and a polymer electrolyte " Journal ofPhotochemistry and Photobiology A:Chemistry 159 (2003) 33～39 is disclosed].But flexible conducting material non-refractory (≤150 ℃), the high temperature sintering method of traditional preparation process electrode can be destroyed flexible conducting material.Adopt manual method of filming to cause thickness thin uneven easily simultaneously, and thickness is uncontrollable in a big way, has therefore influenced TiO
2Nano-crystal porous film electrode performance stable and repeated.
Summary of the invention
A purpose of the present invention is to overcome the deficiency of above-mentioned prior art, adopts the alcoholic solution and the TiO that contain titanium salt or do not contain titanium salt
2Particle mixes and makes TiO through the method for ultrasonic dispersion
2Colloidal solution, it is even that the reprocessing by electrophoretic deposition and certain condition just can make thickness at low temperatures, and stability is better, does not contain the TiO of other organic impurities again
2Nano-crystal porous film electrode.
Another object of the present invention is to provide electrophoretic deposition to prepare dye sensitization TiO
2The method of nano-crystal porous film electrode.
The method that electrophoretic deposition low temperature of the present invention prepares TiO 2 nanocrystal porous film electrode may further comprise the steps:
(1) with alcoholic solution with after titanium dioxide granule mixes by a certain percentage, make colloidal tio 2 through ultrasonic dispersion;
(2) the colloidal tio 2 electrophoretic deposition with step (1) gained makes titanium dioxide membrane electrode provided on the conductive substrates that cleans up;
(3) after the titanium dioxide membrane electrode provided air dry with step (2), select for use again in 40 ℃～100 ℃ hot-air atmosphere and handle, handle in 40 ℃～100 ℃ steam atmosphere, any one method under 40 ℃～100 ℃ temperature in three kinds of methods such as poach, or three kinds of methods are united use in any order, obtain TiO 2 nanocrystal porous film electrode of the present invention.
Described conductive substrates is selected from the electric conducting material of electro-conductive glass or flexible substrate without limitation, as PET/ITO etc.
Described alcoholic solution is selected from one or more the mixture in ethanol, isopropyl alcohol, the n-butanol without limitation, is preferably the mixed solution of ethanol, isopropyl alcohol, n-butanol; Wherein, n-butanol: isopropyl alcohol: the volume ratio of ethanol is 8: 2: 2～8: 5: 2, is preferably 8: 4: 2.
Contain titanium salt in the described alcoholic solution, described titanium salt is a butyl titanate, tetraisopropyl titanate, metatitanic acid four own esters or tetraethyl titanate etc.Be preferably the mixed solution of butyl titanate and ethanol, isopropyl alcohol and n-butanol; Wherein, n-butanol: isopropyl alcohol: the volume ratio of ethanol is 8: 2: 2～8: 5: 2, is preferably 8: 4: 2.
Described alcoholic solution and TiO
2After particle mixes, the TiO that makes through ultrasonic dispersion
2TiO in the colloid
2Concentration is 30g/l～50g/l.Be preferably 50g/l.
Described alcoholic solution and the TiO that contains titanium salt
2After particle mixes, the TiO that makes through ultrasonic dispersion
2Butyl titanate in the colloid, tetraisopropyl titanate, the concentration of metatitanic acid four own esters or tetraethyl titanate etc. is 0g/l～50g/l, is preferably 34g/l.TiO
2Concentration be 30g/l～50gl/l, be preferably 50g/l.
TiO of the present invention
2Particle can be by hydrothermal synthesis method, and methods such as sol-gel process prepare, and is selected from commodity TiO without limitation
2Powder (UV100 that P25 that German Degussa company produces or Switzerland SachtlebenChemie GmbH company produce) or other commodity or noncommodity are received brilliant TiO
2Particle is preferably P25.Granular size is 10nm～200nm.
TiO of the present invention
2The preparation method of colloid: will contain titanium salt or not contain the alcoholic solution and the TiO of titanium salt
2Particle mixes the stirring ultrasonic dispersion in back in about 2 hours by a certain percentage and makes TiO about 30 minutes
2Colloid.
TiO of the present invention
2The electrophoretic deposition of colloid: two conductive substrates that clean up are inserted TiO
2In the colloidal solution, (the parallel relative spacing 0.5～2cm of conducting surface of 2cm * 2cm) is preferably 1.0cm to conductive substrates; On two conductive substrates, add 30～80V direct voltage, continue 5～60s, preferred deposition time 30s.Deposition finishes, and the conductive substrates that will connect dc power cathode is taken out, as seen with conductive substrates that negative pole links to each other on deposit TiO
2, form TiO
2Deposited film makes TiO
2The membrane electrode semi-finished product.Adhesive liquor alcoholic solution on the film is preferably butanol solution and washes.
The present invention will deposit TiO
2The conductive substrates membrane electrode adopt earlier natural seasoning in air, to dry after, handled 1～10 hour with dry air heating or humid air heating again, used the water-boiling method heat treated at last 2～12 hours, can make TiO of the present invention
2Nano-crystal porous film electrode.
Described natural seasoning is with TiO
2Conductive substrates membrane electrode semi-finished product place natural environment to volatilize fully up to the alcoholic solvent of film.
Described dry air heating is with the TiO after the air dry
2The conductive substrates membrane electrode was placed 1～10 hour in 40 ℃～100 ℃ hot-air atmosphere.
Described humid air heating is with the TiO after the air dry
2Conductive substrates membrane electrode semi-finished product are placed in 40 ℃～100 ℃ steam atmosphere, and directly do not contact with water, place 1～10 hour.The effect of this processing is to make TiO
2Between the particle and TiO
2Combine between particle and the conductive substrates firmly, improve mechanical performance.The temperature of humid air heating is 40 ℃～100 ℃ among the present invention, is preferably 40 ℃.
Described water-boiling method is with TiO
2Conductive substrates membrane electrode semi-finished product are immersed in the non-closed container that fills redistilled water, under 40 ℃～100 ℃ temperature, place 2～12 hours.This heat treated effect is to promote TiO
2The crystallization of particle is connected with conduction, and the TiO by generating after the titanium salt solution hydrolysis
2Make TiO as bonding agent
2Between the particle and TiO
2Combine firmly between particle and the conductive substrates.The water-boiling method heat treatment temperature is 40 ℃～100 ℃ among the present invention, is preferably 100 ℃.
The TiO 2 nanocrystal porous film that method of the present invention is obtained is again according to the known preparation dye sensitization TiO of those skilled in the art
2The method of nano-crystal porous film electrode is prepared, and can access dye sensitization TiO
2Nano-crystal porous film electrode.For example use document " A new method for manufacturingnanostructured electrodes on glass substrates " { Solar EnergyMaterials﹠amp; The method of introducing among Solar Cells 73 (2002) 91～101}, the document and the document of quoting in the document all are incorporated herein by reference with it in full at this.
Dye sensitization TiO
2Nano-crystal porous film electrode also can be prepared as follows and obtain: the TiO 2 nanocrystal porous film that method of the present invention is obtained is heating 1 hour under 100 ℃ the condition in temperature again.Subsequently electrode is immersed 5 * 10
-4M 4, take out after 12 hours in the ethanolic solution of 4 '-dicarboxylic acids bipyridyl ruthenium (along closing ruthenium (II) in two thiocyanates-two (2,2 '-bipyridine-4,4 '-dicarboxylic acids)), can make dye sensitization TiO with drying after the absolute ethyl alcohol flushing
2Nano-crystal porous film electrode.
The TiO that the present invention prepares with electrophoretic deposition low temperature
2Nano-crystal porous film electrode is specially adapted to flexible TiO in the flexible dye-sensitized nano-crystal thin-film solar cell
2Nano-crystal porous film electrode.
Preparation method of the present invention is easy and simple to handle, energy savings, and cost is low, and film forming is fast, and thickness of deposited film is advantage such as homogeneous and controllable in a big way, and is specially adapted to flexible TiO
2The low temperature preparation of nano-crystal porous film electrode, thus the destruction of high temperature sintering can be avoided to the compliant conductive substrate.Prepared TiO
2Nano-crystal porous film electrode can be applicable to fields such as DSSC and photoelectrocatalysielectrode electrode.The electrode of preparing can be used in the compliant conductive substrate, is dye sensitization TiO
2The Na crystal porous membrane solar cell provides more economical effective electrode low temperature preparation method.
The present invention will describe by the following examples.But, be to be understood that the present invention is not limited to particular example described here and embodiment.The purpose that comprises these particular example and embodiment here is to help those of skill in the art to put into practice the present invention.Any those of skill in the art are easy to be further improved without departing from the spirit and scope of the present invention and perfect, therefore the present invention only is subjected to the restriction of the content and the scope of claim of the present invention, and its intention contains all and is included in interior alternative or the equivalent of spirit and scope of the invention that appendix claim limits.
The subordinate list explanation: table 1 is to use the dye sensitization TiO of electrophoretic deposition low temperature preparation of the present invention
2Nano-crystal porous film electrode and platinum are to the photoelectric properties of the DSSC of electrode assembling.
Method of measurement: with the TiO of dye sensitization the present invention preparation
2Nano-crystal porous film electrode uses the platinized platinum conduct to electrode as work electrode.With containing 0.5M LiI, 0.05M I
2With the trimethoxy propionitrile solution of 0.5M four tertiary butyl pyridines as electrolyte, be assembled into DSSC and carry out photoelectric properties and measure.
(Model 273, EG﹠amp for potentiostat/galvanostat that the photoelectric properties of battery are computerizedd control; G) at room temperature measure.Light source uses 250W tungsten halogen lamp, incident intensity 60mW/cm
2, illuminating area 0.2cm
2Except as otherwise noted, the measurement of photoelectric properties of the present invention is all carried out under room temperature (25 ℃).
Embodiment
Embodiment 1
(1) takes by weighing 0.5g TiO
2Particle (P25) is put in the 10ml butanol solution to mix and stirs after 2 hours ultrasonic dispersion and made TiO in 30 minutes
2Colloid.
(2) use two SnO that mix fluorine
2Electro-conductive glass (FTO) (Heilungkiang Haake new forms of energy Co., Ltd, square resistance 30 Ω cm
-2) as electrode substrate, the parallel TiO that inserts relatively of conducting surface
2In the colloidal solution, spacing is 1cm, electrophoretic deposition 30s.The glass electrode that connects power cathode is taken out, and the visible deposition film forms.Rinse out adhesive liquor on the film with butanol solution, obtain TiO
2Membrane electrode.
(3) with the TiO that makes
2Membrane electrode dries the back naturally and promptly obtained TiO of the present invention in 30 minutes at 450 ℃ of following high temperature sinterings
2Nano-crystal porous film electrode.
Embodiment 2
Remove TiO in the step (1)
2Particle weight changes into beyond the 0.4g, and other step and process conditions are identical with embodiment 1, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 3
Remove TiO in the step (1)
2Particle weight changes into beyond the 0.3g, and other step and process conditions are identical with embodiment 1, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 4
Post-processing approach in the step (3) is changed into: with the TiO that makes
2Immerse after membrane electrode dries naturally again and fill in the non-closed container of redistilled water, heating after 4 hours is poured out water under 100 ℃ of conditions, heats 1 hour in 100 ℃ of following air again, and other step and process conditions are identical with embodiment 1, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 5
Remove TiO in the step (1)
2Particle weight changes into beyond the 0.4g, and other step and process conditions are identical with embodiment 4, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 6
Remove TiO in the step (1)
2Particle weight changes into beyond the 0.3g, and other step and process conditions are identical with embodiment 4, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 7
Take by weighing the 0.034g butyl titanate, 0.5gTiO
2Particle (P25) is measured the 10ml n-butanol, mix to stir after 2 hours ultrasonic dispersion and makes TiO in 30 minutes
2Colloid.
Use the electrophoretic deposition method of step (2) among the embodiment 1 to prepare TiO
2Membrane electrode.
With the TiO that makes
2Membrane electrode dries back elder generation (electrode does not directly contact with water) humid air in 50 ℃ of steam atmosphere naturally and heated 2 hours, again electrode is immersed and fill in the non-closed container of redistilled water, the poach heating after 4 hours is poured out water under 100 ℃ of conditions, heated again 1 hour in 100 ℃ of following air, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 8
Except that 50 ℃ of following humid air heating in the step (3) being become in 50 ℃ of following dry air heating 2 hours in 2 hours, other step and process conditions are identical with embodiment 7, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 9
Except that humid air heating-up temperature in the step (3) is become 100 ℃ by 50 ℃, other step and process conditions are identical with embodiment 7, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 10
Except that dry air heating-up temperature in the step (3) is become 100 ℃ by 50 ℃, other step and process conditions are identical with embodiment 8, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 11
Take by weighing the 0.034g butyl titanate, 0.5gTiO
2Particle (P25) is measured the 8ml n-butanol, the 4ml isopropyl alcohol, and the 2ml absolute ethyl alcohol mix to stir after 2 hours ultrasonic dispersion and made TiO in 30 minutes
2Colloid.
Use the electrophoretic deposition method of step (2) among the embodiment 1 to prepare TiO
2Membrane electrode, other step and process conditions are identical with embodiment 7, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 12
Except that 50 ℃ of following humid air heating in the step (3) being become 50 ℃ of following dry air heating, other step and process conditions are identical with embodiment 11, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 13
Except that humid air heating-up temperature in the step (3) is become 40 ℃ by 50 ℃, other step and process conditions are identical with embodiment 11, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 14
Except that 40 ℃ of following humid air heating in the step (3) being become 40 ℃ of following dry air heating, other step and process conditions are identical in embodiment 13, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 15
Except that humid air heating-up temperature in the step (3) is become 60 ℃ by 50 ℃, other step and process conditions are identical with embodiment 11, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 16
Except that 60 ℃ of following humid air heating in the step (3) being become 60 ℃ of following dry air heating, other step and process conditions are identical with embodiment 15, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 17
Prepare TiO as the method among the embodiment 14
2Colloid and TiO
2Membrane electrode.
With the TiO that makes
2Membrane electrode 40 ℃ of following dry air heating 2 hours, carries out electrophoretic deposition one time, sedimentation time 15s, glass electrode spacing 1.0cm earlier again.Rinse out adhesive liquor on the film with butanol solution, heating 2 hours in 40 ℃ of following dry air once more after drying is naturally immersed then and is filled in the non-closed container of redistilled water poach heating 4h under 100 ℃ of conditions.Water is poured out, in air, heated 2h again under 100 ℃, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Embodiment 18
(PET/ITO, will film Science and Technology Ltd., square resistance 90 Ω cm are held high in Shenzhen except that changing electro-conductive glass substrate in the step (2) into flexible substrates
-2), the electrophoretic deposition time is become by 30s beyond the 2min, and other step and process conditions are identical with embodiment 14, obtain TiO of the present invention
2Nano-crystal porous film electrode.
Table 1
| Embodiment | Short-circuit photocurrent Isc (mAcm -2) | Open circuit photovoltage Voc (mV) | Photoelectric conversion efficiency η (%) | Fill factor, curve factor FF |
| 1 | 9.75 | 712 | 4.90 | 0.71 |
| 2 | 9.30 | 706 | 4.37 | 0.67 |
| 3 | 7.45 | 716 | 3.63 | 0.68 |
| 4 | 2.85 | 776 | 1.67 | 0.76 |
| 5 | 1.50 | 754 | 0.86 | 0.76 |
| 6 | 2.50 | 780 | 1.51 | 0.77 |
| 7 | 4.05 | 758 | 2.46 | 0.80 |
| 8 | 5.15 | 768 | 3.08 | 0.78 |
| 9 | 2.70 | 778 | 1.60 | 0.76 |
| 10 | 4.70 | 768 | 2.92 | 0.81 |
| 11 | 6.25 | 774 | 3.66 | 0.76 |
| 12 | 6.80 | 774 | 3.93 | 0.75 |
| 13 | 7.20 | 796 | 4.59 | 0.80 |
| 14 | 7.75 | 776 | 4.66 | 0.78 |
| 15 | 4.90 | 792 | 3.18 | 0.82 |
| 16 | 5.70 | 790 | 3.54 | 0.79 |
| 17 | 9.35 | 770 | 5.37 | 0.75 |
| 18 | 4.55 | 776 | 2.36 | 0.67 |
Claims (10)
1. an electrophoretic deposition low temperature prepares the method for TiO 2 nanocrystal porous film electrode, and it is characterized in that: described method may further comprise the steps:
(1) with alcoholic solution with after titanium dioxide granule mixes, make colloidal tio 2 through ultrasonic dispersion;
(2) the colloidal tio 2 electrophoretic deposition with step (1) gained makes titanium dioxide membrane electrode provided on the conductive substrates that cleans up;
(3) after the titanium dioxide membrane electrode provided air dry with step (2), select for use again in 40 ℃～100 ℃ hot-air atmosphere and handle, handle in 40 ℃～100 ℃ steam atmosphere, any one method under 40 ℃～100 ℃ temperature in three kinds of methods of poach is handled, or three kinds of methods are united use in any order, obtain TiO 2 nanocrystal porous film electrode.
2. method according to claim 1 is characterized in that: the titanium dioxide concentration in the described colloidal tio 2 is 30g/l～50g/l.
3. method according to claim 1 and 2 is characterized in that: described titanium dioxide granule size is 10nm～200nm.
4. method according to claim 1 and 2 is characterized in that: contain butyl titanate in the described colloidal tio 2, tetraisopropyl titanate, metatitanic acid four own ester or tetraethyl titanates; Butyl titanate, tetraisopropyl titanate, the concentration of metatitanic acid four own esters or tetraethyl titanate is 0g/l～50g/l.
5. method according to claim 1 is characterized in that: described alcoholic solution is selected from one or more the mixture in ethanol, isopropyl alcohol, the n-butanol.
6. method according to claim 1 and 2 is characterized in that: described alcoholic solution is the mixed solution of ethanol, isopropyl alcohol, n-butanol; Wherein, n-butanol: isopropyl alcohol: the volume ratio of ethanol is 8: 2: 2～8: 5: 2.
7. method according to claim 1 is characterized in that: described electrophoretic deposition is that two conductive substrates that clean up are inserted in the colloidal tio 2 solution, the parallel relative spacing 0.5～2cm of the conducting surface of conductive substrates; On two conductive substrates, add 30～80V direct voltage, continue deposition 5～60s.
8. method according to claim 1 is characterized in that: describedly placed 1～10 hour in 40 ℃～100 ℃ hot-air atmosphere.
9. method according to claim 1 is characterized in that: describedly in 40 ℃～100 ℃ steam atmosphere, place 1～10 hour, and TiO
2Conductive substrates membrane electrode semi-finished product directly do not contact with water.
10. method according to claim 1 is characterized in that: describedly carrying out poach under 40 ℃～100 ℃ temperature, is with TiO
2Conductive substrates membrane electrode semi-finished product are immersed in the non-closed container that fills redistilled water and placed under assigned temperature 2～12 hours.
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| CN102168242A (en) * | 2011-04-14 | 2011-08-31 | 南昌航空大学 | Method for preparing colorful titanium dioxide film on surface of porous NiTi alloy at low temperature |
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| CN103924281B (en) * | 2014-04-26 | 2017-08-25 | 广州天极电子科技有限公司 | A kind of method that function film is prepared using conductivity ceramics as substrate electrophoresis |
| CN107177846A (en) * | 2017-05-10 | 2017-09-19 | 同济大学 | A kind of preparation method and applications of two-layer electrode |
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| CN114203967A (en) * | 2021-11-05 | 2022-03-18 | 东方电气集团科学技术研究院有限公司 | Preparation method of novel lithium ion battery negative electrode plate by colloid electrophoresis |
| CN114203967B (en) * | 2021-11-05 | 2024-03-15 | 东方电气集团科学技术研究院有限公司 | Preparation method of novel lithium ion battery negative electrode plate through colloid electrophoresis |
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