CN103354177B - A kind of TiO preparing large-area dye-sensitized solar battery for silk-screen printing technique 2slurry and preparation method thereof - Google Patents

A kind of TiO preparing large-area dye-sensitized solar battery for silk-screen printing technique 2slurry and preparation method thereof Download PDF

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CN103354177B
CN103354177B CN201310302053.4A CN201310302053A CN103354177B CN 103354177 B CN103354177 B CN 103354177B CN 201310302053 A CN201310302053 A CN 201310302053A CN 103354177 B CN103354177 B CN 103354177B
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tio
particle diameter
slurry
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silk
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CN103354177A (en
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文贵华
顾军
邹志刚
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Jiangsu Yanchang sanglaite new energy Co., Ltd
Kunshan Innovation Institute of Nanjing University
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KUNSHAN SUNLAITE NEW ENERGY CO Ltd
Kunshan Innovation Institute of Nanjing University
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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
    • 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 present invention discloses a kind of TiO preparing large-area dye-sensitized solar battery for silk-screen printing technique 2slurry, described slurry comprises TiO 2, terpinol, ethyl cellulose, levelling agent and ethanol; Described TiO 2, terpinol, ethyl cellulose and levelling agent mass ratio be 0.5 ~ 3:3 ~ 13:0.3 ~ 2:0.1 ~ 3; Described TiO 2particle diameter be 10-30nm, wherein, by number, 10nm≤particle diameter < 20nm accounts for 10% ~ 25%, 20nm accounts for 60% ~ 75%, 20nm < particle diameter≤30nm accounts for 10-20%; The viscosity of described slurry is 2.1 × 10 5~ 2.5 × 10 5mPas.This slurry can be repeated print and can not produce be full of cracks, after high temperature sintering, and excellent bonding performance between particle, incrust, be applicable to silk-screen printing technique and prepare large-area dye-sensitized solar battery, there is industrialized mass prospect.

Description

A kind of TiO preparing large-area dye-sensitized solar battery for silk-screen printing technique 2slurry and preparation method thereof
Technical field
The invention belongs to field of dye-sensitized solar cells, be specifically related to a kind of TiO used when adopting silk-screen printing technique to prepare large-area dye-sensitized solar battery 2slurry and preparation method thereof.
Background technology
Dye-sensitized nano TiO 2solar cell becomes the focus of solar cell research gradually, and the light anode of battery is the important component part of DSSC, nano-TiO in light anode 2vital effect is played to the photoelectric properties and conversion efficiency that improve battery, studies the pure anatase structured TiO finding about 20nm through correlative study group for many years 2effectively can improve photoelectric properties and the conversion efficiency of battery.Silk-screen printing technique be preparation large area and scale DSSC usually adopt technique.
CN102231304A discloses a kind of nano-TiO 2the preparation method of slurry, the method directly adds P25 powder and pore creating material in the TiO 2 sol generated, and causes the dispersing uniformity extreme difference of P25 powder in slurry, rough surface, be made into large-area photo-anode film and easily produce be full of cracks.
CN101572190A discloses a kind of TiO of organic carrier system 2the preparation method of slurry, this slurry is by TiO 2nanometer mixed crystal joins by ethyl cellulose and terpinol 1:(10-5 in mass ratio) viscosity that formed is that the organic carrier of 5.9-6.1 Kcp obtains, the viscosity of organic carrier used is high, TiO 2there is the uneven problem of dispersion equally in nanometer mixed crystal, and TiO 2the particle diameter of nanometer mixed crystal divides face scope wide, makes large-area photo-anode film and easily produces be full of cracks and peel off.
Summary of the invention
The object of the invention is to overcome existing TiO 2the problem that slurry easily produces be full of cracks when adopting silk-screen printing technique to prepare large-area dye-sensitized solar battery and peels off, provides a kind of TiO being exclusively used in silk-screen printing technique and preparing large-area dye-sensitized solar battery 2slurry and preparation method thereof.
It is as follows that the present invention realizes the technical scheme that above-mentioned purpose adopts:
A kind of TiO preparing large-area dye-sensitized solar battery for silk-screen printing technique 2slurry,
Described slurry comprises TiO 2, terpinol, ethyl cellulose, levelling agent and ethanol;
Described TiO 2, terpinol, ethyl cellulose and levelling agent mass ratio be 0.5 ~ 3:3 ~ 13:0.3 ~ 2:0.1 ~ 3;
Described TiO 2particle diameter be 10-30nm, wherein, by number, 10nm≤particle diameter < 20nm accounts for 10% ~ 25%, 20nm accounts for 60% ~ 75%, 20nm < particle diameter≤30nm accounts for 10-20%;
The viscosity of described slurry is 2.1 × 10 5~ 2.5 × 10 5mPas.
Further, described levelling agent is OP-10 or naphthols.
Described TiO 2, terpinol, ethyl cellulose and levelling agent mass ratio be preferably 1 ~ 2:4 ~ 6:0.55 ~ 0.75:0.4 ~ 0.5.
The preparation method of described slurry, comprises the steps:
1) by TiO 2ultrasonic disperse, in ethanol, makes TiO in dispersion liquid 2by the domain size distribution of number be: 10nm≤particle diameter < 20nm accounts for 10% ~ 25%, 20nm accounts for 60% ~ 75%, 20nm < particle diameter≤30nm accounts for 10 ~ 20%;
2) ethyl cellulose ethanol dissolves;
3) successively by terpinol, levelling agent and step 2) ethyl cellulose solution be added in the dispersion liquid of step 1), through mechanical agitation and ultrasonic agitation alternate treatment, obtain colloidal solution;
4) rotary evaporation at 40 DEG C of colloidal solution described in step 3) obtains viscosity is 2.1 × 10 5~ 2.5 × 10 5the described slurry of mPas.
Further, for ease of adjustment TiO 2domain size distribution, the TiO that particle diameter is 20nm can be obtained according to following method 2:
A) be (0.20 ~ 0.21) by the mass ratio of glacial acetic acid, titanium tetraisopropylate and water: 1:(4.9 ~ 5.0), first glacial acetic acid is instilled titanium tetraisopropylate, after stirring 10 ~ 15min, then solution is instilled in water, stir 1 hour, obtain cotton-shaped liquid;
B) in the cotton-shaped liquid of step a), drip red fuming nitric acid (RFNA) by cotton-shaped liquid quality 2% ~ 2.2%, be warmed up to 80 DEG C, cool after insulation 50min, obtain colloidal solution;
C) colloidal solution reacts 12h in the autoclave of 230-240 DEG C, namely obtains the TiO that particle diameter is 20nm 2.
Adopt the oiliness TiO that the inventive method obtains 2tiO in slurry 2be uniformly dispersed, and TiO 2have specific domain size distribution at about 20nm, bulky grain increases perforated membrane to the scattering of light as scattering center, thus adds light capture ability, effectively can improve the transmission performance of electronics, and then improve photoelectricity transmission efficiency as transport layer.By improving TiO 2domain size distribution, the levelling agent that improves its dispersion and add, and control viscosity to 2.1 × 10 of slurry 5~ 2.5 × 10 5mPas, makes slurry can repeat print and can not produce be full of cracks, after high temperature sintering, and excellent bonding performance between particle, incrust, be applicable to silk-screen printing technique and prepare large-area dye-sensitized solar battery, there is industrialized mass prospect.
Accompanying drawing explanation
Fig. 1 is TiO prepared by the present invention 2electron microscopic picture.
Fig. 2 is mixed TiO 2electron microscopic picture.
Fig. 3 is TiO after mixing 2domain size distribution statistics.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further details.
Due to commercially available TiO 2domain size distribution wider, for obtaining the TiO of domain size distribution of the presently claimed invention 2, adopt commercially available particle diameter to be the TiO of 10-30nm 2aqueous liquid dispersion and homemade particle diameter are the TiO of 20nm 2carry out mixture, to adjust domain size distribution, domain size distribution can be obtained by statistics by transmission electron microscope or scanning electron microscopic picture.
embodiment 1
Prepare the TiO that particle diameter is 20nm 2:
(1) take titanium tetraisopropylate 29g, glacial acetic acid 6g, glacial acetic acid is dropwise added in titanium tetraisopropylate, stir 10 ~15min, is added drop-wise to solution in the deionized water of 143g in 3 ~ 5min, produces white flock precipitate, vigorous stirring 1 hour;
In above-mentioned cloudy solution, drip 2.6ml red fuming nitric acid (RFNA) (commercially available 65wt%, 1.4g/ml), the pre-heat treatment is carried out to solution: in 40min, be raised to 80 DEG C by room temperature, and be incubated 50min, obtain transparent light blue colloidal solution, be cooled to room temperature;
Above-mentioned colloidal solution deionized water is settled to 185mL, pours in the autoclave of 250ml, at 240 DEG C of reaction under high pressure 12h;
After reaction, drip 1.2ml red fuming nitric acid (RFNA) to reactant liquor, ultrasonic disperse, centrifugation, removing liquid, then use ethanol purge, repeatedly carry out three times, confirm through Electronic Speculum the TiO obtaining the 20nm of uniform particle diameter 2nanocrystalline (as Fig. 1) about 5g.
TiO 2the preparation of slurry:
Be the TiO of 10-30nm by commercially available particle diameter 2aqueous liquid dispersion (solid content 30%) 20g and homemade TiO 2nanocrystallinely to mix, be scattered in 120ml ethanol after centrifugal, ethanol purge again, carry out number by transmission electron microscope photo through domain size distribution software to add up and confirm (as Fig. 2 and 3), 10nm≤particle diameter < 20nm accounts for 24%, 20nm accounts for 64%, 20nm < particle diameter≤30nm accounts for 12%.
Ethyl cellulose is mixed with the ethanolic solution of 10wt%.
To above-mentioned TiO 240g terpinol is added successively, 4g OP-10(commercial emulsifier in alcohol dispersion liquid), 55g ethyl cellulose ethanolic solution, the colloidal solution obtained carries out mechanical agitation and ultrasonic agitation, alternate treatment three times.
The colloidal solution obtained heats in the water-bath of 40 DEG C, carries out rotary evaporation, and obtaining viscosity is 2.15 × 10 5the TiO of mPas 2slurry.
embodiment 2
Prepare the TiO that particle diameter is 20nm 2:
(1) take titanium tetraisopropylate 36.6g, glacial acetic acid 7.7g, glacial acetic acid is dropwise added in titanium tetraisopropylate, stir 10 ~15min, is added drop-wise to solution in the deionized water of 181g in 3 ~ 5min, produces white flock precipitate, vigorous stirring 1 hour;
In above-mentioned cloudy solution, drip 3.5ml red fuming nitric acid (RFNA) (commercially available 65wt%, 1.4g/ml), the pre-heat treatment is carried out to solution: in 45min, be raised to 80 DEG C by room temperature, and be incubated 50min, obtain transparent light blue colloidal solution, be cooled to room temperature;
Above-mentioned colloidal solution deionized water is settled to 239mL, pours in the autoclave of 300ml, at 230 DEG C of reaction under high pressure 12h;
After reaction, drip 1.52ml red fuming nitric acid (RFNA) to reactant liquor, ultrasonic disperse, centrifugation, removing liquid, then use ethanol purge, repeatedly carry out three times, confirm through Electronic Speculum the TiO obtaining the 20nm of uniform particle diameter 2nanocrystalline about 6g.
TiO 2the preparation of slurry:
Be the TiO of 10-30nm by commercially available particle diameter 2aqueous liquid dispersion (solid content 30%) 30g and homemade TiO 2nanocrystallinely to mix, be scattered in 120ml ethanol after centrifugal, ethanol purge again, carry out number by transmission electron microscope photo through domain size distribution software to add up and confirm, 10nm≤particle diameter < 20nm accounts for 17%, 20nm accounts for 68%, 20nm < particle diameter≤30nm accounts for 15%.
Ethyl cellulose is mixed with the ethanolic solution of 10wt%.
To above-mentioned TiO 2add 50g terpinol successively in alcohol dispersion liquid, 5g OP-10,75g ethyl cellulose ethanolic solution, the colloidal solution obtained carries out mechanical agitation and ultrasonic agitation, alternate treatment three times.
The colloidal solution obtained heats in the water-bath of 40 DEG C, carries out rotary evaporation, and obtaining viscosity is 2.3 × 10 5the TiO of mPas 2slurry.
embodiment 3
Prepare the TiO that particle diameter is 20nm 2:
(1) take titanium tetraisopropylate 50g, glacial acetic acid 10.24g, glacial acetic acid is dropwise added in titanium tetraisopropylate, stir 10 ~15min, is added drop-wise to solution in the deionized water of 247.4g in 3 ~ 5min, produces white flock precipitate, vigorous stirring 1 hour;
In above-mentioned cloudy solution, drip 4.75ml red fuming nitric acid (RFNA) (commercially available 65wt%, 1.4g/ml), the pre-heat treatment is carried out to solution: in 50min, be raised to 80 DEG C by room temperature, and be incubated 50min, obtain transparent light blue colloidal solution, be cooled to room temperature;
Above-mentioned colloidal solution deionized water is settled to 320mL, pours in the autoclave of 500ml, at 240 DEG C of reaction under high pressure 12h;
After reaction, drip 1.2ml nitric acid to reactant liquor, ultrasonic disperse, centrifugation, removing liquid, then use ethanol purge, repeatedly carry out three times, obtain the TiO of the 20nm of uniform particle diameter 2nanocrystalline about 9g.
TiO 2the preparation of slurry:
Be the TiO of 10-30nm by commercially available particle diameter 2aqueous liquid dispersion (solid content 30%) 20g and homemade TiO 2mixing, be scattered in 120ml ethanol after centrifugal, ethanol purge again, carry out number by transmission electron microscope photo through domain size distribution software to add up and confirm, 10nm≤particle diameter < 20nm accounts for 16%, 20nm accounts for 74%, 20nm < particle diameter≤30nm accounts for 10%.
Ethyl cellulose is mixed with the ethanolic solution of 10wt%.
To above-mentioned TiO 2add 60g terpinol successively in alcohol dispersion liquid, 5g OP-10,75g ethyl cellulose ethanolic solution, the colloidal solution obtained carries out mechanical agitation and ultrasonic agitation, alternate treatment three times.
The colloidal solution obtained heats in the water-bath of 40 DEG C, carries out rotary evaporation, and obtaining viscosity is 2.2 × 10 5the TiO of mPas 2slurry.
Adopt the oiliness TiO that the inventive method obtains 2tiO in slurry 2be uniformly dispersed, and TiO 2have specific domain size distribution at about 20nm, bulky grain increases perforated membrane to the scattering of light as scattering center, thus adds light capture ability, effectively can improve the transmission performance of electronics, and then improve photoelectricity transmission efficiency as transport layer.By improving TiO 2domain size distribution, the levelling agent that improves its dispersion and add, and control viscosity to 2.1 × 10 of slurry 5~ 2.5 × 10 5mPas, makes slurry can repeat print and can not produce be full of cracks, after high temperature sintering, excellent bonding performance between particle, incrustly (if only improve domain size distribution, or only adds levelling agent, or only adjust slurry viscosity, the problem of still can produce be full of cracks, peeling off), TiO of the present invention 2slurry is applicable to silk-screen printing technique and prepares large-area dye-sensitized solar battery, has industrialized mass prospect.

Claims (4)

1. prepare the TiO of large-area dye-sensitized solar battery for silk-screen printing technique for one kind 2slurry, is characterized in that: described slurry comprises TiO 2, terpinol, ethyl cellulose, levelling agent and ethanol;
Described TiO 2, terpinol, ethyl cellulose and levelling agent mass ratio be 0.5 ~ 3:3 ~ 13:0.3 ~ 2:0.1 ~ 3;
Described TiO 2particle diameter be 10-30nm, wherein, by number, 10nm≤particle diameter < 20nm accounts for 10% ~ 25%, 20nm accounts for 60% ~ 75%, 20nm < particle diameter≤30nm accounts for 10 ~ 20%;
The viscosity of described slurry is 2.1 × 10 5~ 2.5 × 10 5mPas.
2. the TiO of large-area dye-sensitized solar battery is prepared according to claim 1 for silk-screen printing technique 2slurry, is characterized in that: described levelling agent is OP-10 or naphthols.
3. the preparation method of slurry described in claim 1, is characterized in that, comprises the steps:
1) by TiO 2ultrasonic disperse, in ethanol, makes TiO in dispersion liquid 2by the domain size distribution of number be: 10nm≤particle diameter < 20nm accounts for 10% ~ 25%, 20nm accounts for 60% ~ 75%, 20nm < particle diameter≤30nm accounts for 10-20%;
2) ethyl cellulose ethanol dissolves;
3) successively by terpinol, levelling agent and step 2) ethyl cellulose solution be added in the dispersion liquid of step 1), through mechanical agitation and ultrasonic agitation alternate treatment, obtain colloidal solution;
4) rotary evaporation at 40 DEG C of colloidal solution described in step 3) obtains viscosity is 2.1 × 10 5~ 2.5 × 10 5the described slurry of mPas.
4. the preparation method of slurry according to claim 3, is characterized in that: obtain according to following method the TiO that particle diameter is 20nm 2:
A) be (0.20 ~ 0.21) by the mass ratio of glacial acetic acid, titanium tetraisopropylate and water: 1:(4.9 ~ 5.0), first glacial acetic acid is instilled titanium tetraisopropylate, after stirring 10 ~ 15min, then solution is instilled in water, stir 1 hour, obtain cotton-shaped liquid;
B) in the cotton-shaped liquid of step a), drip red fuming nitric acid (RFNA) by cotton-shaped liquid quality 2% ~ 2.2%, be warmed up to 80 DEG C, cool after insulation 50min, obtain colloidal solution;
C) colloidal solution reacts 12h in the autoclave of 230-240 DEG C, namely obtains the TiO that particle diameter is 20nm 2.
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CN103794376B (en) * 2014-02-21 2017-02-15 南京大学昆山创新研究院 Sizing agent for dyeing light scattering layer on DSSC photoanode and preparation method thereof
CN104028256B (en) * 2014-06-04 2016-01-13 合肥工业大学 A kind of porous TiO 2the preparation method of film
CN104392842A (en) * 2014-11-21 2015-03-04 南京大学昆山创新研究院 Large-area dye-sensitized solar cell and manufacturing method thereof
CN107742580B (en) * 2017-09-15 2019-06-28 华南农业大学 A method of quantum dot solar battery is prepared based on light absorption paint
CN109535782B (en) * 2018-11-07 2021-01-26 三峡大学 TiO22Composite hydrophobic ice-phobic coating and preparation method thereof

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