CN102280271B - Preparation method of screen-printing slurry specially used by dye-sensitized solar cell - Google Patents

Preparation method of screen-printing slurry specially used by dye-sensitized solar cell Download PDF

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CN102280271B
CN102280271B CN201010564588A CN201010564588A CN102280271B CN 102280271 B CN102280271 B CN 102280271B CN 201010564588 A CN201010564588 A CN 201010564588A CN 201010564588 A CN201010564588 A CN 201010564588A CN 102280271 B CN102280271 B CN 102280271B
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ethanol
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quality
titanium dioxide
nano
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CN102280271A (en
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汪远昊
杨洪兴
吕琳
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Hong Kong Polytechnic University HKPU
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Hong Kong Polytechnic University HKPU
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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
    • 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
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention relates to a preparation method of a screen-printing slurry specially used by a dye-sensitized solar cell. The method comprises the following steps: (1), mixing titanium dioxide powder, ethanol and acetic acid with stirring so as to obtain a first mixed solution; (2), mixing terpineol, ethanol and the first mixed solution with stirring so as to obtain a second mixed solution; (3), mixing ethyl cellulose, ethanol and the second mixed solution with stirring so as to obtain a screen-printing slurry specially used by a dye-sensitized solar cell. According to the invention, beneficial effects of the preparation method are as follows: a slurry obtained by the preparation method has advantages of even distribution and good repeatability; meanwhile, a process of low-temperature reduced pressure distillation is avoided according to the preparation method; and instruments that are involved in the preparation method are easy to operate and steps are simple without trifles; therefore, the screen-printing slurry is convenient for mass production that indicates an advantage of industrialization.

Description

The preparation method of the special-purpose silk screen printing slurry of DSSC
Technical field
The present invention relates to a kind of preparation method of silk screen printing slurry, more particularly, relate to the preparation method of the special-purpose silk screen printing slurry of a kind of DSSC.
Background technology
DSSC; As one of outstanding representative of third generation solar cell; Because it is preparation technology easily, higher photoelectric conversion efficiency and cheap production cost receive showing great attention to of countries in the world solar cell enterprise and scientific research institutions always.The anode of DSSC is as one of core component, usually with electro-conductive glass as substrate, cover several microns nano-crystalline titanium dioxide films of one deck on it to tens micron thick.At present, traditional anode preparation method be adopt screen printing technique with the titania slurry silk-screen for preparing on electro-conductive glass.One big advantage of this method is to be easy to control thickness, is convenient to industrialization.Photovoltaic performance is DSSC preferably; The titanium deoxid film that its anode surface covered must be evenly; Should reduce the reunion of nano particle in the middle of the microstructure as far as possible; Thereby avoid the increase of electron recombination effect and the enhancing of light scattering effect, and the quality of this slurry of using when depending primarily on silk screen printing.Therefore, the nano-crystalline titanium dioxide slurry of a high-quality is very crucial for the performance of battery.
In the middle of the preparation technology of the special-purpose silk screen printing slurry of traditional DSSC, a core procedure is the low-temperature reduced-pressure distillation, and this step need be used more equipment; Like outstanding steaming equipment; Vacuum equipment etc., and technology is loaded down with trivial details, and therefore being not easy to industrialization prepares this slurry in a large number.Therefore, how to optimize this technology, seek out that a kind of to be convenient to the preparation method that automatic technology uses particularly important.
Summary of the invention
The technical problem that the present invention will solve is; To the complex steps of prior art, not easy to operate, equipment requirements is high, production cost is high, be unfavorable for the defective of scale of mass production, and the preparation method of the special-purpose silk screen printing slurry of a kind of DSSC is provided.
The technical solution adopted for the present invention to solve the technical problems is: construct the preparation method of the special-purpose silk screen printing slurry of a kind of DSSC, may further comprise the steps:
1) mixing and stirring titanium dioxide powder, ethanol and acetic acid obtain first mixed liquor;
2) mixing and stirring terpinol, ethanol and said first mixed liquor obtain the secondary mixed liquor;
3) mixing and stirring ethyl cellulose, ethanol and said secondary mixed liquor obtain the special-purpose silk screen printing slurry of DSSC.
In preparation method of the present invention, the ratio of the quality of titanium dioxide powder, ethanol and acetic acid described in the said step 1) is 0.8-1.2,0.4-0.6 and 0.16-0.24;
The ratio of the quality of terpinol said step 2), ethanol and first mixed liquor is 2.4-3.6: 2.4-3.6: 1.36-2.04;
The ratio of the quality of ethyl cellulose described in the said step 3), ethanol and secondary mixed liquor is 0.4-0.6: 1.2-1.8: 6.16-9.24.
In preparation method of the present invention, the ratio of the quality of titanium dioxide powder, ethanol and acetic acid described in the said step 1) is 1,0.5 and 0.2;
The ratio of the quality of terpinol said step 2), ethanol and first mixed liquor is 3: 3: 1.7;
The ratio of the quality of ethyl cellulose described in the said step 3), ethanol and secondary mixed liquor is 0.5: 1.5: 7.7.
In preparation method of the present invention, said step 1), step 2) and step 3) described in stir and be the ball milling that in planetary ball mill, carries out and stir.
In preparation method of the present invention, said step 1), step 2) and step 3) described in the rotating speed that stirs of ball milling be per minute 300-800 and change.
In preparation method of the present invention, said step 1), step 2) and step 3) described in ball milling time of stirring be respectively 10-300 minute, 60-1800 minute and 180-1500 minute.
In preparation method of the present invention, said step 1), step 2) and step 3) described in ball milling stir and all carry out at normal temperatures.
In preparation method of the present invention, said nano-titanium dioxide powder is one or more in the following substances: titania nanoparticles, titanium dioxide nano-rod, nano titania flower, titanium dioxide nano-belts, titanium dioxide nano thread, titania nanotube.
The preparation method of the special-purpose silk screen printing slurry of a kind of DSSC also is provided; It is characterized in that; May further comprise the steps: under the normal temperature, nano-titanium dioxide powder and the quality that with quality is 1 part is that the acetic acid that 0.5 part ethanol and quality is 0.2 part mixes, and places in the middle of the planetary ball mill; Regulating rotating speed is 300 to 800 rpms, stirs 10 to 300 minutes at ball milling; Add quality and be 3 parts terpinol and the ethanol that quality is 3 parts, continue ball milling stirring 60 to 1800 minutes; Add quality and be 0.5 part ethyl cellulose and the ethanol that quality is 1.5 parts, continue ball milling and stirred 180 to 1500 minutes, obtain DSSC special use silk screen printing slurry.
In preparation method of the present invention, said nano-titanium dioxide powder is one or more in the following substances: titania nanoparticles, titanium dioxide nano-rod, nano titania flower, titanium dioxide nano-belts, titanium dioxide nano thread, titania nanotube.
The preparation method of the special-purpose silk screen printing slurry of the described a kind of DSSC of embodiment of the present invention; Have following beneficial effect: the slurry that obtains according to this preparation method is evenly distributed; The repetition performance is good; Nano-crystalline titanium dioxide film microstructure by this pulp preparation does not have agglomeration, is easy to the absorption of light; Simultaneously, this preparation method has avoided the process of low-temperature reduced-pressure distillation, has saved some and has been used for the equipment of decompression distillation; Such as outstanding steaming equipment, vacuum equipment; Related instrument is cheap and easy to operate, and step is simply and not loaded down with trivial details, can prepare the special-purpose silk screen printing slurry of DSSC of high-quality within a short period of time through less instrument and equipment; Therefore be easy to amplify volume production, have industrialized advantage.
Description of drawings
To combine accompanying drawing and embodiment that the present invention is described further below, in the accompanying drawing:
Fig. 1 is preparation method's flow chart of the special-purpose silk screen printing slurry of DSSC of the present invention.
Embodiment
See also Fig. 1, be preparation method's flow chart of the special-purpose silk screen printing slurry of DSSC of the present invention.As shown in Figure 1, this preparation method may further comprise the steps:
The first step, the first mixed liquor of preparation intermediate product.Under the normal temperature, titanium dioxide powder, ethanol and acetic acid are uniformly mixed in planetary ball mill, obtain first mixed liquor.The ratio of the quality of titanium dioxide powder, ethanol and acetic acid is 0.8-1.2: 0.4-0.6: 0.16-0.24, and the ratio of preferred mass is 1: 0.5: 0.2.The rotating speed that ball milling stirs is per minute 300-800 to be changeed, and the duration is 10-300 minute.Above-mentioned nano-titanium dioxide powder can be that titania nanoparticles, titanium dioxide nano-rod, nano titania flower, titanium dioxide nano-belts, titanium dioxide nano thread, titania nanotube equidimension are nano level titanium dioxide.Can only select for use wherein a kind ofly in the preparation, also can select for use wherein multiple.
Second step, preparation intermediate product secondary mixed liquor.Under the normal temperature, the first mixed liquor that obtains in terpinol, ethanol and the first step is uniformly mixed in planetary ball mill, obtain the secondary mixed liquor.The ratio of the quality of terpinol, ethanol and first mixed liquor is 2.4-3.6: 2.4-3.6: 1.36-2.04, and the ratio of preferred mass is 3: 3: 1.7.The rotating speed that ball milling stirs is per minute 300-800 to be changeed, and the duration is 60-1800 minute.
The 3rd step, the special-purpose silk screen printing slurry of preparation end product DSSC.Under the normal temperature, the secondary mixed liquor that ethyl cellulose, ethanol and second are obtained in going on foot uniformly mixes in planetary ball mill, obtains the special-purpose silk screen printing slurry of DSSC.The ratio of the quality of ethyl cellulose, ethanol and secondary mixed liquor is 0.4-0.6: 1.2-1.8: 6.16-9.24, and the ratio of preferred mass is 0.5: 1.5: 7.7.The rotating speed that ball milling stirs is per minute 300-800 to be changeed, and the duration is 180-1500 minute.
Stirring among the above-mentioned preparation method also can adopt other blenders to carry out alr mode, such as: turbine agitator, axial flow type stirrer.Because planetary ball mill is to obtain the very desirable equipment of nano-grade matter, so the preferred alr mode of the present invention stirs for the ball milling that in planetary ball mill, carries out.
To introduce the specific embodiment among the present invention in detail below.
Embodiment 1
The 1g nano-titanium dioxide powder is mixed with the ethanol of 0.5g and the acetic acid of 0.2g mutually; Being positioned in the middle of the planetary ball mill, is 500 rpms with rotational speed regulation, grinds after 20 minutes; The adding quality is that terpinol and the quality of 3g is the ethanol of 3g, continues to grind 60 minutes.Adding ethyl cellulose and the quality that quality is 0.5g at last is the ethanol of 1.5g, continues to grind 360 minutes, can obtain to can be applicable in a small amount the special-purpose silk screen printing titania slurry of breadboard DSSC.
Embodiment 2
The 1000g nano-titanium dioxide powder is mixed with the ethanol of 500g and the acetic acid of 500g mutually; Being positioned in the middle of the planetary ball mill, is 800 rpms with rotational speed regulation, grinds after 300 minutes; The adding quality is that terpinol and the quality of 3000g is the ethanol of 3000g, continues to grind 1800 minutes.Adding quality at last and be 500 ethyl cellulose and quality is the ethanol of 1500g, grinds 1500 minutes, can obtain to can be applicable in a large number the DSSC silk private network printing titania slurry of pilot scale.
Embodiment 3
The 1.2g nano-titanium dioxide powder is mixed with the ethanol of 0.4g and the acetic acid of 0.24g mutually; Being positioned in the middle of the planetary ball mill, is 400 rpms with rotational speed regulation, grinds after 60 minutes; The adding quality is that terpinol and the quality of 3.6g is the ethanol of 2.4g, continues to grind 240 minutes.Adding ethyl cellulose and the quality that quality is 0.6g at last is the ethanol of 1.2g, continues to grind 180 minutes, can obtain to can be applicable in a small amount the special-purpose silk screen printing titania slurry of breadboard DSSC.
Embodiment 4
The 0.8g nano-titanium dioxide powder is mixed with the ethanol of 0.6g and the acetic acid of 0.16g mutually; Being positioned in the middle of the planetary ball mill, is 300 rpms with rotational speed regulation, grinds after 10 minutes; The adding quality is that terpinol and the quality of 2.4g is the ethanol of 3.6g, continues to grind 100 minutes.Adding ethyl cellulose and the quality that quality is 0.4g at last is the ethanol of 1.8g, continues to grind 400 minutes, can obtain to can be applicable in a small amount the special-purpose silk screen printing titania slurry of breadboard DSSC.
The ratio of the foregoing description 1 and the preferred mass of embodiment 2 employing raw materials; The special-purpose silk screen printing titania slurry of prepared DSSC is more excellent; Slurry is evenly distributed; The repetition performance is good, does not have agglomeration by the nano-crystalline titanium dioxide film microstructure of this pulp preparation, is easy to the absorption of light.The ratio of embodiment 3 and embodiment 4 other feasible quality of employing raw material, the special-purpose silk screen printing titania slurry of prepared DSSC also is available.
The above is merely embodiments of the invention; Be not so limit claim of the present invention; Every equivalent structure transformation that utilizes specification of the present invention and accompanying drawing content to be done, or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present invention.

Claims (9)

1. the preparation method of the special-purpose silk screen printing slurry of DSSC is characterized in that, may further comprise the steps:
1) mixing and stirring titanium dioxide powder, ethanol and acetic acid obtain first mixed liquor, and the ratio of the quality of said titanium dioxide powder, ethanol and acetic acid is 0.8-1.2:0.4-0.6:0.16-0.24;
2) mixing and stirring terpinol, ethanol and said first mixed liquor obtain the secondary mixed liquor, and the ratio of the quality of said terpinol, ethanol and first mixed liquor is 2.4-3.6:2.4-3.6:1.36-2.04;
3) mixing and stirring ethyl cellulose, ethanol and said secondary mixed liquor obtain the special-purpose silk screen printing slurry of DSSC, and the ratio of the quality of said ethyl cellulose, ethanol and secondary mixed liquor is 0.4-0.6:1.2-1.8:6.16-9.24;
Said step 1), step 2) and step 3) all carry out at normal temperatures.
2. preparation method according to claim 1 is characterized in that, the ratio of the quality of titanium dioxide powder, ethanol and acetic acid described in the said step 1) is 1:0.5:0.2;
The ratio of the quality of terpinol said step 2), ethanol and first mixed liquor is 3:3:1.7;
The ratio of the quality of ethyl cellulose described in the said step 3), ethanol and secondary mixed liquor is 0.5:1.5:7.7.
3. according to any described preparation method among the claim 1-2, it is characterized in that said step 1), step 2) and step 3) described in stir and to be the ball milling that in planetary ball mill, carries out and to stir.
4. preparation method according to claim 3 is characterized in that, said step 1), step 2) and step 3) described in the rotating speed that stirs of ball milling be per minute 300-800 and change.
5. preparation method according to claim 3 is characterized in that, said step 1), step 2) and step 3) described in ball milling time of stirring be respectively 10-300 minute, 60-1800 minute and 180-1500 minute.
6. preparation method according to claim 4 is characterized in that, said step 1), step 2) and step 3) described in ball milling stir and all to carry out at normal temperatures.
7. preparation method according to claim 1; It is characterized in that said nano-titanium dioxide powder is one or more in the following substances: titania nanoparticles, titanium dioxide nano-rod, nano titania flower, titanium dioxide nano-belts, titanium dioxide nano thread, titania nanotube.
8. the preparation method of the special-purpose silk screen printing slurry of a DSSC; It is characterized in that; May further comprise the steps: under the normal temperature, nano-titanium dioxide powder and the quality that with quality is 1 part is that the acetic acid that 0.5 part ethanol and quality is 0.2 part mixes, and places in the middle of the planetary ball mill; Regulating rotating speed is 300 to 800 rpms, stirs 10 to 300 minutes at ball milling; Add quality and be 3 parts terpinol and the ethanol that quality is 3 parts, continue ball milling stirring 60 to 1800 minutes; Add quality and be 0.5 part ethyl cellulose and the ethanol that quality is 1.5 parts, continue ball milling and stirred 180 to 1500 minutes, obtain DSSC special use silk screen printing slurry.
9. preparation method according to claim 8; It is characterized in that said nano-titanium dioxide powder is one or more in the following substances: titania nanoparticles, titanium dioxide nano-rod, nano titania flower, titanium dioxide nano-belts, titanium dioxide nano thread, titania nanotube.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102881458A (en) * 2012-09-25 2013-01-16 南京工业大学 Preparation method for graphene and titanium dioxide composite sizing material

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Publication number Priority date Publication date Assignee Title
CN101174657A (en) * 2007-11-28 2008-05-07 中国科学院上海硅酸盐研究所 Production method for titanium oxide coating material in dye sensitized solar battery
CN101699588A (en) * 2009-10-30 2010-04-28 彩虹集团公司 Method for preparing titanium dioxide slurry for dye-sensitized solar cell
CN101783245A (en) * 2009-12-21 2010-07-21 新奥科技发展有限公司 Titanium dioxide film with macroporous structure and preparation method thereof

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Publication number Priority date Publication date Assignee Title
US8933328B2 (en) * 2006-07-06 2015-01-13 Sharp Kabushiki Kaisha Dye-sensitized solar cell module and method of producing the same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101174657A (en) * 2007-11-28 2008-05-07 中国科学院上海硅酸盐研究所 Production method for titanium oxide coating material in dye sensitized solar battery
CN101699588A (en) * 2009-10-30 2010-04-28 彩虹集团公司 Method for preparing titanium dioxide slurry for dye-sensitized solar cell
CN101783245A (en) * 2009-12-21 2010-07-21 新奥科技发展有限公司 Titanium dioxide film with macroporous structure and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102881458A (en) * 2012-09-25 2013-01-16 南京工业大学 Preparation method for graphene and titanium dioxide composite sizing material
CN102881458B (en) * 2012-09-25 2016-01-20 南京工业大学 A kind of preparation method of Graphene composite titanium dioxide slurry

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