CN103021666A - Method for preparing compound titanium dioxide film - Google Patents
Method for preparing compound titanium dioxide film Download PDFInfo
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- CN103021666A CN103021666A CN2012105133316A CN201210513331A CN103021666A CN 103021666 A CN103021666 A CN 103021666A CN 2012105133316 A CN2012105133316 A CN 2012105133316A CN 201210513331 A CN201210513331 A CN 201210513331A CN 103021666 A CN103021666 A CN 103021666A
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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
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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
- 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 invention provides a method for preparing a compound titanium dioxide film. The method includes firstly, placing mesophase carbon microbeads into hydrogen peroxide for ultrasound processing to obtain preprocessed mesophase carbon microbeads; then dissolving butyl titanate in absolute ethyl alcohol, and adding acetylacetone to prepare a solution A; dropping a mixed solution of nitric acid, deionized water and absolute ethyl alcohol in the solution A under mechanical stirring to prepare a titanium dioxide sol precursor solution; and adding the preprocessed mesophase carbon microbeads to the titanium dioxide sol precursor solution to form a titanium dioxide sol solution, preparing a titanium dioxide sol film by using a pulling method, and subjecting the titanium dioxide sol film to drying and sintering to obtain the compound titanium dioxide film. By means of the prepared compound titanium dioxide film, conduction efficiencies of electrons in the film are improved, transmission resistance of the titanium dioxide film is reduced, short-circuit current is improved, and photoelectric conversion efficiencies of a dye-sensitized solar cell are increased.
Description
Technical field
The present invention relates to a kind of preparation method's of titanium deoxid film, particularly a kind of composite titanium dioxide thin film preparation method.
Background technology
Solar energy is a kind of cleaning, the efficiently and never depleted energy, and research and utilization solar energy is the most real concerning the mankind.1991, Lausanne, SUI engineering college
Nano-crystalline solar battery (DyeSensitized Solar Cell, be called for short DSSC) is with lower cost, for the utilization of solar energy provides a new approach.This battery only has 1/10 of traditional silicon solar cell with its its cost, and manufacture craft is simple, and nontoxic free of contamination characteristics are subject to extensive concern.
The electricity conversion of DSSC is mainly determined by the conduction efficiency of capture rate, transformation efficiency and the electronics of incident light.Titanium deoxid film plays decisive role in the photoelectron conduction, be the key that improves the cell photoelectric conversion efficiency so prepare high performance carbon dioxide film.Yet the titanium deoxid film electronics causes electrical conductivity efficient low larger to the conduction resistance of conductive substrates direction, thereby has limited the electricity conversion of DSSC.
Summary of the invention
The invention provides a kind of preparation method of composite titanium dioxide thin film of simple and effective raising DSSC electricity conversion.
In order to achieve the above object, the technical solution used in the present invention is:
1) gets carbonaceous mesophase spherules and put into hydrogen peroxide, then 40-45 ℃ of ultrasonic processing, again the carbonaceous mesophase spherules filtration washing is obtained pretreated carbonaceous mesophase spherules;
2) butyl titanate is dissolved in the absolute ethyl alcohol, adds again acetylacetone,2,4-pentanedione, wiring solution-forming A; Then under mechanical agitation, the mixed solution of nitric acid, deionized water and absolute ethyl alcohol is splashed in the solution A, be made into the TiO 2 sol precursor liquid; Wherein, the mol ratio of butyl titanate, absolute ethyl alcohol, deionized water, nitric acid and acetylacetone,2,4-pentanedione is (0.8-1.5) in the TiO 2 sol precursor liquid: 18:2:(0.1-0.4): (0.3-0.5);
3) the pretreated carbonaceous mesophase spherules with TiO 2 sol precursor liquid quality 5%-15% joins in the TiO 2 sol precursor liquid, obtains TiO 2 sol solution;
4) substrate with cleaning immerses in the TiO 2 sol solution, adopts czochralski method to prepare the TiO 2 sol film, then with the oven dry under 80 ℃-100 ℃ of TiO 2 sol film, again at 450 ℃ of-500 ℃ of lower sintering, obtains composite titanium dioxide thin film.
Described carbonaceous mesophase spherules particle diameter is at 1 μ m-20 μ m.
The ultrasonic processing of described step 1) carbonaceous mesophase spherules 12-24 hour.
Described concentration of nitric acid is 50%-70%.
Described step 2) the absolute ethyl alcohol volume that is used for the dissolving butyl titanate in is 2/3 of TiO 2 sol precursor liquid absolute ethyl alcohol cumulative volume.
The pull rate of described czochralski method is 1.5-2mm/s.
The substrate of described cleaning is obtained by ultrasonic processing.
Described step 4) sintering time is 2-4 hour.
Compared with prior art, beneficial effect of the present invention is:
The present invention prepares titanium deoxid film by improving sol-gal process, adds carbonaceous mesophase spherules to TiO 2 sol solution, the preparation composite titanium dioxide thin film.The present invention processes carbonaceous mesophase spherules with hydrogen peroxide after, it is coarse that the surface of carbonaceous mesophase spherules can become, the surface of carbosphere can connect hydroxyl isoreactivity group, titania molecule can fully contact with carbonaceous mesophase spherules in the titanium dioxide precursor liquid thereby make, the dispersive property of carbonaceous mesophase spherules can improve, and the specific area of carbonaceous mesophase spherules is increased.Because carbonaceous mesophase spherules can obviously improve the electric conductivity of film; So, just can improve electronics conduction efficiency in film when adding the middle phase microballoon of being processed by hydrogen peroxide in the TiO 2 sol, reduce the transport resistance of titanium deoxid film, thereby reach the raising short circuit current, and then increase the purpose of DSSC electricity conversion.
Description of drawings
Fig. 1 is the I-V resolution chart of the battery of battery of the present invention and the titanium deoxid film that does not add carbonaceous mesophase spherules; Wherein, the cell I-V resolution chart of 1-composite titanium dioxide thin film preparation of the present invention, the titanium deoxid film that 2-does not enter carbonaceous mesophase spherules prepares the cell I-V resolution chart.
Embodiment
Embodiment 1:
1) get particle diameter and put into hydrogen peroxide at 1 μ m-20 μ m carbonaceous mesophase spherules, then 45 ℃ of lower ultrasonic processing 24 hours, then filtration washing obtained pretreated carbonaceous mesophase spherules;
2) butyl titanate is dissolved in the absolute ethyl alcohol, adds again acetylacetone,2,4-pentanedione, wiring solution-forming A; Then the mixed solution that with mass concentration is 50% nitric acid, deionized water and absolute ethyl alcohol under mechanical agitation splashes in the solution A, is made into the TiO 2 sol precursor liquid; Wherein, the mol ratio of butyl titanate, absolute ethyl alcohol, deionized water, nitric acid and acetylacetone,2,4-pentanedione is 1:18:2:0.2:0.5 in the TiO 2 sol precursor liquid, and the absolute ethyl alcohol volume that is used for the dissolving butyl titanate is 2/3 of TiO 2 sol precursor liquid absolute ethyl alcohol cumulative volume;
3) carbonaceous mesophase spherules with the processing of TiO 2 sol precursor liquid quality 5% joins in the TiO 2 sol precursor liquid, obtains TiO 2 sol solution;
4) the clean substrate that ultrasonic cleaning is obtained immerses in the TiO 2 sol solution, adopt czochralski method to prepare the TiO 2 sol film with the pull rate of 1.5-2mm/s, then 80 ℃ of lower oven dry 2 hours, 450 ℃ of lower sintering processes 4 hours, obtain composite titanium dioxide thin film again.
Embodiment 2:
1) get particle diameter and put into hydrogen peroxide at 1 μ m-20 μ m carbonaceous mesophase spherules, during ultrasonic processing 12, then filtration washing obtains pretreated carbonaceous mesophase spherules under 42 ℃ of conditions;
2) butyl titanate is dissolved in the absolute ethyl alcohol, adds again acetylacetone,2,4-pentanedione, wiring solution-forming A; Then the mixed solution that with mass concentration is 65% nitric acid, deionized water and absolute ethyl alcohol under mechanical agitation splashes in the solution A, is made into the TiO 2 sol precursor liquid; Wherein, the mol ratio of butyl titanate, absolute ethyl alcohol, deionized water, nitric acid and acetylacetone,2,4-pentanedione is 0.8:18:2:0.4:0.3 in the TiO 2 sol precursor liquid, and the absolute ethyl alcohol volume that is used for the dissolving butyl titanate is 2/3 of TiO 2 sol precursor liquid absolute ethyl alcohol cumulative volume;
3) the pretreated carbonaceous mesophase spherules with TiO 2 sol precursor liquid quality 10% joins in the TiO 2 sol precursor liquid, obtains TiO 2 sol solution;
4) the clean substrate that ultrasonic cleaning is obtained immerses in the TiO 2 sol solution, adopt czochralski method to prepare the TiO 2 sol film with the pull rate of 1.5-2mm/s, then 90 ℃ of lower oven dry 1 hour, 480 ℃ of lower sintering processes 3 hours, obtain composite titanium dioxide thin film again.
Embodiment 3:
1) get particle diameter and put into hydrogen peroxide at 1 μ m-20 μ m carbonaceous mesophase spherules, ultrasonic processing is 20 hours under 40 ℃ of conditions, and then filtration washing obtains pretreated carbonaceous mesophase spherules;
2) butyl titanate is dissolved in the absolute ethyl alcohol, adds again acetylacetone,2,4-pentanedione, wiring solution-forming A; Then the mixed solution that with mass concentration is 70% nitric acid, deionized water and absolute ethyl alcohol under mechanical agitation splashes in the solution A, is made into the TiO 2 sol precursor liquid; Wherein, the mol ratio of butyl titanate, absolute ethyl alcohol, deionized water, nitric acid and acetylacetone,2,4-pentanedione is 1.5:18:2:0.1:0.4 in the TiO 2 sol precursor liquid, and the absolute ethyl alcohol volume that is used for the dissolving butyl titanate is 2/3 of TiO 2 sol precursor liquid absolute ethyl alcohol cumulative volume;
3) the pretreated carbonaceous mesophase spherules with TiO 2 sol precursor liquid quality 15% joins in the TiO 2 sol precursor liquid, obtains TiO 2 sol solution;
4) the clean substrate that ultrasonic cleaning is obtained immerses in the TiO 2 sol solution, adopt czochralski method to prepare the TiO 2 sol film with the pull rate of 1.5-2mm/s, then 100 ℃ of lower oven dry 0.5 hour, 500 ℃ of lower sintering processes 2 hours, obtain composite titanium dioxide thin film again.
Embodiment 4:
1) get particle diameter and put into hydrogen peroxide at 1 μ m-20 μ m carbonaceous mesophase spherules, ultrasonic processing is 24 hours under 45 ℃ of conditions, and then filtration washing obtains pretreated carbonaceous mesophase spherules;
2) butyl titanate is dissolved in the absolute ethyl alcohol, adds again acetylacetone,2,4-pentanedione, wiring solution-forming A; Then the mixed solution that with mass concentration is 60% nitric acid, deionized water and absolute ethyl alcohol under mechanical agitation splashes in the solution A, is made into the TiO 2 sol precursor liquid; Wherein, the mol ratio of butyl titanate, absolute ethyl alcohol, deionized water, nitric acid and acetylacetone,2,4-pentanedione is 1:18:2:0.2:0.5 in the TiO 2 sol precursor liquid, and the absolute ethyl alcohol volume that is used for the dissolving butyl titanate is 2/3 of TiO 2 sol precursor liquid absolute ethyl alcohol cumulative volume;
3) the pretreated carbonaceous mesophase spherules with TiO 2 sol precursor liquid quality 8% joins in the TiO 2 sol precursor liquid, obtains TiO 2 sol solution;
4) the clean substrate that ultrasonic cleaning is obtained immerses in the TiO 2 sol solution, adopt czochralski method to prepare the TiO 2 sol film with the pull rate of 1.5-2mm/s, then 90 ℃ of lower oven dry 0.5 hour, 470 ℃ of lower sintering processes 4 hours, obtain composite titanium dioxide thin film again.
Embodiment 5:
1) get particle diameter and put into hydrogen peroxide at 1 μ m-20 μ m carbonaceous mesophase spherules, ultrasonic processing is 12 hours under 45 ℃ of conditions, and then filtration washing obtains pretreated carbonaceous mesophase spherules;
2) butyl titanate is dissolved in the absolute ethyl alcohol, adds again acetylacetone,2,4-pentanedione, wiring solution-forming A; Then the mixed solution that with mass concentration is 70% nitric acid, deionized water and absolute ethyl alcohol under mechanical agitation splashes in the solution A, is made into the TiO 2 sol precursor liquid; Wherein, the mol ratio of butyl titanate, absolute ethyl alcohol, deionized water, nitric acid and acetylacetone,2,4-pentanedione is 1:18:2:0.2:0.5 in the TiO 2 sol precursor liquid, and the absolute ethyl alcohol volume that is used for the dissolving butyl titanate is 2/3 of TiO 2 sol precursor liquid absolute ethyl alcohol cumulative volume;
3) the pretreated carbonaceous mesophase spherules with TiO 2 sol precursor liquid quality 15% joins in the TiO 2 sol precursor liquid, obtains TiO 2 sol solution;
4) the clean substrate that ultrasonic cleaning is obtained immerses in the TiO 2 sol solution, adopt czochralski method to prepare the TiO 2 sol film with the pull rate of 1.5-2mm/s, then 100 ℃ of lower oven dry 0.5 hour, 500 ℃ of lower sintering processes 2 hours, obtain composite titanium dioxide thin film again.
As seen from Figure 1, the current density ratio of the battery of the composite titanium dioxide thin film of the present invention preparation titanium deoxid film that the do not enter carbonaceous mesophase spherules current density for preparing battery obviously improves.Owing to added carbonaceous mesophase spherules in the composite titanium dioxide thin film of the present invention, can improve current density; So composite titanium dioxide thin film of the present invention can improve electronics conduction efficiency in film, reduce the transport resistance of titanium deoxid film, thereby reach the raising short circuit current, and then increase the purpose of DSSC electricity conversion.
Claims (8)
1. the preparation method of a composite titanium dioxide thin film is characterized in that:
1) gets carbonaceous mesophase spherules and put into hydrogen peroxide, then 40-45 ℃ of ultrasonic processing, again the carbonaceous mesophase spherules filtration washing is obtained pretreated carbonaceous mesophase spherules;
2) butyl titanate is dissolved in the absolute ethyl alcohol, adds again acetylacetone,2,4-pentanedione, wiring solution-forming A; Then under mechanical agitation, the mixed solution of nitric acid, deionized water and absolute ethyl alcohol is splashed in the solution A, be made into the TiO 2 sol precursor liquid; Wherein, the mol ratio of butyl titanate, absolute ethyl alcohol, deionized water, nitric acid and acetylacetone,2,4-pentanedione is (0.8-1.5) in the TiO 2 sol precursor liquid: 18:2:(0.1-0.4): (0.3-0.5);
3) the pretreated carbonaceous mesophase spherules with TiO 2 sol precursor liquid quality 5%-15% joins in the TiO 2 sol precursor liquid, obtains TiO 2 sol solution;
4) substrate with cleaning immerses in the TiO 2 sol solution, adopts czochralski method to prepare the TiO 2 sol film, then with the oven dry under 80 ℃-100 ℃ of TiO 2 sol film, again at 450 ℃ of-500 ℃ of lower sintering, obtains composite titanium dioxide thin film.
2. require the preparation method of 1 described composite titanium dioxide thin film according to patent, it is characterized in that: described carbonaceous mesophase spherules particle diameter is at 1 μ m-20 μ m.
3. the preparation method of composite titanium dioxide thin film according to claim 1 and 2 is characterized in that: the ultrasonic processing of described step 1) carbonaceous mesophase spherules 12-24 hour.
4. require the preparation method of 1 described composite titanium dioxide thin film according to patent, it is characterized in that: described concentration of nitric acid is 50%-70%.
5. require the preparation method of 1 or 4 described composite titanium dioxide thin films according to patent, it is characterized in that: the absolute ethyl alcohol volume that is used for the dissolving butyl titanate described step 2) is 2/3 of TiO 2 sol precursor liquid absolute ethyl alcohol cumulative volume.
6. require 1 described composite titanium dioxide thin film and preparation method thereof according to patent, it is characterized in that: the pull rate of described czochralski method is 1.5-2mm/s.
7. require 1 described composite titanium dioxide thin film and preparation method thereof according to patent, it is characterized in that: the substrate of described cleaning is obtained by ultrasonic processing.
8. require 1 described composite titanium dioxide thin film and preparation method thereof according to patent, it is characterized in that: described step 4) sintering time is 2-4 hour.
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Cited By (7)
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| CN103295795A (en) * | 2013-05-24 | 2013-09-11 | 东莞上海大学纳米技术研究院 | Method for improving photoelectric property of dye-sensitized solar cells by coadsorbent |
| CN103601273A (en) * | 2013-11-13 | 2014-02-26 | 清华大学 | Nano titanium dioxide modification method of electric adsorption desalinization carbon electrode |
| CN105047860A (en) * | 2014-12-19 | 2015-11-11 | 上海杉杉科技有限公司 | Battery cathode TiO2/intermediate-phase microsphere composite material and preparation method thereof |
| CN108411309A (en) * | 2018-03-28 | 2018-08-17 | 中国石油大学(北京) | A kind of preparation method of iron oxide composite titanium dioxide thin film light anode for photoproduction cathodic protection |
| CN113896236A (en) * | 2021-09-13 | 2022-01-07 | 常州市妇幼保健院 | Titanium dioxide synthesis method based on glutamine modification |
| CN114133600A (en) * | 2021-11-22 | 2022-03-04 | 广西大学 | Method for preparing high-molecular magnetic composite film of friction nano generator |
| CN115090264A (en) * | 2022-07-26 | 2022-09-23 | 中国矿业大学 | Super-hydrophobic/super-oleophylic adsorbent prepared from coal gasification slag as raw material and preparation method and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103295795A (en) * | 2013-05-24 | 2013-09-11 | 东莞上海大学纳米技术研究院 | Method for improving photoelectric property of dye-sensitized solar cells by coadsorbent |
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| CN103601273B (en) * | 2013-11-13 | 2015-01-14 | 清华大学 | Nano titanium dioxide modification method of electric adsorption desalinization carbon electrode |
| CN105047860A (en) * | 2014-12-19 | 2015-11-11 | 上海杉杉科技有限公司 | Battery cathode TiO2/intermediate-phase microsphere composite material and preparation method thereof |
| CN108411309A (en) * | 2018-03-28 | 2018-08-17 | 中国石油大学(北京) | A kind of preparation method of iron oxide composite titanium dioxide thin film light anode for photoproduction cathodic protection |
| CN113896236A (en) * | 2021-09-13 | 2022-01-07 | 常州市妇幼保健院 | Titanium dioxide synthesis method based on glutamine modification |
| CN114133600A (en) * | 2021-11-22 | 2022-03-04 | 广西大学 | Method for preparing high-molecular magnetic composite film of friction nano generator |
| CN114133600B (en) * | 2021-11-22 | 2023-09-05 | 广西大学 | Method for preparing high-molecular magnetic composite film of friction nano generator |
| CN115090264A (en) * | 2022-07-26 | 2022-09-23 | 中国矿业大学 | Super-hydrophobic/super-oleophylic adsorbent prepared from coal gasification slag as raw material and preparation method and application thereof |
| CN115090264B (en) * | 2022-07-26 | 2023-10-20 | 中国矿业大学 | Super-hydrophobic/super-oleophylic adsorbent prepared from coal gas slag as raw material, and preparation method and application thereof |
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Application publication date: 20130403 |