CN105632772A - Preparation method for titanium dioxide photoanode of titanium-based flexible dye-sensitized solar cell - Google Patents
Preparation method for titanium dioxide photoanode of titanium-based flexible dye-sensitized solar cell Download PDFInfo
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- CN105632772A CN105632772A CN201610153498.4A CN201610153498A CN105632772A CN 105632772 A CN105632772 A CN 105632772A CN 201610153498 A CN201610153498 A CN 201610153498A CN 105632772 A CN105632772 A CN 105632772A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
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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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Abstract
The invention relates to a preparation method for a titanium dioxide photoanode of a titanium-based flexible dye-sensitized solar cell. The preparation method comprises the following steps of dispersing titanium dioxide in a binding agent, and carrying out ball milling to obtain a titanium dioxide paste; coating the surface of an aluminum foil with the titanium dioxide paste in a room temperature condition, and allowing the aluminum foil to stand to obtain a titanium foil photoanode substrate; rolling the titanium foil photoanode substrate by a roller-to-roller method in a die releasing agent condition; and carrying out thermal treatment, washing, drying, calcination and cooling to obtain the titanium dioxide photoanode. The preparation method can be used for a flexible titanium foil substrate, is simple, is low in production device requirement and is easy for industrial production at a large scale; moreover, the flexible thin film which is compacted by a roller-to-roller process and of which the surface is smoothened has the characteristics of light, high compactness, high porosity and the like, can be bent substantially, and is difficult to crack, and thus, the battery quality can be improved.
Description
Technical field
The invention belongs to the preparation field of solar battery light anode, in particular to the preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode.
Background technology
Dye sensitization solar battery cost of manufacture is cheap, technique is simple, nontoxic, pollute little, therefore thought the substitute of silicon solar cell by industry. The core of such battery is semi-conducting electrode, and this type of semi-conducting electrode many employings titanium deoxid film forms. 1991, Switzerland scientist M.Having delivered the work about dye sensitization solar battery for the first time, it adopts titanium oxide colloid to prepare porous titanium dioxide thin-film at FTO glass basic surface, by 450 DEG C of calcinings, is applied to dye sensitization solar battery, and its photoelectric transformation efficiency is 7.12%. At present to the preparation technology of such electrode, add organic binder bond after mostly being synthesis of nano titanium dioxide granule and it is prepared into titania slurry, in substrate, titanium deoxid film is prepared to scrape the techniques such as painting or silk screen printing, organics removal is calcined, to form the titanium deoxid film of porous with 450��500 DEG C.
Thickness is that the titanium paper tinsel of 0.2mm is as flexible base board by group, the method of silk screen printing is adopted to prepare titanium deoxid film, under 500 DEG C of high temperature, sintering obtains light anode, electrode is adopted the flexible ITO-PEN film of platinum plating, finally make Grazing condition solar cell, sunlight is injected to electrode direction, and photoelectric transformation efficiency reaches 7.2%. Be compared to the present invention, the method for silk screen printing can not big area continuous print suitability for industrialized production, therefore product rate is lower.
Summary of the invention
Technical problem to be solved by this invention is to provide the preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode, and the preparation method of the present invention is simple and reliable, easy to maintenance, running cost is lower, is easy to big area, suitability for industrialized production; And obtained flexible dye sensitized solar energy cell photoanode film has and can significantly bend, not easily breaking, light weight is even, the features such as compactness is good, porosity height; Photo-anode film makes the network between particle with particle be connected closely after high-temperature calcination, is conducive to electric transmission, thus improves the photoelectric transformation efficiency of dye sensitization solar battery, promotes the quality of dye sensitization solar battery.
The preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode of the present invention, comprising:
(1) being disperseed in a binder by titanium dioxide, ball milling, rotary evaporation, obtains titania slurry;
(2) under room temperature condition, above-mentioned titania slurry is coated on aluminium foil surface, leaves standstill, obtain the titanium paper tinsel light anode substrate of surface irregularity;
(3) when releasing agent, adopt roll-to-roll method that the titanium paper tinsel light anode substrate of step (2) is carried out roll-in compacting pressing, obtain the titanium paper tinsel light anode substrate of smooth surface, then substrate heat-treat, wash, dry, calcining, cooling, obtain titanium base flexible dye-sensitized solar battery titanium dioxide photo anode.
In described step (1), titanium dioxide dispersion is specially in a binder: add ethanol, binding agent, ethyl cellulose dispersion in titanium dioxide respectively; Wherein each composition accounts for the weight ratio of gross weight: titanium dioxide to be 2.9-3.8wt%, ethanol be 79.7-80.3wt%, binding agent are 14.4-14.6wt%, ethyl cellulose is 2.1-2.2wt%.
In described step (1), binding agent is Terpineol 350; The mass percentage concentration of titania slurry is 15-18wt%.
In described step (1), the ball milling time is 24-48h, and ball milling speed is 20-30 rev/min.
In described step (2), time of repose is 5-10min.
In described step (3), titanium paper tinsel light anode substrate is carried out roll-in and is specially by roll-to-roll method: titanium paper tinsel light anode substrate is positioned over roll-in in roll-to-roll equipment, and roller wheel linear velocity is 10-15cm/s, and roller wheel spacing is 0.3-0.5mm.
In described step (3), releasing agent is Terpineol 350.
In described step (3), thermal treatment temp is 100-130 DEG C, and the time is 10-30min.
In described step (3), washing is deionized water, and washing times is 3-5 time.
In described step (3), calcining temperature is 450-500 DEG C, and calcination time is 30-50min.
In step (3), in titanium base flexible dye-sensitized solar battery titanium dioxide photo anode, titanium dioxide film thickness is 15-20 micron.
Fig. 1 comprises flexible parent metal 1 for this present invention flexible dye-sensitized solar battery, to electrode 2, the conductor oxidate 3 being laminated in flexible parent metal 1 top, is coated on the dyestuff (not shown) on conductor oxidate 3 surface and is filled in above-mentioned flexible parent metal 1 and to the ionogen 4 between electrode 2.
The present invention is as substrate using tinsel, the substrate of glass thick and heavy with rigidity compares, flexible base board not only decreases the weight of battery to a great extent, also make battery cost of manufacture be declined to a great extent simultaneously, and because of its flexural deformation and portable performance good so that the use range of flexible substrates dye sensitization solar battery has greatly been expanded. Owing to flexible metal base plate can be high temperature resistant, the crystal property of the oxide nanocrystalline film therefore obtained is better. In addition, conductive plastics substrate of comparing, metal base also has the advantages such as cheap, conductivity is good.
The present invention adopts roll-to-roll technique to have the series of advantages such as simple and reliable, easy to maintenance, running cost is lower, spacing size can regulate, and production unit is required low by this method, is easy to big area, suitability for industrialized production; And the fexible film that the present invention obtains has and can significantly bend, not easily breaking, light weight, the features such as compactness is good, porosity height, thus can improve the quality of battery.
Useful effect
(1) preparation method of the present invention is simple and reliable, easy to maintenance, running cost is lower, is easy to big area, suitability for industrialized production;
(2) the flexible dye sensitized solar energy cell photoanode film that the present invention obtains has and can significantly bend, and not easily breaks, and light weight is even, the features such as compactness is good, porosity height;
(3) photo-anode film of the present invention makes the network between particle with particle be connected closely after high-temperature calcination, is conducive to electric transmission, thus improves the photoelectric transformation efficiency of dye sensitization solar battery, promotes the quality of dye sensitization solar battery.
Accompanying drawing explanation
Fig. 1: the structural representation of flexible dye-sensitized solar battery prepared by roll-to-roll technique; Wherein 1 flexible parent metal, 2 is to electrode, 3 conductor oxidates, 4 ionogen;
Fig. 2: roll-to-roll technique prepares the equipment schematic diagram of titanium dioxide photo anode;
Fig. 3: the current density voltage curve schematic diagram of material prepared by embodiment 1;
Fig. 4: the three-D profile figure of titanium dioxide photo anode prepared by embodiment 2;
Fig. 5: the titanium dioxide photo anode film thickness measuring figure that embodiment 3 obtains;
Fig. 6: the titanium dioxide photo anode electron scanning micrograph of embodiment 4.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further. Limit the scope of the invention it will be understood that these embodiments are only not used in for illustration of the present invention. In addition it will be understood that after having read the content that the present invention lectures, the present invention can be made various changes or modifications by those skilled in the art, and these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
4.0 grams of titanium dioxide are taken under room temperature, add ethanol 100mL, Terpineol 350 20 grams and massfraction are the ethyl cellulose (3 grams: 30 grams of ethanol) of 10wt%, ball-milling processing 24 hours, ball milling speed is 30 revs/min, forming finely dispersed solution, last rotary evaporation obtains the titania slurry that massfraction is about 15wt%. The titanium paper tinsel surface of washes clean will be coated under above-mentioned titania slurry room temperature, leave standstill 10min. Above-mentioned titanium paper tinsel substrate is positioned over roll-in in the roll-to-roll equipment applying Terpineol 350 (releasing agent), roller wheel spacing 0.3mm, roller wheel linear velocity 15cm/s; And in thermal station 100 DEG C of heat treated, 30 minutes time length. Drying after substrate being washed three times with deionized water after being cooled to room temperature. Dried substrate is placed in retort furnace 500 DEG C calcining 30 minutes. The efficiency of battery is dressed up, by this application of electrode in dye sensitization solar battery: be soaked in 0.5mMN719 dyestuff 24 hours by above-mentioned sample when it is cooled to 80 DEG C for testing this light anode unit. As shown in Figure 3, open circuit voltage is 0.99V, and current density is 16.98mA/cm2, packing factor is 0.64, and photoelectric transformation efficiency is 10.70%.
Embodiment 2
5.0 grams of titanium dioxide are taken under room temperature, add ethanol 100mL, Terpineol 350 20 grams and massfraction are the ethyl cellulose (3 grams: 30 grams of ethanol) of 10wt%, ball-milling processing 24 hours, ball milling speed is 30 revs/min, forming finely dispersed solution, last rotary evaporation obtains the titania slurry that massfraction is about 18wt%. The titanium paper tinsel surface of washes clean will be coated under above-mentioned titania slurry room temperature, leave standstill 10min. Above-mentioned titanium paper tinsel substrate is positioned over roll-in in the roll-to-roll equipment applying Terpineol 350 (releasing agent), roller wheel spacing 0.3mm, roller wheel linear velocity 15cm/s; And in thermal station 100 DEG C of heat treated, 30 minutes time length. Drying after substrate being washed five times with deionized water after being cooled to room temperature. Dried substrate is placed in retort furnace 450 DEG C calcining 50 minutes. As shown in Figure 4, it may also be useful to flexible dye sensitized solar energy cell photoanode thickness prepared by roll-to-roll method is comparatively even, at 15-20 micron. By this application of electrode in dye sensitization solar battery: when it is cooled to 80 DEG C, above-mentioned sample is soaked in 0.5mMN719 dyestuff 24 hours, recording open circuit voltage is 1.00V, current density is 17.29mA/cm2, and packing factor is 0.62, and photoelectric transformation efficiency is 10.85%.
Embodiment 3
4.0 grams of titanium dioxide are taken under room temperature, add ethanol 100mL, Terpineol 350 20 grams and massfraction are the ethyl cellulose (3 grams: 30 grams of ethanol) of 10wt%, ball-milling processing 48 hours, ball milling speed is 20 revs/min, forming finely dispersed solution, last rotary evaporation obtains the titania slurry that massfraction is about 15wt%. The titanium paper tinsel surface of washes clean will be coated under above-mentioned titania slurry room temperature, leave standstill 10min. Above-mentioned titanium paper tinsel substrate is positioned over roll-in in the roll-to-roll equipment applying Terpineol 350 (releasing agent), roller wheel spacing 0.5mm, roller wheel linear velocity 10cm/s; And in thermal station 100 DEG C of heat treated, 30 minutes time length. Drying after substrate being washed three times with deionized water after being cooled to room temperature. Dried substrate is placed in retort furnace 450 DEG C calcining 50 minutes. As shown in Figure 5, light anode titanium dioxide film thickness can be controlled in 15-20 micron level.
Embodiment 4
5.0 grams of titanium dioxide are taken under room temperature, add ethanol 100mL, Terpineol 350 20 grams and massfraction are the ethyl cellulose (3 grams: 30 grams of ethanol) of 10wt%, ball-milling processing 24 hours, ball milling speed is 30 revs/min, forming finely dispersed solution, last rotary evaporation obtains the titania slurry that massfraction is about 18wt%. The titanium paper tinsel surface of washes clean will be coated under above-mentioned titania slurry room temperature, leave standstill 10min. Above-mentioned titanium paper tinsel substrate is positioned over roll-in in the roll-to-roll equipment applying Terpineol 350 (releasing agent), roller wheel spacing 0.5mm, roller wheel linear velocity 10cm/s; And in thermal station 130 DEG C of heat treated, 10 minutes time length. Drying after substrate being washed five times with deionized water after being cooled to room temperature. Dried substrate is placed in retort furnace 500 DEG C calcining 30 minutes. As shown in Figure 6, the flexible dye sensitized solar energy cell photoanode surface that Terpineol 350 uses roll-to-roll method to prepare as releasing agent is comparatively smooth, and particle diameter is at 100 ran and is evenly distributed, and connectivity is good, defines fine and close network structure.
Claims (10)
1. a preparation method for titanium base flexible dye-sensitized solar battery titanium dioxide photo anode, comprising:
(1) being disperseed in a binder by titanium dioxide, ball milling, rotary evaporation, obtains titania slurry;
(2) under room temperature condition, above-mentioned titania slurry is coated on aluminium foil surface, leaves standstill, obtain titanium paper tinsel light anode substrate;
(3) when releasing agent, adopt roll-to-roll method that the titanium paper tinsel light anode substrate of step (2) is carried out roll-in, then thermal treatment, washing, drying, calcining, cooling, obtain titanium base flexible dye-sensitized solar battery titanium dioxide photo anode.
2. the preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode according to claim 1, it is characterised in that: in described step (1), titanium dioxide dispersion is specially in a binder: add ethanol, binding agent, ethyl cellulose dispersion in titanium dioxide respectively; Wherein each composition accounts for the weight ratio of gross weight: titanium dioxide to be 2.9-3.8wt%, ethanol be 79.7-80.3wt%, binding agent are 14.4-14.6wt%, ethyl cellulose is 2.1-2.2wt%.
3. the preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode according to claim 1, it is characterised in that: in described step (1), binding agent is Terpineol 350; The mass percentage concentration of titania slurry is 15-18wt%.
4. the preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode according to claim 1, it is characterised in that: in described step (1), the ball milling time is 24-48h, and ball milling speed is 20-30 rev/min.
5. the preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode according to claim 1, it is characterized in that: in described step (3), titanium paper tinsel light anode substrate is carried out roll-in and is specially by roll-to-roll method: titanium paper tinsel light anode substrate is positioned over roll-in in roll-to-roll equipment, roller wheel linear velocity is 10-15cm/s, and roller wheel spacing is 0.3-0.5mm.
6. the preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode according to claim 1, it is characterised in that: in described step (3), releasing agent is Terpineol 350.
7. the preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode according to claim 1, it is characterised in that: in described step (3), thermal treatment temp is 100-130 DEG C, and the time is 10-30min.
8. the preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode according to claim 1, it is characterised in that: in described step (3), washing is deionized water, and washing times is 3-5 time.
9. the preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode according to claim 1, it is characterised in that: in described step (3), calcining temperature is 450-500 DEG C, and calcination time is 30-50min.
10. the preparation method of a kind of titanium base flexible dye-sensitized solar battery titanium dioxide photo anode according to claim 1, it is characterised in that: in step (3), in titanium base flexible dye-sensitized solar battery titanium dioxide photo anode, titanium dioxide film thickness is 15-20 micron.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113458143A (en) * | 2021-09-02 | 2021-10-01 | 西安稀有金属材料研究院有限公司 | Method for preparing aluminum electrolytic capacitor anode foil by using cold rolling mill |
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| CN101770869A (en) * | 2010-02-09 | 2010-07-07 | 新奥科技发展有限公司 | Method for preparing titanium dioxide films for dye-sensitized solar battery |
| CN102290254A (en) * | 2011-06-02 | 2011-12-21 | 天津大学 | Light anode of dye sensitized solar cell and preparation method thereof |
| CN102543472A (en) * | 2012-01-31 | 2012-07-04 | 奇瑞汽车股份有限公司 | Photoanode preparation method for dye-sensitized solar cell |
| CN102623186A (en) * | 2012-04-01 | 2012-08-01 | 东华大学 | Titanium-foil-based flexible dye-sensitized solar cell and preparation method thereof |
| US20140216536A1 (en) * | 2013-02-06 | 2014-08-07 | National Cheng Kung University | Flexible dye-sensitized solar cell |
| CN105390299A (en) * | 2015-12-16 | 2016-03-09 | 湖南耐普恩科技有限公司 | Preparation method for supercapacitor pole piece |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101770869A (en) * | 2010-02-09 | 2010-07-07 | 新奥科技发展有限公司 | Method for preparing titanium dioxide films for dye-sensitized solar battery |
| CN102290254A (en) * | 2011-06-02 | 2011-12-21 | 天津大学 | Light anode of dye sensitized solar cell and preparation method thereof |
| CN102543472A (en) * | 2012-01-31 | 2012-07-04 | 奇瑞汽车股份有限公司 | Photoanode preparation method for dye-sensitized solar cell |
| CN102623186A (en) * | 2012-04-01 | 2012-08-01 | 东华大学 | Titanium-foil-based flexible dye-sensitized solar cell and preparation method thereof |
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| CN113458143A (en) * | 2021-09-02 | 2021-10-01 | 西安稀有金属材料研究院有限公司 | Method for preparing aluminum electrolytic capacitor anode foil by using cold rolling mill |
| CN113458143B (en) * | 2021-09-02 | 2021-11-23 | 西安稀有金属材料研究院有限公司 | Method for preparing aluminum electrolytic capacitor anode foil by using cold rolling mill |
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