CN102983005A - Preparation method for photo-anode with TiO2 compact layer - Google Patents

Preparation method for photo-anode with TiO2 compact layer Download PDF

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CN102983005A
CN102983005A CN2012105095390A CN201210509539A CN102983005A CN 102983005 A CN102983005 A CN 102983005A CN 2012105095390 A CN2012105095390 A CN 2012105095390A CN 201210509539 A CN201210509539 A CN 201210509539A CN 102983005 A CN102983005 A CN 102983005A
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tio
electro
tio2
conductive glass
compacted zone
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冯亚青
杨雁博
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Tianjin 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 invention discloses a preparation method for a photo-anode with a TiO2 compact layer, and belongs to the technical field of dye-sensitized solar cells. The method comprises the following steps: preparing TiO2 transparent sol; preparing a TiO2 film on conducting glass in the TiO2 transparent sol by using a dip-coating method and calcining the TiO2 film to obtain the TiO2 compact layer; preparing TiO2 porous layer slurry; coating the TiO2 porous layer slurry on the TiO2 compact layer by using a silk screen print method; and carrying out calcining to obtain the photo-anode with the TiO2 compact layer. The preparation method has the advantages that the light current of the cells is improved due to the barrier effect of the TiO2 compact layer; the connection between the TiO2 porous layer and a conducting substrate is reinforced at the same time; and the method has simple preparation technique, and is suitable for industrial mass production.

Description

Has TiO 2The preparation method of the light anode of compacted zone
Technical field
The present invention relates to a kind of TiO of having 2The preparation method of the light anode of compacted zone belongs to the DSSC technical field.
Background technology
In recent years, DSSC is owing to its pollution-free, lower production cost, simple manufacture craft, the higher advantages such as electricity conversion have obtained domestic and international extensive and deep research.
The principal element that the restriction efficiency of dye-sensitized solar battery promotes is the compound of electronics and passback.The electronics passback makes battery produce backward current, has reduced largely the electric current of battery.At conductive substrates and TiO 2Introduce compacted zone between the porous layer and can prevent effectively that the substrate of light anode conducting from directly contacting with electrolyte, avoided the generation of backward current, reinforced simultaneously TiO 2Porous layer is connected with substrate, is conducive to the raising of electricity conversion.Traditional sol-gal process is difficult for making the TiO with desirable particle size particle 2Compacted zone (CN101740229A) can't prevent at utmost that conductive substrates from directly contacting with electrolyte, so that the raising of cell photoelectric transformation efficiency limited (7 %-10 %).Utilize water TiO 2Colloidal sol can make has the compacted zone that particle diameter is 10 nm left and right sides particles, but can't reach the compactness extent of the compacted zone that organic phase colloidal sol obtains, and stops that the effect of electrolyte is relatively poor.So utilize water colloidal sol to prepare compacted zone and reach preferably blocking effect, need to adopt spraying or spin-coating film method (CN101697321A).This has increased the cost of making and the difficulty of operation greatly.
Summary of the invention
The object of the present invention is to provide a kind of TiO of having 2The preparation method of the light anode of compacted zone, the method preparation process is simple, and the light anode that makes with the method has improved photoelectric current, and then has improved the electricity conversion of battery.
The present invention realized by the following technical programs, and a kind of have a TiO 2The preparation method of the light anode of compacted zone is characterized in that comprising following process:
1) butyl titanate, acetylacetone,2,4-pentanedione and ethanol in molar ratio 1:1:25-30 under stirring condition, mix, be A liquid; You mix lauryl amine, 0.01 mol/L HCl, ethanol and hydromassage than 1:0.1:30-40:200, be B liquid, under temperature 35-45 ℃, A liquid mixed with lauryl amine mol ratio 4:1 by butyl titanate with B liquid, and stir 2-3 h, be positioned over dark place ageing 160-180 h, obtain TiO 2Vitreosol;
2) employing lifts the infusion process plated film, and at the sticking adhesive waterproof tape in the electro-conductive glass both sides of 7.5 cm * 4 cm, this part links to each other with wire when to be tested, and electro-conductive glass is at TiO 2Speed with 1-3 mm/s in the colloidal sol lifts, and lifts in the process, leaves standstill electro-conductive glass 3-5 min in colloidal sol, after lifting operation and finishing electro-conductive glass is put into 110 ℃ the dry 5-10 min of vacuum drying oven.So lift 3 times, obtain white translucent TiO at electro-conductive glass 2Compacted zone;
3) will be coated with TiO 2The electro-conductive glass of compacted zone is put into Muffle furnace and is calcined, and temperature rises to 450-500 ℃ with the programming rate of 5-10 ℃/min from room temperature, keeps 450-500 ℃ of constant temperature 15-30 min, and obtaining thickness is the even smooth TiO of 600-700 nm 2Compacted zone;
4) titanium dioxide, terpinol, ethyl cellulose, ethanol and the zirconium pearl ratio ball milling take mass ratio as 1:4.06:0.5:20:60 is mixed, revolve to steam and remove ethanol, make TiO 2The porous layer slurry;
5) TiO that step 4) is made 2The porous layer slurry is printed on the compacted zone of electro-conductive glass with scraper, print six layers, then calcining after 110 ℃ of lower oven dry, in Muffle furnace, rise to 500 ℃ with 5 ℃/min from room temperature, constant temperature 30 min, gained light anode is soaked into two-tetrabutylammonium-two (isothiocyanos) two (2,2'-bipyridines-4 after will calcining, the 4'-dicarboxyl) 20 h in ruthenium (II) dye solution make and have TiO 2The dye sensitization light anode of compacted zone.
The present invention has following advantage: at first, utilize water TiO 2Colloidal sol makes has the compacted zone that particle diameter is 10 nm left and right sides particles, and this compacted zone has good blocking effect, prevents the passback of electronics on the conductive substrates, has improved photoelectric current.Secondly, TiO 2Compacted zone has been reinforced TiO 2Porous layer is connected with substrate, is conducive to the raising of electricity conversion.At last, the production operation process of the method is simple, and equipment requirement is low, and raw material is industrial goods and is easy to obtain, is suitable for suitability for industrialized production.
Description of drawings:
Fig. 1 is that the particle diameter that the embodiment of the invention 1 makes is the TiO of 10 nm 2Compacted zone surface topography Electronic Speculum figure.
Fig. 2 is that the particle diameter that the embodiment of the invention 1 makes is the TiO of 10 nm 2Compacted zone cross section Electronic Speculum figure.
Embodiment:
Embodiment 1:
1) gets 13.6 ml butyl titanates and mix with 4.0 ml acetylacetone,2,4-pentanediones, be added to again in the 60ml ethanol and under stirring condition, mix, be A liquid; 1.80 the g lauryl amine mixes in 36 ml water and 22.5 ml ethanolic solutions with 9.7 ml, 0.1 mol/L HCl, is B liquid.Under 40 ℃ B liquid is dropwise joined in the A liquid, reaction is 2 hours under stirring condition, obtains transparent salmon liquid.Colloidal sol is positioned over dark place ageing 168 h obtains stable TiO 2Vitreosol.
2) at the sticking adhesive waterproof tape in the electro-conductive glass both sides of 7.5 cm*4 cm, this part links to each other with wire when to be tested.Electro-conductive glass is at TiO 2Speed with 2 mm/s in the colloidal sol lifts, and lifts in the process, leaves standstill electro-conductive glass 5 min in colloidal sol, after lifting operation and finishing electro-conductive glass is put into 110 ℃ dry 5 min of vacuum drying oven.So lift 3 times, obtain white translucent TiO 2Film.
3) will be coated with TiO 2The electro-conductive glass of compacted zone is put into Muffle furnace and is calcined, and temperature rises to 500 ℃ with the programming rate of 5 ℃/min from room temperature, keeps 500 ℃ of constant temperature 30 min.Can obtain thickness is the smooth TiO of 655 nm 2Compacted zone.
4) take by weighing the 4.06g terpinol, 20g absolute ethyl alcohol, 1g TiO 2Powder (P25), 0.5g ethyl cellulose and 60 g zirconium pearls, ball milling mixing 2h, ball milling is complete removes ethanol afterwards with rotary evaporator, obtains TiO 2The porous layer slurry.
5) with scraper with TiO 2Porous layer slurry printing multilayer is calcined after the oven dry on electro-conductive glass.Gained light anode is soaked into 20h in two-tetrabutylammonium-two (isothiocyanos) two (2,2'-bipyridine-4,4'-dicarboxyl) ruthenium (II) dye solution after will calcining, and makes to have TiO 2The dye sensitization light anode of compacted zone.
6) take platinum electrode as to electrode with above-mentionedly have a TiO 2The dye sensitization light anode of compacted zone is assembled, and intermediate course injects electrolyte, namely prepares to have TiO 2The DSSC of compacted zone.Employed electrolyte is that component is: LiI (0.1 mol/L), I 2(0.05 mol/L), 4-TBP (0.5 mol/L), GuSCN (0.05 mol/L), DMPII (0.6 mol/L).Employing Keithley 2400 digital sourcemeters and solar simulator (xenon lamp of light source 500 W, AM 1.5, and optical power density is 100 mW/cm 2) test the battery of having assembled, test result sees the following form.
Embodiment 2:
1) gets the 13ml butyl titanate and mix with 3.9 ml acetylacetone,2,4-pentanediones, be added to again in the 55 ml ethanol and under stirring condition, mix, be A liquid; 1.76 the g lauryl amine mixes in 34.2 ml water and 21ml ethanolic solution with 9.5 ml, 0.1 mol/L HCl, is B liquid.Under 35 ℃ B liquid is dropwise joined in the A liquid, reaction is 3 hours under stirring condition, obtains transparent salmon liquid.Colloidal sol is positioned over dark place ageing 180h obtains stable TiO 2Vitreosol.
2) at the sticking adhesive waterproof tape in the electro-conductive glass both sides of 7.5 cm*4 cm, this part links to each other with wire when to be tested.Electro-conductive glass is at TiO 2Speed with 1.5 mm/s in the colloidal sol lifts, and lifts in the process, leaves standstill electro-conductive glass 3 min in colloidal sol, after lifting operation and finishing electro-conductive glass is put into 110 ℃ dry 10 min of vacuum drying oven.So lift 3 times, obtain white translucent TiO 2Film.
3) will be coated with TiO 2The electro-conductive glass of compacted zone is put into Muffle furnace and is calcined, and temperature rises to 450 ℃ with the programming rate of 8 ℃/min from room temperature, keeps 450 ℃ of constant temperature 15 min.Can obtain thickness is the smooth TiO of 640nm 2Compacted zone.
4) take by weighing the 4.06g terpinol, the 20g absolute ethyl alcohol, 1g P25,0.5g ethyl cellulose and 60g zirconium pearl, ball milling mixes 2 h, and ball milling is complete removes ethanol afterwards with rotary evaporator, makes TiO 2The porous layer slurry.
5) with scraper with TiO 2Porous layer slurry printing multilayer is calcined after the oven dry on electro-conductive glass.Gained light anode is soaked into 20h in two-tetrabutylammonium-two (isothiocyanos) two (2,2'-bipyridine-4,4'-dicarboxyl) ruthenium (II) dye solution after will calcining, and makes to have TiO 2The dye sensitization light anode of compacted zone.
6) take platinum electrode as to electrode with above-mentionedly have a TiO 2The dye sensitization light anode of compacted zone is assembled, and intermediate course injects electrolyte, namely prepares to have TiO 2The DSSC of compacted zone.Employed electrolyte is that component is: LiI (0.1 mol/L), I 2(0.05mol/L), 4-TBP (0.5mol/L), GuSCN (0.05mol/L), DMPII (0.6mol/L).(optical power density is 100mW/cm for the xenon lamp of light source 500W, AM1.5 to adopt Keithley2400 digital sourcemeter and solar simulator 2) test the battery of having assembled, test result sees the following form.
Embodiment 3:
1) gets 14 ml butyl titanates and mix with 4.2 ml acetylacetone,2,4-pentanediones, be added to again in the 65 ml ethanol and under stirring condition, mix, be A liquid; 1.90 the g lauryl amine mixes in 37ml water and 23ml ethanolic solution with 10.3 ml, 0.1 mol/L HCl, is B liquid.Under 45 ℃ B liquid is dropwise joined in the A liquid, reaction is 3 hours under stirring condition, obtains transparent salmon liquid.Colloidal sol is positioned over dark place ageing 170h obtains stable TiO 2Vitreosol.
2) at the sticking adhesive waterproof tape in the electro-conductive glass both sides of 7.5 cm*4 cm, this part links to each other with wire when to be tested.Electro-conductive glass is at TiO 2Speed with 2.5 mm/s in the colloidal sol lifts, and lifts in the process, leaves standstill electro-conductive glass 4 min in colloidal sol, after lifting operation and finishing electro-conductive glass is put into 110 ℃ dry 8 min of vacuum drying oven.So lift 3 times, obtain white translucent TiO 2Film.
3) will be coated with TiO 2The electro-conductive glass of compacted zone is put into Muffle furnace and is calcined, and temperature rises to 500 ℃ with the programming rate of 10 ℃/min from room temperature, keeps 500 ℃ of constant temperature 30 min.Can obtain thickness is the smooth TiO of 670nm 2Compacted zone.
4) take by weighing the 4.06g terpinol, the 20g absolute ethyl alcohol, 1g P25,0.5g ethyl cellulose and 60g zirconium pearl, ball milling mixing 2h, ball milling is complete removes ethanol afterwards with rotary evaporator, obtains TiO 2The porous layer slurry.
5) with scraper with TiO 2Porous layer slurry printing multilayer is calcined after the oven dry on electro-conductive glass.Gained light anode is soaked into 20 h in two-tetrabutylammonium-two (isothiocyanos) two (2,2'-bipyridine-4,4'-dicarboxyl) ruthenium (II) dye solution after will calcining, and makes to have TiO 2The dye sensitization light anode of compacted zone.
6) take platinum electrode as to electrode with above-mentionedly have a TiO 2The dye sensitization light anode of compacted zone is assembled, and intermediate course injects electrolyte, namely prepares to have TiO 2The DSSC of compacted zone.Employed electrolyte is that component is: LiI (0.1 mol/L), I 2(0.05 mol/L), 4-TBP (0.5 mol/L), GuSCN (0.05 mol/L), DMPII (0.6 mol/L).Employing Keithley 2400 digital sourcemeters and solar simulator (xenon lamp of light source 500 W, AM 1.5, and optical power density is 100 mW/cm 2) test the battery of having assembled, test result sees the following form.
Comparative Examples 1:
1) take by weighing the 4.06g terpinol, the 20g absolute ethyl alcohol, 1g P25,0.5g ethyl cellulose and 60g zirconium pearl, ball milling mixing 2h, ball milling is complete removes ethanol afterwards with rotary evaporator, obtains TiO 2The porous layer slurry.
2) electro-conductive glass is not done any processing, with scraper with TiO 2Porous layer slurry printing multilayer is calcined after the oven dry on electro-conductive glass.Gained light anode is soaked into 20 h in two-tetrabutylammonium-two (isothiocyanos) two (2,2'-bipyridine-4,4'-dicarboxyl) ruthenium (II) dye solution after will calcining, and makes to have TiO 2The dye sensitization light anode of compacted zone.
3) take platinum electrode as electrode and the above-mentioned dye sensitization light anode that does not contain compacted zone are assembled, intermediate course injects electrolyte, namely makes not contain TiO 2The DSSC of compacted zone.Employed electrolyte is that component is: LiI (0.1 mol/L), I 2(0.05 mol/L), 4-TBP (0.5 mol/L), GuSCN (0.05 mol/L), DMPII (0.6 mol/L).Employing Keithley 2400 digital sourcemeters and solar simulator (xenon lamp of light source 500 W, AM 1.5, and optical power density is 100 mW/cm 2) test the battery of having assembled, test result sees the following form.
Comparative Examples 2:
1) takes by weighing 47.43g TiCl 4Solution dropwise joins under stirring condition in the 100 ml frozen water, obtains water white TiCl 4The aqueous solution is with gained TiCl 4The aqueous solution moves to constant volume in the 500 ml volumetric flasks, obtains the TiCl of 0.5mol/L 4The aqueous solution.
2) electro-conductive glass is placed culture dish, add the TiCl of 0.5 mol/L 4The aqueous solution makes electro-conductive glass be fully immersed in TiCl 4In the aqueous solution, put into 70 ℃ vacuum drying oven with after the preservative film sealing, take out behind 30 min, remain in TiCl on the electro-conductive glass with alcohol flushing 4, afterwards electro-conductive glass is put into Muffle furnace, rise to 500 ℃ with the programming rate of 5 ℃/min from room temperature, keep 500 ℃ of constant temperature 30 min, obtain conventional Ti O 2Compacted zone.
3) take by weighing the 4.06g terpinol, the 20g absolute ethyl alcohol, 1g P25,0.5g ethyl cellulose and 60g zirconium pearl, ball milling mixing 2h, ball milling is complete removes ethanol afterwards with rotary evaporator, obtains TiO 2The porous layer slurry.
4) with scraper with TiO 2Porous layer slurry printing multilayer is calcined after the oven dry on electro-conductive glass.Gained light anode is soaked into 20h in two-tetrabutylammonium-two (isothiocyanos) two (2,2'-bipyridine-4,4'-dicarboxyl) ruthenium (II) dye solution after will calcining, and makes to have TiO 2The dye sensitization light anode of compacted zone.
5) take platinum electrode as to electrode with above-mentionedly have a conventional Ti O 2The dye sensitization light anode of compacted zone is assembled, and intermediate course injects electrolyte, namely makes to have conventional Ti O 2The DSSC of compacted zone.Employed electrolyte is that component is: LiI (0.1 mol/L), I 2(0.05 mol/L), 4-TBP (0.5 mol/L), GuSCN (0.05 mol/L), DMPII (0.6 mol/L).Employing Keithley 2400 digital sourcemeters and solar simulator (xenon lamp of light source 500 W, AM 1.5, and optical power density is 100 mW/cm 2) test the battery of having assembled, test result sees the following form.
Following table is that the performance parameter of embodiment and the prepared DSSC of Comparative Examples compares

Claims (1)

1. one kind has TiO 2The preparation method of the light anode of compacted zone is characterized in that comprising following process:
1) butyl titanate, acetylacetone,2,4-pentanedione and ethanol in molar ratio 1:1:25-30 under stirring condition, mix, be A liquid; You mix lauryl amine, 0.01 mol/L HCl, ethanol and hydromassage than 1:0.1:30-40:200, be B liquid, under temperature 35-45 ℃, A liquid mixed with lauryl amine mol ratio 4:1 by butyl titanate with B liquid, and stir 2-3 h, be positioned over dark place ageing 160-180 h, obtain TiO 2Vitreosol;
2) employing lifts the infusion process plated film, and at the sticking adhesive waterproof tape in the electro-conductive glass both sides of 7.5 cm * 4 cm, this part links to each other with wire when to be tested, and electro-conductive glass is at TiO 2Speed with 1-3 mm/s in the colloidal sol lifts, lift in the process, leave standstill electro-conductive glass 3-5 min in colloidal sol, after lifting operation and finishing electro-conductive glass is put into 110 ℃ the dry 5-10min of vacuum drying oven, so lift 3 times, obtain white translucent TiO at electro-conductive glass 2Compacted zone;
3) will be coated with TiO 2The electro-conductive glass of compacted zone is put into Muffle furnace and is calcined, and temperature rises to 450-500 ℃ with the programming rate of 5-10 ℃/min from room temperature, keeps 450-500 ℃ of constant temperature 15-30min, and obtaining thickness is the even smooth TiO of 600-700 nm 2Compacted zone;
4) titanium dioxide, terpinol, ethyl cellulose, ethanol and the zirconium pearl ratio ball milling take mass ratio as 1:4.06:0.5:20:60 is mixed, revolve to steam and remove ethanol, make TiO 2The porous layer slurry;
5) TiO that step 4) is made 2The porous layer slurry is printed on the compacted zone of electro-conductive glass with scraper, print six layers, then calcining after 110 ℃ of lower oven dry, in Muffle furnace, rise to 500 ℃ with 5 ℃/min from room temperature, constant temperature 30min, gained light anode is soaked into two-tetrabutylammonium-two (isothiocyanos) two (2,2'-bipyridines-4 after will calcining, the 4'-dicarboxyl) 20 h in ruthenium (II) dye solution make and have TiO 2The light anode of compacted zone.
CN2012105095390A 2012-12-04 2012-12-04 Preparation method for photo-anode with TiO2 compact layer Pending CN102983005A (en)

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Cited By (4)

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CN104599844A (en) * 2015-01-16 2015-05-06 华东理工大学 Dye-sensitized solar cell photo-anode producing method
CN105185594A (en) * 2015-09-22 2015-12-23 中国科学院上海硅酸盐研究所 Dye-sensitized solar cell anode substrate pretreatment sol and preparation method and application thereof
CN105489771A (en) * 2015-11-24 2016-04-13 青岛黑金热工能源有限公司 Solar cell compact layer slurry and preparation method therefor
CN106589388A (en) * 2016-03-18 2017-04-26 北京华钛高科科技有限公司 Linear titanium oxide polymer, preparation method and application

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104599844A (en) * 2015-01-16 2015-05-06 华东理工大学 Dye-sensitized solar cell photo-anode producing method
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CN105489771A (en) * 2015-11-24 2016-04-13 青岛黑金热工能源有限公司 Solar cell compact layer slurry and preparation method therefor
CN105489771B (en) * 2015-11-24 2019-03-05 青岛黑金热工能源有限公司 Solar battery compacted zone slurry and preparation method thereof
CN106589388A (en) * 2016-03-18 2017-04-26 北京华钛高科科技有限公司 Linear titanium oxide polymer, preparation method and application

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Application publication date: 20130320