CN101794670B - Preparation method of photo anode of dye-sensitized solar cell with optical gradient - Google Patents
Preparation method of photo anode of dye-sensitized solar cell with optical gradient Download PDFInfo
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- CN101794670B CN101794670B CN2010101399504A CN201010139950A CN101794670B CN 101794670 B CN101794670 B CN 101794670B CN 2010101399504 A CN2010101399504 A CN 2010101399504A CN 201010139950 A CN201010139950 A CN 201010139950A CN 101794670 B CN101794670 B CN 101794670B
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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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- 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
- H01G9/2059—Light-sensitive devices comprising an organic dye as the active light absorbing material, e.g. adsorbed on an electrode or dissolved in solution
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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
Abstract
The invention relates to a preparation method of photo anode of dye-sensitized solar cell with optical gradient, comprising the following steps: (1), adding sodium hydroxide or ammonia water into the inorganic titanium slat used as the precursor to generate the precipitation, washing the precipitation with water to acquire solid in the gel manner, peptizing the same to prepare the pale yellow transparent solution, diluting the prepared solution, and performing hydro-thermal process on the same so as to prepare the transparent TiO2 solution of anatase phase; (2), depositing a TiO2 compact layer on a conductive substrate by spin-coating, dipping/coating or casting method; (3), depositing a layer of porous TiO2 film on the TiO2 compact layer by screen printing, blade coating method or spray coating method; and (4), calcining the film with two structure so as to form the photo anode with optical gradient. In the invention, the colloidal sol for preparing the transparent compact layer does not contain any organic matter and other impurities; the high temperature sintering is not required; the blocking layer formed between the conductive layer and the porous film blocks the corrosion of electrolyte on the substrate; and the preparation method has excellent application foreground.
Description
Technical field
The invention belongs to dye-sensitized solar cell anode and make field, particularly a kind of preparation method with dye-sensitized solar cell anode of optical gradient.
Background technology
1991;
etc. prepared a kind of novel solar battery that is similar to the photosynthesis of plant principle, is called dye sensitized nano crystal salar battery (DSSCs).Because its cost is low, preparation technology is simple, electricity conversion is higher, causes the extensive concern of researcher to low-cost photovoltaic battery.
DSSC mainly contains the porous nano titanium oxide film of electro-conductive glass, absorption monolayer dyestuff, the electro-conductive glass and the electrolyte of platinum plating formed.Different with traditional silica-based solar cell, dye sensitization can battery be by means of the strong absorption of dyestuff to light very much, is converted into electric energy to luminous energy, and the absorption of electronics is carried out with transporting to separate.Core component light anode as DSSC is the emphasis that the researcher studies always, comprises that different nanostructures is to the cell photoelectric Effect on Performance.The general problem that the light anode for preparing with the powder coated method now exists is not strong with the adhesion of electro-conductive glass substrate; Porous membrane comes off from conductive glass surface easily; And electrolyte directly contacts with electro-conductive glass easily; Not only influence the derivation of light induced electron, increased I in light induced electron and the electrolyte
3 -Compound probability.And electrolyte can corrode conductive substrates, had a strong impact on the electricity conversion and the stability of battery, hindered the commercial applications of battery.
Common TiCl with 40mm
4The aqueous solution is handled electro-conductive glass, and the fine and close nano-titanium oxide film of preparation one deck reduces back of the body electronics and electrolytical compound, stops the corrosion of electrolyte to substrate simultaneously, finally also can improve the photoelectric current of battery.The problem that this method exists is TiCl
4As a kind of a kind of material of very easily hydrolysis, itself electro-conductive glass there is certain corrosion, discharge acidic materials after the heat treatment.And introduced Cl in the cell preparation process
-
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method with dye-sensitized solar cell anode of optical gradient.The prepared colloidal sol of the present invention approaches neutrality; Do not contain any organic substance and other impurity; Need not pass through high temperature sintering, the barrier layer that between conductive layer and porous membrane, forms has stopped the corrosion of electrolyte to substrate; The final photoelectric current that also can improve battery has a good application prospect.
A kind of preparation method of the present invention with dye-sensitized solar cell anode of optical gradient; Comprise: (1) is presoma with the inorganic titanium salt of 0.4～1M; Adding 0.1～4M NaOH or ammoniacal liquor make it produce deposition under 25～80 ℃, and the deposition process is washed 4～5 times to neutrality, obtains gelatinous solid; With its dispergation 0.5～5 hour; Obtain shallow yellow transparent solution,, form the transparent anatase phase TiO that concentration is 0.1～5wt% after 2～50 hours with 100～200 ℃ of hydrothermal treatment consists with 1～5 times of gained solution dilution
2Colloidal sol;
(2) the employing rotation applies on conductive substrates, dipping lifts or The tape casting deposition one deck anatase-phase nano crystalline substance TiO
2Compacted zone;
(3) through silk screen printing, blade coating or spraying process at TiO
2Deposition one deck porous TiO on the compacted zone
2Film;
The film that (4) will have two kinds of structures is calcined the light anode that formation in 15～120 minutes has optical gradient at 400～550 ℃.
Inorganic titanium salt in the said step (1) is Ti (SO
4)
2, TiOSO
4, Ti (NO
3)
4Or TiCl
4
Dispergation method in the said step (1) for gelatinous solid with 1g: 1～10ml is dispersed in HNO
3Or H
2O
2In.
Conductive substrates in the said step (2) is the SnO of doped with fluorine
2Electro-conductive glass (SnO
2: F) be called for short FTO or indium tin oxide-coated glass and be called for short the ITO electro-conductive glass.
Spin coating process in the said step (2) is with TiO
2Colloidal sol drips to the conductive substrates that is fixed on the sol evenning machine, and even glue is 10～1000 seconds under the rotating speed of sol evenning machine is 50-2000 rev/min, with TiO
2Compacted zone air dry or in baking oven dry 0.1～10 hour, baking temperature is 25～100 ℃, repeats above operation 1 to 50 time.
Dipping czochralski process in the said step (2) is for to put into TiO with conductive substrates
2In the colloidal sol, flooded 1～100 minute, TiO
2Compacted zone air dry or in baking oven dry 0.1～10 hour, baking temperature is 25～100 ℃, repeats above operation 1～10 time.
The brilliant TiO of anatase-phase nano in the said step (2)
2Dense layer thickness is 0.1～5 micron.
Porous TiO in the said step (3)
2Film thickness is 5～20 microns.
TiO on the dye-sensitized solar cell anode base material of optical gradient of the present invention
2Film is made up of two parts, and one deck is transparent TiO
2Nanocrystalline compacted zone, another layer are the titanium dioxide layer of porous.With high degree of dispersion anatase phase TiO
2Colloidal sol is raw material, on conductive substrates, forms transparent titanium dioxide nanocrystalline compacted zone through methods such as rotation coating, curtain coating or dipping lift, and thickness is 0.1～5 micron, under 25～80 ℃ of conditions, keeps 0.1～10 hour; Then through methods such as silk screen printing, blade coating, sprayings at nanocrystalline TiO
2Deposit the certain thickness porous titanium oxide film of one deck on the compacted zone again; Obtain having the dye-sensitized solar cell anode of optical gradient at last through calcining.
The present invention adopts the transparent TiO with high degree of dispersion
2Colloidal sol is raw material, has prepared a kind of dye-sensitized solar cell anode with optical gradient.The transparent anatase-phase nano crystalline substance thin film of titanium oxide of preparation one deck densification earlier under cryogenic conditions, and then the titanium deoxid film of deposition one deck porous form the light anode through Overheating Treatment at last.The advantage of this method is that this colloidal sol is to approach neutrality, and does not contain any organic substance and other impurity, need not pass through high temperature sintering.The sol particle pattern is bar-shaped, even particle size distribution.The use of this novel optical gradient dye-sensitized solar cell anode has at first formed a barrier layer between conductive layer and porous membrane, completely cut off electrolyte and contacted with the direct of electro-conductive glass, has reduced I in light induced electron and the electrolyte
3 -Compound probability.Through the I-V characteristic curve test shows of battery, improve a lot with the cell photoelectric of this smooth anode preparation stream.
Beneficial effect
(1) with the inorganic ti sources is presoma; Do not add under the situation of any surfactant; Adopt the synthetic transparent anatase phase oxidation titanium hydrosol of method of deposition dispergation hydrothermal crystallizing,, therefore no longer need higher calcining heat to make its crystallization owing to be the anatase phase.And colloidal sol can not discharge harmful material in heat treatment process, not residual Cl
-Through at the fine and close thin film of titanium oxide of FTO conductive glass surface deposition one deck, not only reduced the I in suprabasil light induced electron of electro-conductive glass and the electrolyte
3 -Compound, stoped the corrosion of electrolyte simultaneously to electro-conductive glass.
(2) and TiCl
4Preliminary treatment is compared, and the film of the optical gradient that the compacted zone that uses colloidal sol to prepare constitutes has higher short circuit current and open circuit voltage.
Description of drawings
Fig. 1 is the X-ray diffractogram of anatase phase colloidal sol;
Fig. 2 is the transparent compacted zone of employing spin-coating method preparation and the comparison diagram of the transmitance of the electro-conductive glass of sky;
Fig. 3 is the structural representation of optical gradient dye-sensitized solar cell anode;
Fig. 4 is the compacted zone SEM surface topography map of optical gradient dye-sensitized solar cell anode;
Fig. 5 is the porous layer SEM surface topography map of optical gradient dye-sensitized solar cell anode;
Fig. 6 is the porous layer SEM sectional drawing of optical gradient dye-sensitized solar cell anode;
Fig. 7 is a different structure light anode preparation DSSC photovoltaic curve.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
After the 1M titanium sulfate solution is warming up to 60 ℃, drip the sodium hydroxide solution of 4M, be neutralized to the pH value and approximate 7, obtain white precipitate, use the distilled water cyclic washing, obtain gelatinous solid.Get in the hydrogen peroxide solution that moist precipitate 80 gram is dispersed in (containing about 12 grams of titanium dioxide) 100 milliliter 30%,, obtain shallow yellow transparent solution 60 ℃ of dispergation 2 hours.Get 10 milliliters of this clear solutions, be diluted to 40 milliliters, join water heating kettle, 120 ℃ of hydrothermal treatment consists are taken out after 12 hours and are formed vitreosol.Get the powder that 20 milliliters of colloidal sol vacuumizes obtain and carry out XRD analysis, X-ray diffraction (XRD) result shows that titanium dioxide wherein is the anatase phase, and is as shown in Figure 1, can find out to be pure anatase phase, and grain size is the 7-8 nanometer.Compound concentration is 50 milliliters of 0.1wt% TiO 2 sols, is placed in 100 milliliters of empty glass beakers.After the cleaning of FTO electro-conductive glass process; Be immersed in the TiO 2 sol 10 minutes, from beaker, take out electro-conductive glass then and put into baking oven, 50 ℃ of dryings 30 minutes; Repeat above operation 2 times, on electro-conductive glass, form the fine and close transparent anatase-phase nano crystal layer of one deck.Through the electro-conductive glass behind the dipping, transmitance generation significant change useless.The microscopic appearance of nanocrystalline laminar surface is as shown in Figure 4, can find out, and the compacted zone surfacing, sol particle is deposited in together closely.Adopting method deposit thickness on compacted zone of silk screen printing then is the thin film of titanium oxide of 8um.At last this laminated film was calcined 30 minutes at 500 ℃, formed dye-sensitized solar cell anode with optical gradient.The structural representation of light anode of DSSC with optical gradient is as shown in Figure 3, is followed successively by conductive layer, compacted zone, porous film layer from the bottom up.
Embodiment 2
After the 1M titanium sulfate solution is warming up to 60 ℃, drip the ammonia spirit of 4M, be neutralized to the pH value and approximate 7 toward the 1M titanium sulfate solution; Obtain white precipitate, use the distilled water cyclic washing, obtain gelatinous solid; Get moist precipitate 80 gram (amounting to into titanium dioxide is 12 grams) it is dispersed in 300 milliliter 30% the hydrogen peroxide solution,, obtain shallow yellow transparent solution in 60 ℃ of dispergation 1 hour; Get 20 milliliters of this clear solutions; Be diluted to 40 milliliters, join water heating kettle, 180 degree hydrothermal treatment consists are taken out after 12 hours and are formed vitreosol.Compound concentration is 50 milliliters of 1wt% TiO 2 sols, is placed in 100 milliliters of glass beakers, and is subsequent use.The FTO electro-conductive glass through after cleaning, is immersed in the TiO 2 sol 30 minutes, took out drying at room temperature then 30 minutes, repeat above operation 2 times.Through the light anode behind the dipping, transmitance generation significant change useless still is transparent, as shown in Figure 2, can find out that transmitance does not have to change basically, explains that compacted zone is transparent.The method that adopts silk screen printing then is at compacted zone above-prepared thin film of titanium oxide, and thickness is 10um, and the laminated film for preparing was 500 ℃ of sintering 30 minutes.The microstructure of porous membrane is as shown in Figure 5, presents typical cellular.It is as shown in Figure 7 to assemble behind the battery photovoltaic performance of different structure; The DSSC density of photocurrent that can find out traditional light anode preparation is minimum; The light anodic current density of handling with titanium tetrachloride secondly, two have the DSSC density of photocurrent of optical gradient light anode preparation maximum.
Embodiment 3
After the 0.85M titanium sulfate solution is warming up to 70 ℃, drip the sodium hydroxide solution of 4M, be neutralized to the pH value and approximate 7 toward the 0.85M titanium sulfate solution; Obtain white precipitate, use the distilled water cyclic washing, obtain gelatinous solid; Getting moist precipitate 80 gram (amounting to into titanium dioxide is 12 grams) is dispersed in it in 200 milliliter 30% the hydrogen peroxide solution; Obtain shallow yellow transparent solution, get 30 milliliters of this clear solutions, be diluted to 70 milliliters; Join water heating kettle, 150 degree hydrothermal treatment consists are taken out after 24 hours and are formed vitreosol.Compound concentration is 50 milliliters of 2wt% TiO 2 sols, is placed in 100 milliliters of glass beakers, and is subsequent use.The ITO electro-conductive glass through after cleaning, is immersed in the TiO 2 sol 50 minutes, takes out then and put into oven drying 30 minutes, baking temperature is 80 ℃.Through the light anode behind the dipping, transmitance generation significant change useless still is transparent.The method that adopts silk screen printing then is at compacted zone above-prepared thin film of titanium oxide, and thickness is 12um, and the laminated film for preparing was 400 ℃ of sintering 30 minutes.The microstructure of porous membrane is as shown in Figure 5, can find out to be typical loose structure, connects loose between the particle.
Embodiment 4
After the 1M titanium sulfate solution is warming up to 60 ℃, drip the ammonia spirit of 4M, be neutralized to the pH value and approximate 7 toward the 1M titanium sulfate solution; Obtain white precipitate, use the distilled water cyclic washing, obtain gelatinous solid; Get moist precipitate 80 gram (amounting to into titanium dioxide is 12 grams) it is dispersed in 800 milliliter 30% the hydrogen peroxide solution,, obtain shallow yellow transparent solution in 50 ℃ of dispergation 2 hours; Get 10 milliliters of this clear solutions; Be diluted to 70 milliliters, join water heating kettle, 200 degree hydrothermal treatment consists are taken out after 10 hours and are formed vitreosol.Compound concentration is 50 milliliters of 5wt% TiO 2 sols, is placed in 100 milliliters of glass beakers, and is subsequent use.The ITO electro-conductive glass through after cleaning, is placed on above the sol evenning machine, and rotary speed is 500 rpms.Rotational time is 30 seconds.Take out then and put into oven drying 20 minutes, baking temperature is 50 ℃, repeats above operation 4 times.Through the light anode after the rotation coating, transmitance generation significant change useless still is transparent.The method that adopts silk screen printing then is at compacted zone above-prepared thin film of titanium oxide, and thickness is 15um, and the laminated film for preparing was 500 ℃ of sintering 30 minutes.The structural representation of light anode of DSSC with optical gradient is as shown in Figure 6, and can find out clearly that optical gradient light anode construction is a double-layer structure: one deck is the anatase phase titanium dioxide compacted zone, and one deck is the titanium dioxide layer of porous.
Claims (8)
1. preparation method with dye-sensitized solar cell anode of optical gradient comprises:
(1) be presoma with the inorganic titanium salt of 0.4～1M; Adding 0.1～4M NaOH or ammoniacal liquor make it produce deposition under 25～80 ℃, and the deposition process is washed 4～5 times to neutrality, obtains gelatinous solid; With it in 25～80 ℃ of dispergation 0.5～5 hour; Obtain shallow yellow transparent solution,, form the transparent anatase phase TiO that concentration is 0.1～5wt% after 2～50 hours with 100～200 ℃ of hydrothermal treatment consists with 1～5 times of gained solution dilution
2Colloidal sol;
(2) the employing rotation applies on conductive substrates, dipping lifts or The tape casting deposition one deck anatase-phase nano crystalline substance TiO
2Compacted zone, dry then;
(3) through silk screen printing, blade coating or spraying process at TiO
2Deposition one deck porous TiO on the compacted zone
2Film;
The film that (4) will have two kinds of structures is calcined the light anode that formation in 15～120 minutes has optical gradient at 400～550 ℃.
2. a kind of preparation method with dye-sensitized solar cell anode of optical gradient according to claim 1 is characterized in that: the inorganic titanium salt in the said step (1) is Ti (SO
4)
2, TiOSO
4, Ti (NO
3)
4Or TiCl
4
3. a kind of preparation method with dye-sensitized solar cell anode of optical gradient according to claim 1 is characterized in that: the dispergation in the said step (1) is meant gelatinous solid with 1g: 1～10ml is dispersed in HNO
3Or H
2O
2In handle.
4. a kind of preparation method with dye-sensitized solar cell anode of optical gradient according to claim 1 is characterized in that: the conductive substrates in the said step (2) is the SnO of doped with fluorine
2Electro-conductive glass (SnO
2: F) be called for short FTO or indium tin oxide-coated glass and be called for short the ITO electro-conductive glass.
5. a kind of preparation method with dye-sensitized solar cell anode of optical gradient according to claim 1 is characterized in that: the spin coating process in the said step (2) is with TiO
2Colloidal sol drips to the conductive substrates that is fixed on the sol evenning machine, and even glue is 10～1000 seconds under the rotating speed of sol evenning machine is 50-2000 rev/min, with TiO
2Compacted zone air dry or in baking oven dry 0.1～10 hour, baking temperature is 25～100 ℃, repeats above operation 1 to 50 time.
6. a kind of preparation method with dye-sensitized solar cell anode of optical gradient according to claim 1 is characterized in that: the dipping czochralski process in the said step (2) is for to put into TiO with conductive substrates
2In the colloidal sol, flooded 1～100 minute, TiO
2Compacted zone air dry or in baking oven dry 0.1～10 hour, baking temperature is 25～100 ℃, repeats above operation 1～10 time.
7. a kind of preparation method with dye-sensitized solar cell anode of optical gradient according to claim 1 is characterized in that: the brilliant TiO of the anatase-phase nano in the said step (2)
2Dense layer thickness is 0.1～5 micron.
8. a kind of preparation method with dye-sensitized solar cell anode of optical gradient according to claim 1 is characterized in that: the porous TiO in the said step (3)
2Film thickness is 5～20 microns.
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| CN102136372B (en) * | 2011-01-22 | 2012-11-14 | 上海联孚新能源科技有限公司 | Dye sensitized solar cell treated by ion implantation and preparation method thereof |
| CN102176387B (en) * | 2011-03-02 | 2012-09-26 | 东莞宏威数码机械有限公司 | Methods for preparing porous spherical titanium dioxide paste and sensitized photo-anode |
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| CN103714975B (en) * | 2013-12-16 | 2017-01-18 | 华侨大学 | Method for preparing light anode barrier layer of sensitized solar cell |
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| CN106206031A (en) * | 2015-05-08 | 2016-12-07 | 北京纳米能源与系统研究所 | Light anode, preparation method, battery and the photovoltaic device of fiber dyes sensitization |
| CN104966620B (en) * | 2015-05-15 | 2018-02-13 | 重庆大学 | Flexible dye-sensitized solar battery light anode based on active metal |
| US9620466B1 (en) * | 2015-11-30 | 2017-04-11 | Infineon Technologies Ag | Method of manufacturing an electronic device having a contact pad with partially sealed pores |
| CN105895378B (en) * | 2016-06-28 | 2018-09-28 | 郑州大学 | The preparation method of dye-sensitized solar cells two-layer titanium dioxide light anode |
| CN106587282B (en) * | 2016-12-08 | 2020-02-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Double-functional multi-template molecularly imprinted photoelectric anode material and preparation and application thereof |
| CN108470623B (en) * | 2018-03-09 | 2019-09-24 | 三峡大学 | Used by dye sensitization solar battery silica and zinc oxide anti-reflection film and preparation method thereof |
| CN108823590A (en) * | 2018-06-19 | 2018-11-16 | 上海大学 | TiO is carried out using electron irradiation2The modified method and its application of nano-wire array |
| CN113751294A (en) * | 2021-09-09 | 2021-12-07 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing titanium-based nano anticorrosive film by taking titanium tetrachloride as titanium source |
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| CN101101929A (en) * | 2006-07-07 | 2008-01-09 | 北京大学 | Dye-sensitized solar battery and structure of its work pole |
| CN101320631A (en) * | 2008-07-08 | 2008-12-10 | 西安交通大学 | Demixing-adsorption cooperated-sensitization wide optical spectrum dye sensitization solar battery |
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