CN103903857B - Method for preparing dye-sensitized solar cell photoanode by using titanium dioxide - Google Patents
Method for preparing dye-sensitized solar cell photoanode by using titanium dioxide Download PDFInfo
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- CN103903857B CN103903857B CN201210577992.5A CN201210577992A CN103903857B CN 103903857 B CN103903857 B CN 103903857B CN 201210577992 A CN201210577992 A CN 201210577992A CN 103903857 B CN103903857 B CN 103903857B
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- dye
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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 dye-sensitized solar cell photoanode by using titanium dioxide. The method includes the steps of: ball-milling and mixing a titanium dioxide material, an organic carrier and an additive to obtain titanium dioxide slurry; coating the titanium dioxide slurry obtained by step 1 on a conductive substrate, and calcining to obtain a titanium dioxide film; immersing the titanium dioxide film in a dye solution, and taking the film out to obtain the dye-sensitized solar cell photoanode. The method provided by the invention is simple in process, can effectively improve the defect of poor dispersity of titanium dioxide powder, the obtained titanium dioxide film has a strong capability of being bonded to the conductive substrate, and is not easy to crack, and light permeability of the film is good, so the obtained dye-sensitized solar cell photoanode has a stable structure, good light transmission, and high photoelectric conversion efficiency.
Description
Technical field
The present invention relates to a kind of method for preparing dye-sensitized solar cell anode, more particularly to one kind titanium dioxide
The method that titanium prepares dye-sensitized solar cell anode.
Background technology
Instead the energy of Fossil fuel, make use of the solaode of sunlight to receive publicity, and people are carried out to which
Various researchs.Solaode is a kind of photoelectric conversion device for converting light energy into electric energy, due to using sunlight as energy
Source, so the impact to earth environment is minimum, widely can be popularized.
The research and development of luminous energy is converted solar energy in recent years quickly.Apply and moved by the photoinduction electronics of dye sensitization
Dynamic dye-sensitized solar cell(Dye-Sensitized Solar Cell, DSSC), instead silicon in recent years(Si)
The solaode of future generation of class solaode etc. receives publicity, and is extensively studied.DSSC
(DSSC)Advantage it is very prominent:1st, make simple, low cost;2nd, the dye sensitizing agent for being used can be in very low light energy
Saturation is issued to, therefore can be used under various illumination conditions;3rd, can be in normal work within the scope of very wide temperature;4th, can be with
Transparent product is made, door and window, roof and vehicle top is applied to.Therefore it rapidly becomes the research emphasis and heat of countries in the world
Point, achieves abundant achievement, has started the upsurge that DSSC solaodes are studied by various countries.Current liquid dye sensitization solar
The electricity conversion of battery is up to 11.2%.
In DSSC, the impact of the performance of light anode to battery efficiency is even more important.In order to the greatest extent may be used
High dye adsorption amount, good conductive substrates binding ability and electron transfer rate, the transmission of titanium dioxide photo anode can be realized
Porous of rate, particle dispersion and film etc. are all very crucial.
The raw material of nano titanium oxide light anode mainly has hydro-thermal method and commercially available titanium dioxide powder etc. at present.Hydro-thermal
The titania slurry grain crystalline degree height of method preparation, good dispersion, corresponding photoelectric transformation efficiency are also high, but hydro-thermal method will
The slurry washing that reacted in autoclave for a long time, obtains but also the step such as need to disperse, rotate, this preparation technology phase
When complicated, high cost.Therefore commercially available titanium dioxide powder directly prepares titania slurry and just receives more and more higher
Attention, its process is simple, low price, but titanium dioxide powder bad dispersibility, by it prepare titanium dioxide film and base
Bear building-up closes ability, easily the translucidus of cracking and film can be poor.Therefore improve titanium dioxide powder and substrate adhesion and
Transmitance is just particularly important.
The content of the invention
It is an object of the invention to overcome above-mentioned deficiency, there is provided one kind titanium dioxide prepares DSSC
The method of light anode, preparation process is simple, obtained light anode Stability Analysis of Structures, light transmission are good, and electricity conversion is high.
The invention provides a kind of method that titanium dioxide prepares dye-sensitized solar cell anode, including it is following
Step:
Titanic oxide material, organic carrier and additive ball milling mixing are obtained titania slurry, wherein two by step 1
The weight ratio of titania meterial and organic carrier is 1:(3~6), the weight of additive is titanic oxide material and organic carrier
The 0.1% ~ 10% of gross weight;
Step 2, step 1 gained titania slurry is coated in conductive substrates, and calcining obtains titanium dioxide film;
Step 3, in the titanium dioxide film immersion dye solution that step 2 is obtained, taking-up obtains dye sensitization of solar electricity
Pond light anode.
Wherein, titanic oxide material can be commercially available titanium dioxide powder, such as P25, ST21 etc..
Preferably, the additive at least includes the combination for dispersant, the dressing agent for improving film cracking or both.
Preferably, one or more in ethylene glycol, tween, Span etc. of the dispersant.
Preferably, one or more in the compound containing carboxyl, hydroxyl or its combination of the dressing agent.
Wherein, the carboxylated compound can be formic acid, acetic acid, ethanedioic acid, trifluoroacetic acid etc..
Wherein, the hydroxy-containing compounds can be methanol, ethanol, ethylene glycol, propanol, isopropanol, Propylene Glycol, tertiary fourth
Alcohol, glycerol, butanediol, pentanediol, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, trifluoroethanol, hexafluoro are different
Propanol etc..
Preferably, the dressing agent selected from methanol, ethanol, ethylene glycol, propanol, isopropanol, Propylene Glycol, the tert-butyl alcohol, glycerol,
Butanediol, pentanediol, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, formic acid, acetic acid, ethanedioic acid, trifluoro second
One or more in acid, trifluoroethanol, hexafluoroisopropanol etc..
Preferably, organic carrier described in step 1 is the mixture of ethyl cellulose and terpineol, wherein ethyl cellulose
Mass ratio with terpineol is 1:5~1:10.
Preferably, ethyl cellulose is dissolved in terpineol in 60 ~ 100 DEG C of water-baths, mix homogeneously is obtained described to be had
Airborne body.
Wherein, bath temperature is preferably 80 DEG C.
Preferably, in step 1, ball milling speed is 400 ~ 600rpm/sec, and Ball-milling Time is 10 ~ 16 hours
Preferably, in step 2, calcining heat is 400 ~ 600 degree, and calcination time is 10 ~ 60min.
Preferably, conductive substrates described in step 2 are FTO electro-conductive glass.
Wherein, FTO electro-conductive glass is through cleaning treatment.
FTO cleaning steps:Glass shelf EtOH Sonicate 15 minutes, deionized water ultrasound 15 minutes;FTO is placed in into shelf
On, ultrasonic detergent 15 minutes, water wash 5 minutes;Dilute nitric acid solution ultrasound 15 minutes, deionized water drip washing 5 minutes;Hydroxide
Soda solution ultrasound 15 minutes, deionized water drip washing 5 minutes;Deionized water ultrasound 15 minutes, acetone drip washing 5 minutes;Acetone surpasses
Sound 15 minutes, drying machine drying is standby.
Preferably, step 2 gained titanium dioxide film first carries out TiCl carrying out step 3 before processing4Process.
Preferably, the TiCl4It is processed as:Step 2 gained titanium dioxide film is immersed in into 10 ~ 80mmol/L TiCl4It is molten
In liquid, soaking temperature is 10 ~ 90 DEG C, and soak time is 1min ~ 100h.
Preferably, in step 3, dyes concentration is 0.001mmol/L ~ 3mol/L, and soak time is 2 ~ 100h.
Preferably, 0.3 mmol/L of dyes concentration.
Wherein, dyestuff can selected from N3, N719, N749, Z907, Z991, K8, K19, N945, Z910, K73, K51,
One or more in Z955, Z991, cyanine, coumarin, porphyrin, indole, perylene flower cyanines, half Hua Jing etc..
The dyestuff is preferably Z991.
The method process is simple that the present invention is provided, can be effectively improved the defect of titanium dioxide powder bad dispersibility, obtained
Titanium dioxide film is strong with conductive substrates binding ability, be not easily susceptible to cracking and the translucidus of film are good, and obtained dye sensitization is too
Positive energy battery light anode Stability Analysis of Structures, light transmission are good, and electricity conversion is high.
Description of the drawings
Fig. 1 is schemed for the 3D of 1 gained dye-sensitized solar cell anode of embodiment 1 and comparative example;
Scanning electron microscope (SEM) photographs of the Fig. 2 for 1 gained dye-sensitized solar cell anode of embodiment 1 and comparative example;
Light transmission rate measurement results of the Fig. 3 for 1 gained dye-sensitized solar cell anode of embodiment;
Fig. 4 is schemed for the 3D of 2 gained dye-sensitized solar cell anode of embodiment 4 ~ 5 and comparative example;
Scanning electron microscope (SEM) photographs of the Fig. 5 for 2 gained dye-sensitized solar cell anode of embodiment 5 and comparative example.
Specific embodiment
With reference to the accompanying drawings, the invention will be further described in conjunction with the embodiments, to more fully understand the present invention.
Embodiment 1
According to mass ratio 1 in 80 DEG C of water-baths:8 are dissolved into ethyl cellulose in terpineol, magnetic agitation mix homogeneously
Prepared organic carrier.
Take 5g titania powder ST21(Japanese stone is former)It is put in ball grinder with the organic carrier that 20g is prepared, adds
1ml ethylene glycol, by this mixture ball milling 24 hours, rotating speed was 500rpm/sec, is transferred to three roll machine rolling and obtains titanium dioxide
Slurry is sealed up for safekeeping standby.
Gained titania slurry automatic screen printing machine is coated on FTO electro-conductive glass, is then calcined at 500 DEG C
30min, obtains titanium dioxide film.
By gained titanium dioxide film ultra-vioket radiation 30 minutes, then with the TiCl of 40 mmol/L4Aqueous solution is soaked at 70 DEG C
Bubble 30 minutes, taking-up water and alcohol flushing, dry for standby.
Again titanium dioxide film is immersed in the Z991 dye solutions that concentration is 0.3mmol/L, soak time is 48 hours,
Prepared dye-sensitized solar cell anode, is then assembled into DSSC, and electrolyte used is Z960.
Embodiment 2
According to mass ratio 1 in 80 DEG C of water-baths:8 are dissolved into ethyl cellulose in terpineol, magnetic agitation mix homogeneously
Prepared organic carrier.
Take 5g titania powder ST21(Japanese stone is former)It is put in ball grinder with the organic carrier that 23g is prepared, adds
1ml glacial acetic acid, by this mixture ball milling 24 hours, rotating speed was 500rpm/sec, is transferred to three roll machine rolling and obtains titanium dioxide
Slurry is sealed up for safekeeping standby.
Gained titania slurry automatic screen printing machine is coated on FTO electro-conductive glass, is then calcined at 500 DEG C
30min, obtains titanium dioxide film.
By gained titanium dioxide film ultra-vioket radiation 30 minutes, then with the TiCl of 40 mmol/L4Aqueous solution is soaked at 70 DEG C
Bubble 30 minutes, taking-up water and alcohol flushing, dry for standby.
Again titanium dioxide film is immersed in the Z991 dye solutions that concentration is 0.3mmol/L, soak time is 48 hours,
Prepared dye-sensitized solar cell anode, is then assembled into DSSC, and electrolyte used is Z960.
Embodiment 3
According to mass ratio 1 in 80 DEG C of water-baths:8 are dissolved into ethyl cellulose in terpineol, magnetic agitation mix homogeneously
Prepared organic carrier.
Take 5g titania powder ST21(Japanese stone is former)It is put in ball grinder with the organic carrier that 23g is prepared, adds
0.5ml glacial acetic acid, by this mixture ball milling 24 hours, rotating speed was 500rpm/sec, is transferred to three roll machine rolling and obtains titanium dioxide
Titanium slurry seals standby up for safekeeping.
Gained titania slurry automatic screen printing machine is coated on FTO electro-conductive glass, is then calcined at 500 DEG C
30min, obtains titanium dioxide film.
By gained titanium dioxide film ultra-vioket radiation 30 minutes, then with the TiCl of 40 mmol/L4Aqueous solution is soaked at 70 DEG C
Bubble 30 minutes, taking-up water and alcohol flushing, dry for standby.
Again titanium dioxide film is immersed in the Z991 dye solutions that concentration is 0.3mmol/L, soak time is 48 hours,
Prepared dye-sensitized solar cell anode, is then assembled into DSSC, and electrolyte used is Z960.
Embodiment 4
According to mass ratio 1 in 80 DEG C of water-baths:8 are dissolved into ethyl cellulose in terpineol, magnetic agitation mix homogeneously
Prepared organic carrier.
Take the organic carrier that 5g titania powder P25 and 20g prepare to be put in ball grinder, add 1ml glacial acetic acid, will
This mixture ball milling 24 hours, rotating speed is 500rpm/sec, is transferred to three roll machine rolling and obtains titania slurry and seals standby up for safekeeping.
Gained titania slurry automatic screen printing machine is coated on FTO electro-conductive glass, is then calcined at 500 DEG C
30min, obtains titanium dioxide film.
By gained titanium dioxide film ultra-vioket radiation 30 minutes, then with the TiCl of 40 mmol/L4Aqueous solution is soaked at 70 DEG C
Bubble 30 minutes, taking-up water and alcohol flushing, dry for standby.
Again titanium dioxide film is immersed in the Z991 dye solutions that concentration is 0.3mmol/L, soak time is 48 hours,
Prepared dye-sensitized solar cell anode, is then assembled into DSSC, and electrolyte used is Z960.
Embodiment 5
According to mass ratio 1 in 80 DEG C of water-baths:8 are dissolved into ethyl cellulose in terpineol, magnetic agitation mix homogeneously
Prepared organic carrier.
Take the organic carrier that 5g titania powder P25 and 20g prepare to be put in ball grinder, add 0. 5ml pure water
With 1ml glacial acetic acid, by this mixture ball milling 24 hours, rotating speed was 500rpm/sec, is transferred to three roll machine rolling and obtains titanium dioxide
Titanium slurry seals standby up for safekeeping.
Gained titania slurry automatic screen printing machine is coated on FTO electro-conductive glass, is then calcined at 500 DEG C
30min, obtains titanium dioxide film.
By gained titanium dioxide film ultra-vioket radiation 30 minutes, then with the TiCl of 40 mmol/L4Aqueous solution is soaked at 70 DEG C
Bubble 30 minutes, taking-up water and alcohol flushing, dry for standby.
Again titanium dioxide film is immersed in the Z991 dye solutions that concentration is 0.3mmol/L, soak time is 48 hours,
Prepared dye-sensitized solar cell anode, is then assembled into DSSC, and electrolyte used is Z960.
Comparative example 1
According to mass ratio 1 in 80 DEG C of water-baths:8 are dissolved into ethyl cellulose in terpineol, magnetic agitation mix homogeneously
Prepared organic carrier.
Take 5g titania powder ST21(Japanese stone is former)It is put in ball grinder with the organic carrier that 20g is prepared, ball milling
24 hours, rotating speed was 500rpm/sec, is transferred to three roll machine rolling and obtains titania slurry and seals standby up for safekeeping.
Gained titania slurry automatic screen printing machine is coated on FTO electro-conductive glass, is then calcined at 500 DEG C
30min, obtains titanium dioxide film.
By gained titanium dioxide film ultra-vioket radiation 30 minutes, then with the TiCl of 40 mmol/L4Aqueous solution is soaked at 70 DEG C
Bubble 30 minutes, taking-up water and alcohol flushing, dry for standby.
Again titanium dioxide film is immersed in the Z991 dye solutions that concentration is 0.3mmol/L, soak time is 48 hours,
Prepared dye-sensitized solar cell anode, is then assembled into DSSC, and electrolyte used is Z960.
Comparative example 2
According to mass ratio 1 in 80 DEG C of water-baths:8 are dissolved into ethyl cellulose in terpineol, magnetic agitation mix homogeneously
Prepared organic carrier.
Take the organic carrier that 5g titania powder P25 and 20g prepare to be put in ball grinder, ball milling 24 hours, rotating speed
For 500rpm/sec, it is transferred to three roll machine rolling and obtains titania slurry and seal standby up for safekeeping.
Gained titania slurry automatic screen printing machine is coated on FTO electro-conductive glass, is then calcined at 500 DEG C
30min, obtains titanium dioxide film.
By gained titanium dioxide film ultra-vioket radiation 30 minutes, then with the TiCl of 40 mmol/L4Aqueous solution is soaked at 70 DEG C
Bubble 30 minutes, taking-up water and alcohol flushing, dry for standby.
Again titanium dioxide film is immersed in the Z991 dye solutions that concentration is 0.3mmol/L, soak time is 48 hours,
Prepared dye-sensitized solar cell anode, is then assembled into DSSC, and electrolyte used is Z960.
As 3D and scanning electron microscopic observation embodiment 1 and dye-sensitized solar cell anode obtained by comparative example 1, as a result
As illustrated in fig. 1 and 2, by obtained in method provided by the present invention, ST21 titanium dioxide photoelectrodes film is more uniform, titanium dioxide
Nano-particle is scattered more uniform.
The light transmission rate of detection 1 gained dye-sensitized solar cell anode of embodiment, as shown in figure 3,1 institute of embodiment
Obtain ST21 titanium dioxide photoelectrode light transmission rates and be much higher than the optoelectronic pole obtained by comparative example 1.
Embodiment 4 ~ 5 and dye-sensitized solar cell anode obtained by comparative example 2 are observed as 3D, as a result such as Fig. 4 institutes
Show, scanning electron microscopic observation embodiment 5 and 2 gained dye-sensitized solar cell anode result of comparative example are as shown in figure 5, by this
, without cracking phenomena, membrane granule good dispersion, film surface are equal for P25 titanium dioxide photoelectrodes film obtained in the provided method of invention
It is even.
The performance of detection 1 ~ 2 gained DSSC of embodiment 1 ~ 5 and comparative example, as a result as shown in table 1, by
Obtained in method provided by the present invention, the battery performance of optoelectronic pole is improved, the photoelectricity of optoelectronic pole obtained by the inventive method
Conversion efficiency is up to more than 8.5%, and the photoelectric transformation efficiency of optoelectronic pole by obtained in common law only has 8.1-8.2%.
The DSSC characterization result of 1 embodiment 1 ~ 5 of table and comparative example 1 ~ 2
* thickness is the thickness of titanium dioxide film in DSSC optoelectronic pole.
Above the specific embodiment of the present invention is described in detail, but which has been intended only as example, the present invention has not been limited
It is formed on particular embodiments described above.To those skilled in the art, any equivalent modifications carried out by the present invention and
Replacement is also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Modification, should all cover within the scope of the invention.
Claims (12)
1. a kind of method that titanium dioxide prepares dye-sensitized solar cell anode, it is characterised in that including following step
Suddenly:
Titanic oxide material, organic carrier and additive ball milling mixing are obtained titania slurry, wherein titanium dioxide by step 1
The weight ratio of titanium material and organic carrier is 1:(4~6), the weight of additive are the gross weight of titanic oxide material and organic carrier
The 0.1%~4.4% of amount;
Step 2, carries out cleaning treatment to FTO electro-conductive glass, by step 1 gained titania slurry coating FTO after treatment
On electro-conductive glass, calcining obtains titanium dioxide film;
Step 3, the titanium dioxide film that step 2 is obtained is dipped in Z991 dye solutions, and taking-up obtains dye sensitization of solar
Battery light anode.
2. method according to claim 1, it is characterised in that the additive at least includes for dispersant, improves film and open
The combination of the dressing agent for splitting or both.
3. method according to claim 2, it is characterised in that the dispersant in ethylene glycol, tween, Span
Plant or various.
4. method according to claim 2, it is characterised in that the dressing agent is selected from containing carboxyl, hydroxyl or its combination
One or more in compound.
5. the method according to claim 2 or 4, it is characterised in that the dressing agent selected from methanol, ethanol, ethylene glycol, third
Alcohol, isopropanol, Propylene Glycol, the tert-butyl alcohol, glycerol, butanediol, pentanediol, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol list
One or more in butyl ether, formic acid, acetic acid, ethanedioic acid, trifluoroacetic acid, trifluoroethanol, hexafluoroisopropanol.
6. method according to claim 1, it is characterised in that organic carrier described in step 1 is ethyl cellulose and pine
The mass ratio of the mixture of oleyl alcohol, wherein ethyl cellulose and terpineol is 1:5~1:10.
7. method according to claim 6, it is characterised in that ethyl cellulose is dissolved in 60~100 DEG C of water-baths
In terpineol, mix homogeneously is obtained the organic carrier.
8. method according to claim 1, it is characterised in that ball milling speed is 400~600rpm/sec in step 1, ball
Consume time as 10~24 hours.
9. method according to claim 1, it is characterised in that calcining heat is 400~600 degree in step 2, calcination time
For 10~60min.
10. method according to claim 1, it is characterised in that step 2 gained titanium dioxide film is processed carrying out step 3
It is front first to carry out TiCl4Process.
11. methods according to claim 10, it is characterised in that the TiCl4It is processed as:By step 2 gained titanium dioxide
Film is immersed in 10~80mmol/L TiCl4In solution, soaking temperature is 10~90 DEG C, and soak time is 1min~100h.
12. methods according to claim 1, it is characterised in that in step 3, the Z991 dyes concentrations are
0.001mmol/L~3mol/L, soak time are 2~100h.
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CN101699588A (en) * | 2009-10-30 | 2010-04-28 | 彩虹集团公司 | Method for preparing titanium dioxide slurry for dye-sensitized solar cell |
CN101783245A (en) * | 2009-12-21 | 2010-07-21 | 新奥科技发展有限公司 | Titanium dioxide film with macroporous structure and preparation method thereof |
CN102153138A (en) * | 2010-11-02 | 2011-08-17 | 中山大学 | Graded titanium dioxide microspheres consisting of nano rods and nano granules |
CN102290257A (en) * | 2011-05-19 | 2011-12-21 | 内蒙古大学 | Method for preparing dye sensitized solar cell with selective light transmission |
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CN101699588A (en) * | 2009-10-30 | 2010-04-28 | 彩虹集团公司 | Method for preparing titanium dioxide slurry for dye-sensitized solar cell |
CN101783245A (en) * | 2009-12-21 | 2010-07-21 | 新奥科技发展有限公司 | Titanium dioxide film with macroporous structure and preparation method thereof |
CN102153138A (en) * | 2010-11-02 | 2011-08-17 | 中山大学 | Graded titanium dioxide microspheres consisting of nano rods and nano granules |
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