CN101567268A - Method for preparing ternary two-layer titanium dioxide film - Google Patents
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Abstract
The invention belongs to the technical field of solar batteries, and in particular relates to a method for preparing a multi-layer titanium dioxide film, which comprises the following steps: 1) adding ethyl cellulose into terpineol, and stirring the mixture in a water bath to form an organic carrier; 2) taking titanium dioxide powder and P25 titanium dioxide powder, adding the powder into the organic carrier prepared in the step 1) in proportion, and mixing and grinding the mixture to form first organic carrier slurry; 3) taking the titanium dioxide powder and the P25 titanium dioxide powder, adding the powder into the prepared organic carrier according to a proportion of 1:1-3:1, and grinding the mixture to form second organic carrier slurry; 4) performing screen printing on a conductive surface of conductive glass which is cleaned and dried, printing the first organic carrier slurry, and performing leveling drying; and 5) performing annealing treatment to obtain a ternary two-layer titanium dioxide film. The method enhances the absorption of sunlight by a light anode, and the combination of ternary particles and a two-layer film greatly improves the efficiency of the solar batteries.
Description
Technical field
The invention belongs to technical field of solar batteries, relate to a kind of preparation method of multilayer titanium dioxide film.
Background technology
Along with the aggravation of global energy crisis and problem of environmental pollution, how to utilize cleaning, solar energy resources pollution-free, that not limited by geographical environment to become worldwide research focus.In various novel solar batteries, DSSC with its tool theoretical conversion efficient height, technology is simple, transparency good, to temperature and incident angle of light rely on little, preparation process power consumption less, numerous advantages such as cost is low, more and more be subjected to extensive attention.
In each structure of DSSC was formed, porous light anode was its skeleton part, and it is not only the support and the absorption carrier of dye molecule, also was the transport vehicle of electronics simultaneously.Parameters such as the porosity of photo-anode film, aperture, thickness, crystal orientation, directly influence the adsorbance of dyestuff in the DSSC, influence the transmission of electronics, and have influence on the right effective transmission of OR electricity in the electrolyte from dyestuff excitation state to conductive substrates.Thereby the characteristic of porous photo-anode film has very crucial influence to the DSSC performance, can realize that the controllable microstructure of nanocrystalline porous film and the optimization of nanostructure are the important channels of improving efficiency of dye-sensitized solar battery.
The oxide semiconductor material that the porous photo-anode film is commonly used is a nano-crystalline titanium dioxide, preparation method commonly used is deployed into slurry with the P25 type titanium dioxide granule of particle diameter 20-30nm, vapor phase method preparation, make it form rete by methods such as spraying, spin coating, coating or printings, be interconnected to constitute the porous network structure titanium dioxide film behind the sintering between particle.This perforated membrane has bigger specific area, helps increasing the adsorbance of dyestuff, reaches the purpose that fully absorbs solar energy.
Studies show that TiO 2 particles except that advantage such as stable performance, corrosion resistance be good, also has stronger light scattering effect.The specific area of nano-crystal thin-film is all directly relevant with the TiO 2 particles size with light scattering property: the small-particle of titanium dioxide helps increasing the specific area of film, but light scattering property is poor; The macroparticle of titanium dioxide has stronger light scattering property but reduces specific area.Therefore the nano-crystal titanium dioxide particle of small particle diameter can be combined with the titanium dioxide powder of big particle diameter, small particle diameter nano-crystal titanium dioxide particle satisfies the requirement of the high-specific surface area of DSSC requirement, big particle diameter particle can improve the repeatedly scattering effect in the film, increase the distance of photon in porous network, increase the probability that dye molecule absorbs photon, the luminous energy absorption efficiency is further improved, particularly improve the luminous energy absorption efficiency of dye molecule in the long-wavelength region, this can increase the output of photoelectric current greatly, improves photoelectric conversion efficiency.
Summary of the invention
Small-particle light scattering property at titanium dioxide in the prior art is poor; The macroparticle of titanium dioxide reduces the technical problem of specific area, the present invention proposes a kind of preparation method of ternary two-layer titanium dioxide film, comprises the steps:
1) preparation organic carrier: 1 part of ethyl cellulose is slowly joined in 9 parts of terpinols 60 ℃ of-80 ℃ of stirring in water bath 1-2h, the organic carrier of formation viscosity 5.9KcP in 1: 9 ratio of mass ratio;
2) press mass fraction, the titanium dioxide powder of the P25 that titanium dioxide powder that to get 9 parts of powder diameters be 5nm-15nm and 9-27 purchase especially, according to 1: 1-1: 3 ratio adds the organic carrier of 82-64 part step 1) preparation, abundant mixed grinding 1h, form the first organic carrier system slurry, the titania powder mass percentage content is 18-36% in the slurry;
3) press mass fraction, getting 9-27 part powder diameter is the titanium dioxide powder of 100nm-500nm and the titanium dioxide powder of 9 parts of P25, according to 1: 1-3: 1 ratio, the organic carrier that adds the preparation of 82-64 part step 1), abundant mixed grinding 1h, form the second organic carrier system slurry, the titania powder mass percentage content is 18-36% in the slurry;
4) clean up and the dry electro-conductive glass conducting surface of crossing on use silk screen printing, print the first organic carrier system slurry, to print the electro-conductive glass of ground floor titanium dioxide film at 80 ℃ of dry 15min of following levelling, repeat above-mentioned printing process after the drying, form second layer titanium dioxide film, same 80 ℃ of following levelling dryings;
5) put into Muffle furnace and anneal, with the speed intensification of 5 ℃/min, 375 ℃ of insulation 15min, 450 ℃ of insulation 15min, 500 ℃ of insulation 15min, slow cooling in the stove obtains ternary two-layer titanium dioxide film in the air atmosphere.
Beneficial effect of the present invention is:
Use the ground floor titanium dioxide film of 5nm-15nm small particle diameter titanium dioxide and the blend of 20-30nmP25 titanium dioxide powder preparation, have bigger specific surface; Use the second layer titanium dioxide film of 20-30nmP25 and 100-500nm blend preparation to make battery have stronger light scattering property, strengthened of the absorption of light anode sunlight.The combination of three elementary particles and duplicature is greatly improved the efficient of DSSC.Technology of the present invention is simple, can be used for large tracts of land production, for the industrialization production of DSSC provides technical support.
Description of drawings
Fig. 1 DSSC battery of the present invention V-P performance such as Fig. 1 curve.
The V-P performance curve 0 of the DSSC of general P25 powder preparing;
The V-P performance curve 1 of the DSSC of embodiment 1;
The V-P performance curve 2 of the DSSC of embodiment 2;
The V-P performance curve 3 of the DSSC of embodiment 3.
Embodiment:
Below in conjunction with concrete embodiment technical scheme of the present invention is described further.
Embodiment 1:
1) 40g ethyl cellulose EC7 is slowly joined in the 360g terpinol in 1: 9 ratio of mass ratio, 60 ℃ of stirring in water bath 2h, the organic carrier of formation viscosity 5.9KcP, standby.
2) get the titanium dioxide powder that the 0.9g particle diameter is 5nm, 0.9g the titanium dioxide powder of P25 of outsourcing, promptly 1: 1 ratio, the organic carrier that adds the preparation of 8.2g step 1), abundant mixed grinding 1h, form the first organic carrier system slurry, the titania powder mass percentage content is 18% in the slurry.
3) get the titanium dioxide powder that the 2.7g powder diameter is 100nm, 0.9g the titanium dioxide powder of the P25 of outsourcing, promptly 3: 1 ratio, the organic carrier that adds the preparation of 6.4g step 1), abundant mixed grinding 1h, form the second organic carrier system slurry, the titania powder mass percentage content is 36% in the slurry.
4) clean up and the dry electro-conductive glass conducting surface of crossing on use silk screen printing, print the first organic carrier system slurry, to print the electro-conductive glass of ground floor titanium dioxide film at 80 ℃ of dry 15min of following levelling, repeat above-mentioned printing process after the drying, form second layer titanium dioxide film, same 80 ℃ of following levelling dryings.
5) put into Muffle furnace and anneal, with the speed intensification of 5 ℃/min, 375 ℃ of insulation 15min, 450 ℃ of insulation 15min, 500 ℃ of insulation 15min, slow cooling in the stove obtains ternary two-layer titanium dioxide film, thickness 17 μ m, effective area 2 * 0.8cm in the air atmosphere
2
Embodiment 2:
1) 40g ethyl cellulose EC7 is slowly joined in the 360g terpinol in 1: 9 ratio of mass ratio, 80 ℃ of stirring in water bath 1h, the organic carrier of formation viscosity 5.9KcP, standby.
2) get the titanium dioxide powder of the P25 of the titanium dioxide powder of 1.0g particle diameter 11nm and 1.5g outsourcing, promptly 1: 1.5 ratio, the organic carrier that adds the preparation of 7.5g step 1), abundant mixed grinding 1h, form the first organic carrier system slurry, the titania powder mass percentage content is 25% in the slurry.
3) get the titanium dioxide powder of the P25 of the titanium dioxide powder of 1.5g particle diameter 300nm and 1.0g outsourcing, promptly 1.5: 1 ratio, the organic carrier that adds the preparation of 7.5g step 1), abundant mixed grinding 1h, form the second organic carrier system slurry, the titania powder mass percentage content is 25% in the slurry.
4) clean up and the dry electro-conductive glass conducting surface of crossing on use silk screen printing, print the first organic carrier system slurry, to print the electro-conductive glass of ground floor titanium dioxide film at 80 ℃ of dry 15min of following levelling, repeat above-mentioned printing process after the drying, form second layer titanium dioxide film, same 80 ℃ of following levelling dryings.
5) put into Muffle furnace and anneal, with the speed intensification of 5 ℃/min, 375 ℃ of insulation 15min, 450 ℃ of insulation 15min, 500 ℃ of insulation 15min, slow cooling in the stove obtains ternary two-layer titanium dioxide film, thickness 15 μ m, effective area 2 * 0.8cm in the air atmosphere
2Battery V-P performance is shown in Fig. 1 curve 2.
Embodiment 3:
1) 40g ethyl cellulose EC7 is slowly joined in the 360g terpinol in 1: 9 ratio of mass ratio, 70 ℃ of stirring in water bath 1.5h, the organic carrier of formation viscosity 5.9KcP, standby.
2) get the titanium dioxide powder of the P25 of the titanium dioxide powder of 0.9g particle diameter 15nm and 2.7g outsourcing, promptly 1: 3 ratio, the organic carrier that adds the preparation of 6.4g step 1), abundant mixed grinding 1h, form the first organic carrier system slurry, the titania powder mass percentage content is 36% in the slurry.
3) get the titanium dioxide powder of the P25 of the titanium dioxide powder of 0.9g particle diameter 500nm and 2.7g outsourcing, promptly 1: 1 ratio, the organic carrier that adds the preparation of 8.2g step 1), abundant mixed grinding 1h, form the second organic carrier system slurry, the titania powder mass percentage content is 18% in the slurry.
4) clean up and the dry electro-conductive glass conducting surface of crossing on use silk screen printing, print the first organic carrier system slurry, to print the electro-conductive glass of ground floor titanium dioxide film at 80 ℃ of dry 15min of following levelling, repeat above-mentioned printing process after the drying, form second layer titanium dioxide film, same 80 ℃ of following levelling dryings.
5) put into Muffle furnace and anneal, with the speed intensification of 5 ℃/min, 375 ℃ of insulation 15min, 450 ℃ of insulation 15min, 500 ℃ of insulation 15min, slow cooling in the stove obtains ternary two-layer titanium dioxide film, thickness 16 μ m, effective area 2 * 0.8cm2 in the air atmosphere.Battery V-P performance is shown in Fig. 1 curve 3.
The two-layer titanium dioxide film of the present invention's preparation has carried out sintering twice, promptly print first organic ink, sintering forms the ground floor titanium dioxide film, after naturally cooling to room temperature, sintering again after republishing second organic ink on the ground floor titanium dioxide film, promptly form used ternary two-layer titanium dioxide film behind the natural cooling, twice sintering temperature and heating rate are identical.
For the present invention, also can directly after two-layer titanium dioxide film printing, carry out sintering, perhaps after ground floor titanium dioxide film drying, republish second layer titanium dioxide film → drying → two kinds of methods of sintering and select to use according to the actual conditions of producing.
Other each several part parameter and test condition when ternary two-layer titanium dioxide film is assembled into device:
I, Pt electrode are the Pt black electrode of pyrolysis chloroplatinic acid preparation, and dyestuff is the N719 of 0.3mmol/L, and redox electrolytes liquid proportioning is: in acetonitrile solvent, and 0.05mol/L I
2, 0.1mol/L LiI, 0.4mol/L TBP.
Ii, test condition: Oriel solar simulator, simulation AM1.5, exposure light power 1000W/m
2Use the photoelectric characteristic of Keithley data source table test battery down.
From the battery V-P performance chart of test result as can be seen, use the DSSC of this patent ternary two-layer titanium dioxide film preparation, ratio improves a lot with the power output of the DSSC of general P25 powder preparing, and the unit are peak power output is by 2.61mW/cm
2Be increased to 3.21mW/cm respectively
2, 2.93mW/cm
2, 3.06mW/cm
2Thereby, make photoelectric conversion efficiency that the lifting of 12%-23% be arranged.
Claims (4)
1. the preparation method of a ternary two-layer titanium dioxide film is characterized in that, comprises the steps:
1) preparation organic carrier: 1 part of ethyl cellulose is slowly joined in 9 parts of terpinols 60 ℃ of-80 ℃ of stirring in water bath 1-2h, the organic carrier of formation viscosity 5.9KcP in 1: 9 ratio of mass ratio;
2) press mass fraction, titanium dioxide powder that to get 9 parts of powder diameters be 5nm-15nm and the titanium dioxide powder of 9-27 part P25, according to 1: 1-1: 3 ratio adds the organic carrier of 82-64 part step 1) preparation, abundant mixed grinding 1h, form the first organic carrier system slurry, the titania powder mass percentage content is 18-36% in the slurry;
3) press mass fraction, getting 9-27 part powder diameter is the titanium dioxide powder of 100nm-500nm and the titanium dioxide powder of 9 parts of P25, according to 1: 1-3: 1 ratio, the organic carrier that adds the preparation of 82-64 part step 1), abundant mixed grinding 1h, form the second organic carrier system slurry, the titania powder mass percentage content is 18-36% in the slurry;
4) clean up and the dry electro-conductive glass conducting surface of crossing on use silk screen printing, print the first organic carrier system slurry, to print the electro-conductive glass of ground floor titanium dioxide film at 80 ℃ of dry 15min of following levelling, repeat above-mentioned printing process after the drying, form second layer titanium dioxide film, same 80 ℃ of following levelling dryings;
5) put into Muffle furnace and anneal, with the speed intensification of 5 ℃/min, 375 ℃ of insulation 15min, 450 ℃ of insulation 15min, 500 ℃ of insulation 15min, slow cooling in the stove obtains ternary two-layer titanium dioxide film in the air atmosphere.
2. the preparation method of ternary two-layer titanium dioxide film according to claim 1 is characterized in that, comprises the steps:
1) preparation organic carrier: 1 part of ethyl cellulose EC7 is slowly joined in 9 parts of terpinols 60 ℃ of stirring in water bath 2h, the organic carrier of formation viscosity 5.9KcP in 1: 9 ratio of mass ratio;
2) press mass fraction, the titanium dioxide powder that to get 9 parts of powder diameters be 5nm, the titanium dioxide powder of 9 parts of P25, ratio according to 1: 1, the organic carrier that adds 82 parts of step 1) preparations, fully mixed grinding 1h forms the first organic carrier system slurry, and the titania powder mass percentage content is 18% in the slurry;
3) press mass fraction, the titanium dioxide powder that to get 27 parts of powder diameters be 100nm, the titanium dioxide powder of 9 parts P25, ratio according to 3: 1, the organic carrier that adds 64 parts of step 1) preparations, fully mixed grinding 1h forms the second organic carrier system slurry, and the titania powder mass percentage content is 36% in the slurry;
4) clean up and the dry electro-conductive glass conducting surface of crossing on use silk screen printing, print the first organic carrier system slurry, to print the electro-conductive glass of ground floor titanium dioxide film at 80 ℃ of dry 15min of following levelling, repeat above-mentioned printing process after the drying, form second layer titanium dioxide film, same 80 ℃ of following levelling dryings;
5) put into Muffle furnace and anneal, with the speed intensification of 5 ℃/min, 375 ℃ of insulation 15min, 450 ℃ of insulation 15min, 500 ℃ of insulation 15min, slow cooling in the stove obtains ternary two-layer titanium dioxide film in the air atmosphere.
3. the preparation method of ternary two-layer titanium dioxide film according to claim 1 is characterized in that, comprises the steps:
1) preparation organic carrier: 1 part of ethyl cellulose is slowly joined in 9 parts of terpinols 80 ℃ of stirring in water bath 1h, the organic carrier of formation viscosity 5.9KcP in 1: 9 ratio of mass ratio;
2) press mass fraction, the titanium dioxide powder that to get 10 parts of powder diameters be 11nm, the titanium dioxide powder of 15 parts of P25, ratio according to 1: 1.5, the organic carrier that adds 75 parts of step 1) preparations, fully mixed grinding 1h forms the first organic carrier system slurry, and the titania powder mass percentage content is 25% in the slurry;
3) press mass fraction, the titanium dioxide powder that to get 15 parts of powder diameters be 300nm, the titanium dioxide powder of 10 parts P25, ratio according to 1.5: 1, the organic carrier that adds 75 parts of step 1) preparations, fully mixed grinding 1h forms the second organic carrier system slurry, and the titania powder mass percentage content is 25% in the slurry;
4) clean up and the dry electro-conductive glass conducting surface of crossing on use silk screen printing, print the first organic carrier system slurry, to print the electro-conductive glass of ground floor titanium dioxide film at 80 ℃ of dry 15min of following levelling, repeat above-mentioned printing process after the drying, form second layer titanium dioxide film, same 80 ℃ of following levelling dryings;
5) put into Muffle furnace and anneal, with the speed intensification of 5 ℃/min, 375 ℃ of insulation 15min, 450 ℃ of insulation 15min, 500 ℃ of insulation 15min, slow cooling in the stove obtains ternary two-layer titanium dioxide film in the air atmosphere.
4. the preparation method of ternary two-layer titanium dioxide film according to claim 1 is characterized in that, comprises the steps:
1) preparation organic carrier: 1 part of ethyl cellulose is slowly joined in 9 parts of terpinols 70 ℃ of stirring in water bath 1.5h, the organic carrier of formation viscosity 5.9KcP in 1: 9 ratio of mass ratio;
2) press mass fraction, the titanium dioxide powder that to get 9 parts of powder diameters be 15nm, the titanium dioxide powder of 27 parts of P25, ratio according to 1: 3, the organic carrier that adds 64 parts of step 1) preparations, fully mixed grinding 1h forms the first organic carrier system slurry, and the titania powder mass percentage content is 36% in the slurry;
3) press mass fraction, the titanium dioxide powder that to get 9 parts of powder diameters be 500nm, the titanium dioxide powder of 9 parts of P25, ratio according to 1: 1, the organic carrier that adds 82 parts of step 1) preparations, fully mixed grinding 1h forms the second organic carrier system slurry, and the titania powder mass percentage content is 18% in the slurry;
4) clean up and the dry electro-conductive glass conducting surface of crossing on use silk screen printing, print the first organic carrier system slurry, to print the electro-conductive glass of ground floor titanium dioxide film at 80 ℃ of dry 15min of following levelling, repeat above-mentioned printing process after the drying, form second layer titanium dioxide film, same 80 ℃ of following levelling dryings;
5) put into Muffle furnace and anneal, with the speed intensification of 5 ℃/min, 375 ℃ of insulation 15min, 450 ℃ of insulation 15min, 500 ℃ of insulation 15min, slow cooling in the stove obtains ternary two-layer titanium dioxide film in the air atmosphere.
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| CN102602989A (en) * | 2012-03-21 | 2012-07-25 | 奇瑞汽车股份有限公司 | Titanium dioxide as well as preparation method thereof, slurry material of solar battery as well as preparation method thereof and solar battery |
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