KR101787529B1 - Manufacturing method of low temperature sintered titanium dioxide paste for fabricating photo-electrodes of dye sensitized solar cell, titanium dioxide paste manufactured thereby and fabricating photo-electrodes of dye sensitized solar cell using the titanium dioxide paste - Google Patents
Manufacturing method of low temperature sintered titanium dioxide paste for fabricating photo-electrodes of dye sensitized solar cell, titanium dioxide paste manufactured thereby and fabricating photo-electrodes of dye sensitized solar cell using the titanium dioxide paste Download PDFInfo
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- KR101787529B1 KR101787529B1 KR1020140148339A KR20140148339A KR101787529B1 KR 101787529 B1 KR101787529 B1 KR 101787529B1 KR 1020140148339 A KR1020140148339 A KR 1020140148339A KR 20140148339 A KR20140148339 A KR 20140148339A KR 101787529 B1 KR101787529 B1 KR 101787529B1
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- Y02E10/542—Dye sensitized solar cells
Abstract
A method of manufacturing a titanium dioxide paste for a dye-sensitized solar cell photo-electrode can be provided. Specifically, the present invention relates to a method for producing a titanium dioxide colloid solution by hydrothermally synthesizing an acidic solution, a solvent, and a titanium dioxide precursor to form a titanium dioxide colloid solution, dispersing the titanium dioxide colloid solution by ultrasonic waves and concentrating the titanium dioxide colloid solution with a titanium dioxide slurry, Adding an aqueous ammonia solution to form a titanium dioxide paste, wherein the aqueous ammonia solution is added in an amount of 0.015 to 0.020 part by weight based on the titanium dioxide slurry. Can be provided. Thus, the titanium dioxide paste for a photo-electrode for a dye-sensitized solar cell of the present invention can have a high viscosity characteristic without a binder, and can form a photo-electrode thin film layer having a desired thickness. In addition, the titanium dioxide paste for a photo-electrode of the dye-sensitized solar cell of the present invention can be sintered even at a low temperature (150 ° C or less) and can be easily formed on a flexible substrate.
Description
The present invention relates to a method for producing a titanium dioxide (TiO 2 ) paste, and more particularly, to a method for producing a titanium dioxide paste for dye-sensitized solar cell photoelectrode capable of sintering at a low temperature, a titanium dioxide paste, And a method of manufacturing a dye-sensitized solar cell optical electrode using the titanium dioxide paste.
The dye-sensitized solar cell is a clean technology that transforms light energy into electrical energy through dye molecules coated on nanoparticles by applying the principle that plants convert solar energy into electrons flow through photosynthesis. Specifically, the structure of the dye-sensitized solar cell is mainly composed of a photoelectrode containing titanium dioxide on which a dye is adsorbed on a substrate coated with a thin film of fluorine-doped tin oxide (FTO) The catalytic metal layer on which the catalytic platinum (Pt) is deposited faces each other, and the inside is filled with the electrolyte. Generally, the titanium dioxide forming the photo-electrode is used in the form of a paste, and the material forming the paste may be composed of titanium dioxide, a binder and a solvent having a size of several tens nanoparticles. The binder is mainly composed of a polymer, and a thick photoelectrode thin film can be formed in order to impart viscosity to facilitate coating. Since the dye that generates electrons is adsorbed on the photoelectrode thin film, the thicker the photoelectrode, the more dye can be adsorbed and the more current can be generated. In addition, the polymer used as the binder included in the paste plays an important role in forming a mesoporous titanium dioxide thin film while the polymer is burnt through heat treatment at 400 ° C or higher, as well as improving adhesion with a conductive substrate .
Such a titanium dioxide paste is mainly made of a photoelectrode of a dye-sensitized solar cell based on an FTO glass substrate, and is difficult to apply to a flexible substrate which deforms at a temperature exceeding 150 ° C. To solve this problem, it is necessary to develop a titanium dioxide paste that does not use a binder. However, it is not easy to generate the viscosity of the titanium dioxide paste unless a binder is used, and it is difficult to form the thickness of the photoelectrode thin film thickly, which lowers energy conversion efficiency.
SUMMARY OF THE INVENTION It is an object of the present invention to provide a method of manufacturing a titanium dioxide paste which can form a photoelectrode thin film having a large thickness without using a binder.
According to an aspect of the present invention, there is provided a method for preparing a titanium dioxide colloid solution, comprising the steps of: hydrothermally reacting a mixed solution containing an acidic solution, a solvent, and a titanium dioxide precursor to form a titanium dioxide colloid solution; Titanium slurry; and adding an aqueous ammonia solution to the titanium dioxide slurry to form a titanium dioxide paste, wherein the aqueous ammonia solution comprises 0.015 part by weight to 0.020 parts by weight, based on 100 parts by weight of the titanium dioxide slurry, By weight based on the total weight of the dye-sensitized solar cell.
The solvent may be water, an alcohol, or a mixture thereof.
The titanium dioxide precursor may be at least one selected from the group consisting of titanium isopropoxide, titanium tetraisopropoxide, titanium methoxide, titanium ethoxide, titanium butoxide, titanium tertiary butoxide, titanium tetra butoxide, and titanium ethylhexoside And at least one selected from the group consisting of
The acid solution may be added in an amount of 1M to 10M and at least one selected from acetic acid, sulfuric acid, phosphoric acid, nitric acid and hydrochloric acid may be used.
According to another aspect of the present invention, there is provided a titanium dioxide paste for a photo-electrode for a dye-sensitized solar cell, which is produced through the above-described method for producing a titanium dioxide paste for a photo-electrode for a dye-sensitized solar cell.
The concentration of titanium dioxide contained in the titanium dioxide paste may be 15 wt% to 25 wt%.
According to another aspect of the present invention, there is provided a method for producing a titanium dioxide thin film, comprising the steps of: coating the substrate with the titanium dioxide paste; drying the coated titanium dioxide paste at 100 to 200 DEG C to form a titanium dioxide thin film layer; The method comprising the steps of: (a) forming a dye-sensitized solar cell;
In the step of forming the titanium dioxide thin film layer by drying the coated titanium dioxide paste at 100 ° C. to 200 ° C., the thickness of the titanium dioxide thin film layer may be 4 μm to 12 μm.
The titanium dioxide paste for a photo-electrode of the dye-sensitized solar cell of the present invention can have a high viscosity characteristic without a binder, and can form a photo-electrode thin film layer having a desired thickness.
In addition, the titanium dioxide paste for a photo-electrode of the dye-sensitized solar cell of the present invention can be sintered even at a low temperature (150 ° C or less) and can be easily formed on a flexible substrate.
However, the effects of the present invention are not limited to those mentioned above, and other effects not mentioned can be clearly understood by those skilled in the art from the following description.
1 is a flow chart showing a method of manufacturing a titanium dioxide paste for a photoelectrode for a low-temperature sintered dye-sensitized solar cell according to an embodiment of the present invention.
2 is a graph showing an image and a viscosity of the titanium dioxide paste prepared in Example 1 of the present invention.
3 is a chart showing the results of thermogravimetric analysis (TGA) of the titanium dioxide paste prepared in Example 1 of the present invention.
Figs. 4 (a) to 4 (b) are SEM images of the titanium dioxide thin film layer prepared in Example 2 of the present invention, and nitrogen physical adsorption isotherms of titanium dioxide particles.
5 is a chart showing the UV-vis-nIR transmittance of the dye-sensitized solar cell photo-electrode prepared in Example 2 of the present invention.
6 is a graph showing photocurrent density-voltage characteristics of a dye-sensitized solar cell including a photo electrode in which the drying temperature of the titanium dioxide paste is different in Example 3 of the present invention.
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
While the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail. Rather, the intention is not to limit the invention to the particular forms disclosed, but rather, the invention includes all modifications, equivalents and substitutions that are consistent with the spirit of the invention as defined by the claims.
In the drawings, the thicknesses of the layers and regions may be exaggerated or reduced for clarity. Like reference numerals designate like elements throughout the specification.
1 is a flowchart illustrating a method of manufacturing a titanium dioxide paste for a photoelectrode for a low-temperature sintered dye-sensitized solar cell according to an embodiment of the present invention.
Referring to FIG. 1, a titanium dioxide colloid solution may be formed by hydrothermal reaction of a mixed solution containing an acidic solution, a solvent, and a titanium dioxide precursor (S10).
The titanium dioxide colloid solution may be one obtained by dissolving a titanium dioxide precursor in a solvent to provide nano-sized titanium dioxide particles, which is further subjected to a hydrothermal reaction by adding an acidic solution thereto. The hydrothermal reaction can be carried out through a known hydrothermal reaction process, so that it is not particularly limited. In one embodiment of the present invention, the hydrothermal reaction may be carried out using an autoclave for 2 to 12 hours at a temperature range of 200 ° C to 250 ° C.
The solvent may be water, an alcohol, or a mixture thereof. The solvent is for dissolving the titanium dioxide precursor and may be removed through a subsequent drying process. The alcohol may be, for example, methanol, ethanol, propanol, butanol or the like, but is not limited thereto. The solvent may be added in an appropriate amount to dissolve the titanium dioxide, and is not particularly limited.
The titanium dioxide precursor may be at least one selected from the group consisting of titanium isopropoxide, titanium tetraisopropoxide, titanium methoxide, titanium ethoxide, titanium butoxide, titanium tertiary butoxide, titanium tetra butoxide, and titanium ethylhexoside And at least one selected from the group consisting of
The acidic solution may be an acidic substance that is dissociated into the titanium dioxide colloid to generate hydrogen ions. Specifically, the acid solution may be at least one selected from the group consisting of acetic acid, sulfuric acid, phosphoric acid, nitric acid and hydrochloric acid in an amount of about 1M to 10M.
The titanium dioxide colloid solution formed through the hydrothermal reaction may be one containing titanium dioxide nanoparticles synthesized by hydrolysis of the titanium dioxide precursor. The nano-sized titanium dioxide particles may have a small size distribution of about 10 nm to 25 nm.
Before the mixture is dispersed by ultrasonic waves, the mixture may be refluxed and then cooled. This can be carried out through a known reflux process and cooling process, and is not particularly limited.
The titanium dioxide colloid solution may then be dispersed by ultrasonication and concentrated to a titanium dioxide slurry (S20).
Dispersion of the titanium dioxide colloid solution by ultrasonic waves may be for uniformly dispersing the nano-sized titanium dioxide particles contained in the titanium dioxide colloid solution to form a uniform titanium dioxide thin film layer at the time of forming the photoelectrode later. This is not particularly limited because it can be carried out through a known ultrasonic dispersion process. Specifically, it may be performed for 5 to 10 hours at an intensity of 10 kHz to 30 kHz.
An aqueous ammonia solution may be added to the titanium dioxide slurry to form a titanium dioxide paste (S30).
When an aqueous ammonia solution is added to the titanium dioxide slurry, an acid-base reaction may occur between the acidic substance contained in the titanium dioxide slurry and the basic substance of the aqueous ammonia solution. As the acid-base bond is formed in the titanium dioxide paste by the acid-base reaction, the viscosity of the titanium dioxide paste can be changed. That is, the titanium dioxide particles contained in the titanium dioxide paste are agglomerated by acid-base bonding through the acid-base reaction between the acidic substance contained in the titanium dioxide slurry and the basic substance of the aqueous ammonia solution, It can be changed.
Specifically, the aqueous ammonia solution may be added in an amount of 0.015 part by weight to 0.020 part by weight based on 100 parts by weight of the titanium dioxide slurry. By appropriately adding ammonia water within the above range, it is possible to produce the titanium dioxide paste of the present invention having high viscosity characteristics capable of being sintered at a low temperature without a binder.
Another aspect of the present invention provides a titanium dioxide paste for a photo-electrode for a dye-sensitized solar cell, which is produced through the above-described method for producing a titanium dioxide paste for a photo-electrode for a dye-sensitized solar cell.
The titanium dioxide paste can have a high viscosity without addition of a binder in the form of a separate polymer, and includes nanosized titanium dioxide particles. This may be an improvement in the fact that the titanium dioxide paste using a conventional binder is limited in terms of the substrate that can be applied due to the difficulty of applying to a substrate where deformation occurs at a specific temperature (150 DEG C) or higher. That is, the titanium dioxide paste of the present invention can have the effect of easily forming the photoelectrode on various flexible substrates.
The concentration of titanium dioxide contained in the titanium dioxide paste may be 15 wt% to 25 wt%. When the dye-sensitized solar cell photoelectrode is formed using the titanium dioxide paste having the concentration within the above range, the thickness of the photoelectrode thin film can be increased to a desired size, and the energy conversion efficiency can be improved to 3% or more. This can be specifically illustrated by the following examples and drawings.
According to another aspect of the present invention, there is provided a method of manufacturing a dye-sensitized solar cell optical electrode using the titanium dioxide paste for a photo-electrode for a dye-sensitized solar cell. Specifically, 1) a method of manufacturing the dye-sensitized solar cell photoelectrode includes: coating the substrate with the titanium dioxide paste; 2) drying the coated titanium dioxide paste at 100 ° C to 200 ° C to form a titanium dioxide thin film layer And 3) adsorbing the dye to the titanium dioxide layer.
In the step 1), the method of manufacturing the dye-sensitized solar cell photoelectrode may include coating the titanium dioxide paste on the substrate.
The substrate may be a flexible substrate as well as a substrate of a known dye-sensitized solar cell. Specifically, the flexible substrate may be a metal flexible substrate, an ultra-thin glass substrate, or a plastic substrate, but is not limited thereto.
The coating of the titanium dioxide paste for a photo-electrode for a dye-sensitized solar cell of the present invention on the substrate can be carried out through a doctor blade coating, a spin coating, a screen printing or a spraying method, but is not limited thereto.
The step 2) may be a step of drying the coated titanium dioxide paste at 100 ° C to 200 ° C to form a titanium dioxide thin film layer.
That is, when the titanium dioxide paste coated on the substrate is dried at 100 ° C to 200 ° C through the above step 1), a uniform thin film titanium dioxide thin film layer may be formed on the substrate. The method of drying the titanium dioxide paste is not particularly limited as it can use a known paste drying method.
In the step 2), the thickness of the titanium dioxide thin film layer may be 4 to 12 μm. When the titanium dioxide thin film layer is formed to a thickness within the above range, the current amount of the dye-sensitized solar cell including the titanium dioxide thin film layer can be increased to an appropriate range, and the energy conversion efficiency can be improved.
The step 3) may be a step of adsorbing the dye to the titanium dioxide thin film layer. The dye is not particularly limited because it can use all dyes of known dye-sensitized solar cells. The dye may be selected from the group consisting of ruthenium (Ru), platinum (Pt), palladium (Pd), aluminum (Al), iridium (Ir), lead (Pb) composites, natural materials, or perovskite Can be used. Specific examples of the dyes include dyes such as ruthenium complexes. The ruthenium complexes may be, for example, ruthenium 535 dyes, ruthenium 535 bis-TBA dyes, or ruthenium 620-1H3TBA dyes. have.
Thus, the dye-sensitized solar cell including the photo-electrode of the dye-sensitized solar cell manufactured through the method of manufacturing the photo-electrode of the dye-sensitized solar cell can be manufactured. In the dye-sensitized solar cell, the energy conversion efficiency can be improved by the titanium dioxide thin film layer formed using the titanium dioxide paste. Specifically, this will be described later in the following examples and drawings.
[Example]
≪ Example 1: Dye-sensitized solar cell >
(IV) isopropoxide (TTIP), 98%, manufactured by Junsei) and 117 mmol of 2-propanol (2-propanol, 99.5%, Aldrich) , And a solution of 5.33 M of acetic acid (99%, Duksan) was added dropwise thereto and stirred in an ice bath so as to form a white precipitate. It was refluxed at 75 ° C for 3 hours and then cooled at room temperature. Then, hydrothermal synthesis was performed at 230 ° C for about 12 hours using an autoclave to prepare a titanium dioxide colloid solution containing nanocrystalline anatase type titanium dioxide nanoparticles. The colloidal solution was sonicated for about 7 hours and concentrated to a concentration of titanium dioxide of 20 wt% to prepare a titanium dioxide slurry. Ammonia water (NH 4 OH, 28%, Duksan) was added in an amount of about 0.015 part by weight based on 100 parts by weight of the titanium dioxide slurry to prepare a titanium dioxide paste.
2 is a graph showing an image and a viscosity of the titanium dioxide paste prepared in Example 1 of the present invention.
2, it is confirmed that even if a vial containing a titanium dioxide paste is inclined by about 10 ° or placed on a spatula, the titanium dioxide paste keeps a constant shape with almost no flow due to the viscosity of the titanium dioxide paste . The chart of FIG. 2 shows that the viscosity of the titanium dioxide paste was measured with a rotational viscometer (Brookfield viscometer, DV-E, spindle # 64) at 25 ° C. and showed 3.2 × 10 4 cP at a rate of 5 rpm have. As a result, it can be confirmed that the titanium dioxide paste of the present invention has characteristics of high viscosity.
3 is a chart showing the results of thermogravimetric analysis (TGA) of the titanium dioxide paste prepared in Example 1 of the present invention.
Referring to FIG. 3, it can be seen that the weight of the titanium dioxide paste hardly changes at a temperature of 110 ° C. or higher. This may mean that the titanium dioxide paste of the present invention did not use a binder. In addition, it can be confirmed that the content of titanium dioxide in the titanium dioxide paste is about 20 wt%. This may mean that the concentration of the nano-sized titanium dioxide particles contained in the titanium dioxide paste is precisely controlled to a desired concentration through centrifugation.
Example 2: Preparation of dye-sensitized solar cell photoelectrode using titanium dioxide paste [
The titanium dioxide paste prepared in Example 1 was coated on a FTO formed glass substrate (Pilkington) using a doctor blade coating method. Subsequently, the substrate coated with the titanium dioxide paste was divided into three portions and dried at a temperature of 120 ° C, 150 ° C and 180 ° C for about 15 minutes. Then, a titanium dioxide thin film layer having a thickness of about 8 μm was formed on each substrate Respectively.
Subsequently, the substrate on which the dried titanium dioxide thin film layer was formed was immersed in a reactor containing 0.5 mM of N719 (B2 dye, Dyesol) and anhydrous ethanol at a temperature of 40 DEG C for 4 hours to prepare a dye-sensitized solar cell photoelectrode Respectively.
Figs. 4 (a) to 4 (b) are SEM images of the titanium dioxide thin film layer prepared in Example 2 of the present invention, and nitrogen physical adsorption isotherms of titanium dioxide particles.
4 (a) is a SEM image of the titanium dioxide thin film layer dried at 150 ° C. in the specimen of Example 2, and it can be confirmed that the titanium dioxide particles have a spherical shape of about 20 nm in size. Also, it can be seen that the titanium dioxide thin film layer is coated very smoothly without agglomeration lumps through ultrasonic dispersion and agitation. In particular, the SEM image measured at the rightmost, high magnification shows that titanium dioxide particles are well connected without any chemical linking agent between nano-sized titanium dioxide particles. It can be seen that the titanium dioxide paste is dried at 150 ° C and acetic acid is connected between the nano-sized titanium dioxide particles.
Referring to FIG. 4 (b), the adsorption isotherm of the titanium dioxide particles shows a typical IV region curve, and it can be confirmed that the titanium dioxide thin film layer specimen prepared in Example 2 has a porous structure. The specific surface area is about 65.35 m < 2 > g < -1 >.
5 is a chart showing UV-vis-nIR transmittance of a dye-sensitized solar cell photoelectrode including a titanium dioxide thin film layer dried at 150 ° C in Example 2 of the present invention.
5, when the thickness of the titanium dioxide thin film layer was about 8 μm, the average transmittance was 82% in the visible light region (420 nm to 780 nm) as a result of measurement with a UV-vis-nIR spectrophotometer (UV-3600, Shimadzu) As shown in Fig. This may mean that the size of the titanium dioxide particles constituting the titanium dioxide thin film layer is small and uniformly dispersed and coated.
Example 3: Dye-sensitized solar cell using titanium dioxide paste Preparation of dye-sensitized solar cell containing photoelectrode [
Each of the dye-sensitized solar cells including the three kinds of photoelectrodes having different drying temperatures manufactured in Example 2 was prepared. In the preparation, Pt was used as the counter electrode. The electrolyte was prepared by adding 0.6
6 is a graph showing photocurrent density-voltage characteristics of a dye-sensitized solar cell including a photo electrode in which the drying temperature of the titanium dioxide paste is different in Example 3 of the present invention. 6 is specifically shown in Table 1 below.
(fill factor,%)
Referring to FIG. 6 and Table 1, it can be seen that the value of the current greatly increases while the drying temperature is increased from 120 ° C to 150 ° C, and there is no change at the above temperature. It can be seen that the titanium dioxide paste of the present invention exhibits optimum electrical characteristics at an energy conversion efficiency of 3.38% when dried at 150 ° C.
As a result, the titanium dioxide paste of the present invention can be sintered at a low temperature of 150 ° C or lower, and a titanium dioxide thin film layer having a high viscosity can be formed on a variety of flexible substrates without a binder. In addition, as described above, the titanium dioxide paste having the titanium dioxide concentration of 20 wt% can improve the energy conversion efficiency of the dye-sensitized solar cell including the titanium dioxide paste and can be utilized in related fields.
It should be noted that the embodiments of the present invention disclosed in the present specification and drawings are only illustrative of specific examples for the purpose of understanding and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that other modifications based on the technical idea of the present invention are possible in addition to the embodiments disclosed herein.
Claims (8)
Dispersing the titanium dioxide colloid solution by ultrasonic waves and concentrating the titanium dioxide colloid solution with a titanium dioxide slurry; And
Adding an aqueous ammonia solution to the titanium dioxide slurry to form a titanium dioxide paste having a concentration of titanium dioxide of 15 wt% to 25 wt%
Wherein the aqueous ammonia solution is added in an amount of 0.015 part by weight to 0.020 part by weight based on 100 parts by weight of the titanium dioxide slurry.
Wherein the solvent comprises water, an alcohol, or a mixture thereof. The dye-sensitized solar cell according to claim 1, wherein the solvent comprises water, alcohol, or a mixture thereof.
The titanium dioxide precursor may include,
At least one selected from the group consisting of titanium isopropoxide, titanium tetraisopropoxide, titanium methoxide, titanium ethoxide, titanium butoxide, titanium tertiary butoxide, titanium tetra butoxide, and titanium ethylhexoxide Wherein the dye-sensitized solar cell comprises a titanium dioxide paste.
The acid solution is added in an amount of about 1M to 10M,
Wherein the at least one selected from the group consisting of acetic acid, sulfuric acid, phosphoric acid, nitric acid and hydrochloric acid is used.
Drying the coated titanium dioxide paste at 100 ° C to 200 ° C to form a titanium dioxide thin film layer; And
And a step of adsorbing the dye on the titanium dioxide thin film layer.
In the step of drying the coated titanium dioxide paste at 100 ° C to 200 ° C to form a titanium dioxide thin film layer,
Wherein the thickness of the titanium dioxide thin film layer is 4 占 퐉 to 12 占 퐉.
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