CN102522207B - Preparation method for scattering layer of dye-sensitized solar battery - Google Patents
Preparation method for scattering layer of dye-sensitized solar battery Download PDFInfo
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- CN102522207B CN102522207B CN201110401157.1A CN201110401157A CN102522207B CN 102522207 B CN102522207 B CN 102522207B CN 201110401157 A CN201110401157 A CN 201110401157A CN 102522207 B CN102522207 B CN 102522207B
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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
- 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
- Y02E10/549—Organic PV cells
Abstract
The invention relates to a preparation method for a scattering layer of a dye-sensitized solar battery. The preparation method comprises the following steps of: (1) mixing titanium tetrachloride and a salt solution, and then conducting the hydro-thermal reaction on the titanium tetrachloride and the salt solution in a reaction kettle, thus obtaining titanium oxide scattering microspheres; (2) transferring the titanium oxide microspheres into a mortar, adding a pore-forming agent and a solvent in the mortar in sequence, and grinding the mixture for 0.5-3h to obtain uniform slurry; and (3) coating a layer of scattering layer slurry on a small particle base layer of the dye-sensitized solar battery by adopting a screen printing method or a blade coating method, sintering at the temperature of 400 DEG C-500 DEG C, and finally obtaining the scattering layer of the dye-sensitized solar battery. According to the method, the provided process is simple and convenient, the used raw materials are wide in source, a surface active agent does not need to be used, and the cost is low; and due to the provided large-particle scattering layer, the light absorbing capability of the photoanode of the battery is improved, simultaneously, the dye absorbing amount is increased, and the scattering layer has an industrial application prospect.
Description
Technical field
The invention belongs to the preparation field of dye-sensitized solar cell anode, particularly a kind of preparation method of DSSC scattering layer.
Background technology
Swiss Confederation Gao Deng engineering institute (EPFL) in 1991
deng having prepared a kind of novel solar battery that is similar to photosynthesis of plant principle, be called dye sensitized nano crystal salar battery (Dye-Sensitized Solar Cells, DSSCs).Because it is with low cost, raw material wide material sources, preparation technology is simple, electricity conversion is higher, causes the extensive concern of researcher to low-cost solar battery.
Different from silicon solar cell, DSSC is a kind of photochemical cell, it is mainly by nanocrystalline porous film, dyestuff, electrolyte with several parts of electrode are formed, and wherein nano-porous film should play again as the carrier of absorbing dye the effect of transmission light induced electron and become the most crucial parts of DSSC.Common nano-porous film is that the Anatase titanium oxide grain that is 10～30 nanometers by particle diameter is made, the general light transmittance of dye-sensitized solar cell anode of preparing with this little crystal grain is higher, some light directly sees through from battery, does not participate in photoelectric conversion process.Because the light seeing through is not utilized, this battery to catch optical efficiency often not high.
In order to promote the luminous energy power of catching of DSSC, there is researcher to propose to mix bulky grain particle in the little crystal grain of light anode and obtained good effect as scattering center.It is the bulky grain particle of 125～150 nanometers that the people such as Ferber mix 5% particle diameter in the granule of tens nanometers, the good light anode of dispersion effect (Ferber J., et al.Sol.Energy, Mater.Sol.Cells have been obtained, 1998,54,265-275), the people such as Yoon have improved 42% (Yoon J.H. toward the TiOx nano rod that mixes 15% in little crystal grain by the photoelectric conversion efficiency of battery, et al.J.Photochem.Photobio.A, 2006,180,184-188).
Also have researcher the confinement structure of photonic crystal to be incorporated into the light anode of DSSC, they take PS ball as template, titanium oxide are filled in the hole of PS ball, then by sintering, remove template, form the light anode of photon crystal structure.The light anode that the people such as Kwak prepare in this way can effectively improve material sensitization solar battery the absorption of long-wave band visible region (Kwak E.S., et al.Adv.Funct.Mater.2009,19,1093-1099).
But the problem that above two kinds of methods all exist is the ability of the light anode absorbing dye of same thickness after mixing bulky grain or introducing macropore to have declined.In addition, also having a kind of method of catching luminous energy power that promotes light anode that electrode is made to gradient result, is little crystal grain semitransparent layer in the one side of meeting light, the scattering layer that is oarse-grained composition near electrolytical one side.Bulky grain scattering layer has certain diffuse-reflecting power, light scattering can be participated in to photoelectric conversion process in light anode.Such as Hore etc. carried out this respect research (Hore S., et al.Sol.Energy Mater.Sol.Cells, 2006,90,1176-1188).But the people such as Hore bulky grain specific area used is too low, only can scattered light, effectively absorbing dye participates in opto-electronic conversion.The people such as Huang had improved the synthetic method of bulky grain afterwards; prepared a kind of scattering microballoon having compared with high-ratio surface; but the scattering microballoon of gained is Anatase; diffuse-reflecting power is not strong; and loaded down with trivial details process route has limited scale application (Huang F.Z.; et al.Adv.Funct.Mater.2010,20,1301-1305).
In sum, the light absorpting ability of raising battery light anode is to form oarse-grained scattering layer outside the semitransparent layer forming at the little crystal grain of nanometer compared with good method.But the bulky grain at present used logical very low titan oxide particles of specific area, effectively adsorpting dye molecule.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of DSSC scattering layer, the method be take inorganic ti sources as presoma, do not add in the situation of any surfactant, adopt the synthetic bulky grain scattering microballoon of hydro thermal method, process route is easy, has the prospect of commercial application.
The preparation method of a kind of DSSC scattering layer of the present invention, comprising:
(1) under ice-water bath, titanium tetrachloride is added in salting liquid, obtain clear solution; In clear solution, the concentration of titanium tetrachloride is 0.2～0.4M, and the concentration of salting liquid is 2～4M; Clear solution is transferred in reactor and carried out hydro-thermal reaction, and reaction temperature is 100～150 ℃, and temperature retention time is 12～24 hours; Until insulation, finish also after cool to room temperature, to open water heating kettle, by the washing of precipitate obtaining dry, obtain titanium oxide scattering microballoon;
(2) above-mentioned titanium oxide scattering microballoon is transferred in mortar, added successively pore creating material and solvent, grind and within 0.5～3 hour, obtain uniform slurry; Wherein, oarse-grained mass fraction is 10～30%, and the mass fraction of pore creating material is 5～15%;
(3) adopt the method for silk screen printing or blade coating, on the granule basalis of dye-sensitized solar cell anode, apply above-mentioned slurry, 400～500 ℃ of sintering are also incubated 10～30 minutes, obtain DSSC scattering layer.
Salt in described step (1) is villaumite, comprises one or more in lithium chloride, sodium chloride, potassium chloride, calcium chloride, magnesium chloride.
Titanium oxide scattering microballoon in described step (1) is pure rutile phase, and particle diameter is 100～800nm, and specific area is 50～120m
2/ g.
Pore creating material in described step (2) is one or more in polyethylene glycol (200～20000), epoxy resin, cellulose and derivative thereof.
Described cellulose derivative is methylcellulose, ethyl cellulose, hydroxypropyl cellulose or carboxycellulose.
Solvent in described step (2) is one or more in water, alcohols, polyalcohols, terpene.
The thickness of the scattering layer in described step (3) is 1～6 μ m.
Villaumite of the present invention add the ionic strength that has improved solution, by electrostatic screen effect, control bulky grain for comparatively uniform micro-sphere structure, to make nanometer rods be (001) crystal plane direction growth along c-axis in chloride ion selective absorption effect on the other hand, and the microballoon obtaining is all that nanometer rods self assembly forms.Then in the bulky grain scattering microballoon obtaining, add pore creating material and solvent, mixed grinding evenly obtains scattering layer slurry.Method by silk screen printing or blade coating applies bulky grain scattering microballoon on light anode granule basalis, effectively improves the light absorpting ability of light anode, and absorbing dye participation opto-electronic conversion, has finally improved the photoelectric conversion efficiency of DSSC.
beneficial effect
(1) the present invention be take inorganic ti sources as presoma, does not add in the situation of any surfactant, adopts the synthetic bulky grain scattering microballoon of hydro thermal method, and process route is easy, has the prospect of commercial application;
(2) the bulky grain titanium oxide of synthesized of the present invention is pure rutile phase, and refractive index is high, is a kind of splendid scattering layer material; Particle diameter and the visible ray of microballoon are close, and scattering now meets Mie scattering, and scattering is the strongest;
(3) the present invention is coated in scattering layer the short-circuit current density that can effectively promote battery on the little die substrate layer of conventional dyes sensitization solar battery, finally improves the photoelectric conversion efficiency of battery.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of bulky grain scattering microballoon in embodiment 1;
Fig. 2 is the field emission scanning electron microscope collection of illustrative plates of bulky grain microballoon in embodiment 1;
Fig. 3 be in embodiment 1 blade coating the scanning electron microscope (SEM) photograph in light anode cross section of one deck scattering layer;
Fig. 4 be in embodiment 2 silk screen printing the scanning electron microscope (SEM) photograph in light anode cross section of one deck scattering layer;
Fig. 5 is the I-V curve that does not add scattering layer in embodiment 2 and add two kinds of DSSC of scattering layer;
Fig. 6 is with scattering layer with not with the UV-Vis DRS collection of illustrative plates of two kinds of light anodes of scattering layer in embodiment 3.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Take 62 grams of sodium chloride and be made into 340 ml solns, this solution is transferred under ice water bath environment, dropwise splash into 10 milliliters of titanium tetrachlorides, stir on dropping limit, limit, obtains colourless uniform mixed solution after being added dropwise to complete.Mixed solution is transferred to carrying out hydro-thermal reaction in teflon-lined reactor, controlling reaction temperature is 120 ℃, temperature retention time is 12 hours, until insulation, finish also after cool to room temperature, to open water heating kettle, take out inner bag, pour out precipitation, wash 3 times and remove chloride ion and sodium ion, by the dry bulky grain titanium oxide scattering microballoon powder that obtains of pure precipitation.The powder that takes a morsel carries out X-ray diffraction (XRD) analysis, and XRD result shows that titanium dioxide is wherein Rutile Type, as shown in Figure 1.Fig. 2 is the field emission scanning electron microscope collection of illustrative plates of bulky grain microballoon, can see that oarse-grained particle diameter, substantially 600 microns of left and right, is formed by nanometer rods self assembly from scheming.Take 2 grams of bulky grain scattering microballoons and transfer in mortar, add the terpineol solution of ethyl cellulose that 8 grams of mass fractions that prepare are in advance 10%, three's mixture is ground and within 1 hour, obtains uniform slurry.Adopt knife coating; on the granule basalis of conventional dye-sensitized solar cell anode, apply one deck slurry; then by 450 ℃ of sintering and be incubated 30 minutes and can obtain DSSC scattering layer; Fig. 3 the has been blade coating scanning electron microscope (SEM) photograph in light anode cross section of one deck scattering layer; the thickness that can see granule basalis from scheming is about 6 microns, and scattering layer thickness is about 7 microns.
Take 41 grams of sodium chloride and be made into 340 ml solns, this solution is transferred under ice water bath environment, dropwise splash into 10 milliliters of titanium tetrachlorides, stir on dropping limit, limit, obtains colourless uniform mixed solution after being added dropwise to complete.Mixed solution is transferred to carrying out hydro-thermal reaction in teflon-lined reactor, controlling reaction temperature is 120 ℃, temperature retention time is 18 hours, until insulation, finish also after cool to room temperature, to open water heating kettle, take out inner bag, pour out precipitation, wash 3 times and remove chloride ion and sodium ion, by the dry bulky grain titanium oxide scattering microballoon powder that obtains of pure precipitation.Take 2 grams of bulky grain scattering microballoons and transfer in mortar, add the terpineol solution of ethyl cellulose that 8 grams of mass fractions that prepare are in advance 10%, three's mixture is ground and within 2 hours, obtains uniform slurry.Adopt the method for silk screen printing; silk-screen one deck slurry on the granule basalis of conventional dye-sensitized solar cell anode; then by 450 ℃ of sintering and be incubated 30 minutes and can obtain DSSC scattering layer; the scanning electron microscope (SEM) photograph in the light anode cross section of Fig. 3 is silk screen printing one deck scattering layer; the thickness of granule basalis is about 7 microns as seen from Figure 4, and scattering layer thickness is about 2 microns.Be assembled into DSSC photoelectric conversion efficiency and 5.83% risen to 7.32% by what do not add scattering layer, improved 26%, I-V curve as shown in Figure 5.
Embodiment 3
Take 41 grams of potassium chloride and be made into 340 ml solns, this solution is transferred under ice water bath environment, dropwise splash into 10 milliliters of titanium tetrachlorides, stir on dropping limit, limit, obtains colourless uniform mixed solution after being added dropwise to complete.Mixed solution is transferred to carrying out hydro-thermal reaction in teflon-lined reactor, controlling reaction temperature is 150 ℃, temperature retention time is 12 hours, until insulation, finish also after cool to room temperature, to open water heating kettle, take out inner bag, pour out precipitation, wash 3 times and remove chloride ion and potassium ion, by the dry bulky grain titanium oxide scattering microballoon powder that obtains of pure precipitation.Take 2 grams of bulky grain scattering microballoons and transfer in mortar, add the PEG 20000 aqueous solution that 8 grams of mass fractions that prepare are in advance 10%, three's mixture is ground and within 1 hour, obtains uniform slurry.Adopt the method for blade coating; blade coating one deck slurry on the granule basalis of conventional dye-sensitized solar cell anode; then by 500 ℃ of sintering and be incubated 30 minutes and can obtain DSSC scattering layer; Fig. 6 be with scattering layer and not with scattering layer the UV-Vis DRS collection of illustrative plates of light anode, from scheming, can see that having added the diffuse-reflecting power of light anode after scattering layer obviously improves.
Embodiment 4
Take 41 grams of potassium chloride and be made into 340 ml solns, this solution is transferred under ice water bath environment, dropwise splash into 10 milliliters of titanium tetrachlorides, stir on dropping limit, limit, obtains colourless uniform mixed solution after being added dropwise to complete.Mixed solution is transferred to carrying out hydro-thermal reaction in teflon-lined reactor, controlling reaction temperature is 120 ℃, temperature retention time is 24 hours, until insulation, finish also after cool to room temperature, to open water heating kettle, take out inner bag, pour out precipitation, wash 3 times and remove chloride ion and potassium ion, by the dry bulky grain titanium oxide scattering microballoon powder that obtains of pure precipitation.Take 2 grams of bulky grain scattering microballoons and transfer in mortar, add the ethanolic solution of the ethyl cellulose that 10 grams of mass fractions that prepare are in advance 10%, three's mixture is ground and within 1 hour, obtains uniform slurry.Adopt the method for blade coating, blade coating one deck slurry on the granule basalis of conventional dye-sensitized solar cell anode, then by 500 ℃ of sintering and be incubated 20 minutes and can obtain DSSC scattering layer.
Claims (7)
1. a preparation method for DSSC scattering layer, comprising:
(1) under ice-water bath, titanium tetrachloride is added in salting liquid, obtain clear solution; In clear solution, the concentration of titanium tetrachloride is 0.2～0.4M, and the concentration of salting liquid is 2～4M; Clear solution is transferred in reactor and carried out hydro-thermal reaction, and reaction temperature is 100～150 ℃, and temperature retention time is 12～24 hours; Until insulation, finish also after cool to room temperature, to open water heating kettle, by the washing of precipitate obtaining dry, obtain titanium oxide scattering microballoon;
(2) above-mentioned titanium oxide scattering microballoon is transferred in mortar, added successively pore creating material and solvent, grind and within 0.5～3 hour, obtain uniform slurry; Wherein, the mass fraction of titanium oxide scattering microballoon is 10～30%, and the mass fraction of pore creating material is 5～15%;
(3) adopt the method for silk screen printing or blade coating, on the granule basalis of dye-sensitized solar cell anode, apply above-mentioned slurry, 400～500 ℃ of sintering are also incubated 10～30 minutes, obtain DSSC scattering layer.
2. the preparation method of a kind of DSSC scattering layer according to claim 1, is characterized in that: the salt in described step (1) is villaumite, comprises one or more in lithium chloride, sodium chloride, potassium chloride, calcium chloride, magnesium chloride.
3. the preparation method of a kind of DSSC scattering layer according to claim 1, is characterized in that: the titanium oxide scattering microballoon in described step (1) is pure rutile phase, and particle diameter is 100～800nm, and specific area is 50～120m
2/ g.
4. the preparation method of a kind of DSSC scattering layer according to claim 1, is characterized in that: the pore creating material in described step (2) is one or more in polyethylene glycol, epoxy resin, cellulose and derivative thereof.
5. the preparation method of a kind of DSSC scattering layer according to claim 4, is characterized in that: described cellulose derivative is methylcellulose, ethyl cellulose, hydroxypropyl cellulose or carboxycellulose.
6. the preparation method of a kind of DSSC scattering layer according to claim 1, is characterized in that: the solvent in described step (2) is one or more in water, alcohols, polyalcohols, terpene.
7. the preparation method of a kind of DSSC scattering layer according to claim 1, is characterized in that: the thickness of the scattering layer in described step (3) is 1～6 μ m.
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| CN105428073B (en) * | 2015-11-24 | 2018-09-14 | 青岛能迅新能源科技有限公司 | A kind of solar battery light anode scattering layer slurry and preparation method thereof |
| CN108254809A (en) * | 2018-04-08 | 2018-07-06 | 河南师范大学 | A kind of full angle polarizes unrelated Microstructure Optics diffusing reflection coating |
| CN108648917B (en) * | 2018-04-26 | 2019-11-01 | 天津大学 | The preparation method of dye-sensitized solar cells scattering layer material is constituted with ultra-fine clay |
| CN110444688A (en) * | 2019-08-15 | 2019-11-12 | 昆山国显光电有限公司 | The production method and display device of display panel, display panel |
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