CN103440988A - Preparation method of hybridization solar battery for perovskite-like sensitized photoanode - Google Patents

Preparation method of hybridization solar battery for perovskite-like sensitized photoanode Download PDF

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CN103440988A
CN103440988A CN2013103065592A CN201310306559A CN103440988A CN 103440988 A CN103440988 A CN 103440988A CN 2013103065592 A CN2013103065592 A CN 2013103065592A CN 201310306559 A CN201310306559 A CN 201310306559A CN 103440988 A CN103440988 A CN 103440988A
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perovskite
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sensitization
light anode
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CN103440988B (en
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兰章
吴季怀
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Huaqiao University
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Abstract

The invention provides a preparation method of a hybridization solar battery for a perovskite-like sensitized photoanode. The preparation method includes the following steps that a thin film with a thickness of a submicron and made of wide bandgap semiconductor oxide nano materials is manufactured on a transparent conductive substrate at first, then at least one of lead halide PbC12 or PbBr2 or PbI2 is deposited in the thin film by means of an ion exchange method, and finally deposited lead halide reacts with organic halogenated ammonium salt through an impregnation method to generate organic and inorganic perovskite in the thin film in situ to obtain the perovskite-like sensitized photoanode. According to the preparation method, components, grain diameters, thicknesses and other key parameters of the organic and inorganic perovskite can be conveniently controlled, and thus spectral response wave bands and photoelectric performance of the organic and inorganic perovskite can be controlled.

Description

A kind of preparation method of the sensitization of the perovskite-like for hydridization solar cell light anode
[technical field]
The present invention relates to a kind of preparation method of the sensitization of the perovskite-like for hydridization solar cell light anode.
[background technology]
Dyestuff or quantum dot sensitized solar cell are a kind of novel solar cells that the nineties is developed, and have low cost, easy preparation technology and the good performances such as Environmental compatibility, have a good application prospect.The hydridization solar cell of the organic-inorganic perovskite-like sensitization occurred in recent years is the derivation of above-mentioned battery, there is equally low cost, easily preparation, this class cell photoelectric conversion efficiency is in rapid improve simultaneously, high-photoelectric transformation efficiency has reached 15% at present, is expected to become the strong competitor of silica-based solar cell.The key component of the hydridization solar cell of organic-inorganic perovskite-like sensitization is organic-inorganic perovskite-like sensitizer, traditional preparation method is spun to its solution in the light anode consisted of wide bandgap semiconductor oxide-based nanomaterial film, but this method is difficult to evenly apply organic mineral-type perovskite in film, while is the key parameters such as restive its particle diameter, pattern, thickness also, thereby can't carry out Effective Regulation to its photoelectric properties.
In view of this, this process, on the basis through a series of research and test, is developed a kind of preparation method of the sensitization of the perovskite-like for hydridization solar cell light anode, and this case produces thus.
[summary of the invention]
The technical problem to be solved in the present invention, be to provide a kind of preparation method of the sensitization of the perovskite-like for hydridization solar cell light anode, can conveniently control the key parameter such as component, particle diameter, thickness of organic-inorganic perovskite-like, thereby control its spectral response wave band and photoelectric properties.
The present invention is achieved in that
A kind of preparation method of the sensitization of the perovskite-like for hydridization solar cell light anode, described preparation method is as follows:
At first the sub-micron thick film that preparation consists of the wide bandgap semiconductor oxide-based nanomaterial on transparent conductive substrate then deposits lead halide PbCl by ion-exchange in film 2or PbBr 2or PbI 2in at least one, finally by infusion process, the lead halide of deposition react with the organic halogenation ammonium salt, at film situ generation organic-inorganic perovskite-like, the light anode of acquisition perovskite-like sensitization.
Further, by ion-exchange by lead halide PbCl 2or PbBr 2or PbI 2in at least one deposit in wide bandgap semiconductor oxide-based nanomaterial film, Pb wherein 2+ion is by (CH 3cOO) 2pb or Pb (NO 3) 2acetum provide, Cl -, Br -or I -ethanol or alcohol-water mixed solution by NaCl, NaBr or NaI provides respectively; By described Pb 2+with Cl -or Br -or I -in at least one be adsorbed onto successively in film, generate the lead halides of indissolubles after the contact of two kinds of ions.
Further, described organic halogenation ammonium salt reacts generation by the organic substance of kiber alkyl amine or amino-contained with HCl, HBr or HI.
Further, described infusion process is as follows:
First the organic halogenation ammonium salt is dissolved in the polar-nonpolar mixed organic solvents and forms saturated solution, the film that is attached with lead halide is immersed in this saturated solution, make lead halide react with the organic halogenation ammonium salt, generate the organic-inorganic perovskite-like at the film situ, obtain the light anode of perovskite-like sensitization; Wherein, described non-polar organic solvent is the non-solvent of generated organic-inorganic perovskite-like, and polar solvent is the polar solvent of soluble organic halogenation ammonium salt; And the organic-inorganic perovskite-like that described polar-nonpolar mixed organic solvents indissoluble solution generates.
Further, described non-polar organic solvent is at least one in benzene, toluene, cyclohexane, and described polar solvent is at least one in methyl alcohol, ethanol, isopropyl alcohol, methyl-sulfoxide, 1-METHYLPYRROLIDONE.
Further, the volume ratio of described polar organic solvent and non-polar organic solvent is 1/3～1/10.
Further, described wide bandgap semiconductor oxide-based nanomaterial is TiO 2, SnO 2or ZnO.
Further, the sub-micron thick film that described wide bandgap semiconductor oxide-based nanomaterial forms, be specially 0.1～1 micron thick.
The present invention has following advantage:
The sensitization of the perovskite-like for the hydridization solar cell light anode that adopts this method to prepare, can conveniently control the key parameter such as component, particle diameter, thickness of organic-inorganic perovskite-like, thereby control its spectral response wave band and photoelectric properties, for the development of the high-performance hydridization solar cell that consists of the perovskite-like sensitizer provides condition, make the practical possibility that becomes of this novel solar cell.In addition, the product that prepared by the present invention also can be applicable to the fields such as electroluminescence and electrochromism.
[embodiment]
The present invention relates to a kind of preparation method of the sensitization of the perovskite-like for hydridization solar cell light anode, described preparation method is as follows:
At first the sub-micron thick film that preparation consists of the wide bandgap semiconductor oxide-based nanomaterial on transparent conductive substrate then deposits lead halide PbCl by ion-exchange in film 2or PbBr 2or PbI 2in at least one, finally by infusion process, the lead halide of deposition react with the organic halogenation ammonium salt, at film situ generation organic-inorganic perovskite-like, the light anode of acquisition perovskite-like sensitization.
By ion-exchange by lead halide PbCl 2or PbBr 2or PbI 2in at least one deposit in wide bandgap semiconductor oxide-based nanomaterial film, Pb wherein 2+ion is by (CH 3cOO) 2pb or Pb (NO 3) 2acetum provide, Cl -, Br -or I -ethanol or alcohol-water mixed solution by NaCl, NaBr or NaI provides respectively; By described Pb 2+with Cl -or Br -or I -in at least one be adsorbed onto successively in film, generate the lead halides of indissolubles after the contact of two kinds of ions.
Described organic halogenation ammonium salt reacts generation by the organic substance of kiber alkyl amine or amino-contained with HCl, HBr or HI.
Described infusion process is as follows:
First the organic halogenation ammonium salt is dissolved in the polar-nonpolar mixed organic solvents and forms saturated solution, the film that is attached with lead halide is immersed in this saturated solution, make lead halide react with the organic halogenation ammonium salt, generate the organic-inorganic perovskite-like at the film situ, obtain the light anode of perovskite-like sensitization; Wherein, described non-polar organic solvent is the non-solvent of generated organic-inorganic perovskite-like, and polar solvent is the polar solvent of soluble organic halogenation ammonium salt; And the organic-inorganic perovskite-like that described polar-nonpolar mixed organic solvents indissoluble solution generates.
Described non-polar organic solvent is at least one in benzene, toluene, cyclohexane, and described polar solvent is at least one in methyl alcohol, ethanol, isopropyl alcohol, methyl-sulfoxide, 1-METHYLPYRROLIDONE.
The volume ratio of described polar organic solvent and non-polar organic solvent is 1/3～1/10.
Described wide bandgap semiconductor oxide-based nanomaterial is TiO 2, SnO 2or ZnO.
The sub-micron thick film that described wide bandgap semiconductor oxide-based nanomaterial forms, be specially 0.1～1 micron thick.
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
The first, TiO 2the preparation of nano-crystal film: by commercially available TiO 2nano-crystalline granule 2kg is dispersed in the 2L deionized water, adds 0.2kg polyethylene glycol (molecular weight is 20,000), after grinding evenly, the fin oxide condutire that is coated in doped with fluorine is on glass, after 80 ℃ of oven dry, be placed in 450～500 ℃ of Muffle furnaces and dry 0.5h, form 0.1-0.8 micron thick film.
Second step, at TiO 2deposit lead iodide in nano-crystal film: at first by 38g (CH 3cOO) 2pb is dissolved in 1L acetic acid, forms 0.1M Pb 2+acetum; Secondly 15g NaI is dissolved in 1L ethanol, forms 0.1M I -isoionic alcoholic solution; Finally, by TiO 2nano-crystal film is placed in Pb 2+30S in solion, be placed in I after cleaning in ethanol again -30S in solion, then clean in ethanol, complete primary ions exchange deposition, can control the lead iodide thickness of generation by controlling the ion-exchange frequency of depositing.
The 3rd step, CH 3nH 3the preparation of Cl solution: the concentrated hydrochloric acid that the ethanolic solution 125mL that is the 25wt% methylamine by commercially available mass concentration and mass concentration are 36wt% is mixing and stirring at room temperature, and decompression distillation obtains CH 3nH 3cl salt, clean three times with absolute ethyl alcohol, in isopropyl alcohol and cyclohexane solution that to be dissolved into volume ratio after oven dry be 1/6, forms CH 3nH 3the Cl saturated solution.
The 4th step, the infusion process original position generates CH 3nH 3pbI 2cl perovskite-like: the TiO that will deposit lead iodide 2nano-crystal film immerses the CH of the 3rd step preparation 3nH 3in Cl isopropyl alcohol-cyclohexane saturated solution, the standing 0.5-1h of room temperature, CH in lead iodide and solution 3nH 3the Cl reaction generates CH gradually 3nH 3pbI 2the Cl perovskite-like, obtain CH 3nH 3pbI 2the light anode of Cl perovskite-like sensitization.
Finally, obtain the light anode for the organic-inorganic perovskite-like sensitization of hybrid solar cell, there is 10% photoelectric conversion efficiency.
Embodiment 2
The first, TiO 2the preparation of nano-crystal film: by commercially available TiO 2nano-crystalline granule 2kg is dispersed in the 2L deionized water, adds 0.2kg polyethylene glycol (molecular weight is 20,000), after grinding evenly, the fin oxide condutire that is coated in doped with fluorine is on glass, after 80 ℃ of oven dry, be placed in 450～500 ℃ of Muffle furnaces and dry 0.5h, form 0.1-0.8 micron thick film.
Second step, at TiO 2deposit lead bromide in nano-crystal film: at first by 38g (CH 3cOO) 2pb is dissolved in 1L acetic acid, forms 0.1M Pb 2+acetum; Secondly 15g NaBr is dissolved in 1L ethanol, forms 0.1M Br -isoionic alcoholic solution; Finally, by TiO 2nano-crystal film is placed in Pb 2+30S in solion, be placed in Br after cleaning in ethanol again -30S in solion, then clean in ethanol, complete primary ions exchange deposition, can control the lead bromide thickness of generation by controlling the ion-exchange frequency of depositing.
The 3rd step, CH 3nH 3the preparation of I solution: the hydroiodic acid that the ethanolic solution 125mL that is the 25wt% methylamine by commercially available mass concentration and mass concentration are 50wt% is mixing and stirring at room temperature, and decompression distillation obtains CH 3nH 3i salt, clean three times with absolute ethyl alcohol, in isopropyl alcohol and cyclohexane solution that to be dissolved into volume ratio after oven dry be 1/6, forms CH 3nH 3the I saturated solution.
The 4th step, the infusion process original position generates CH 3nH 3pbBr 2i perovskite-like: the TiO that will deposit lead bromide 2nano-crystal film immerses the CH of the 3rd step preparation 3nH 3in I isopropyl alcohol-cyclohexane saturated solution, the standing 0.5-1h of room temperature, CH in lead bromide and solution 3nH 3the I reaction generates CH gradually 3nH 3pbBr 2the I perovskite-like, obtain CH 3nH 3pbBr 2the light anode of I perovskite-like sensitization.
Finally, obtain the light anode for the organic-inorganic perovskite-like sensitization of hybrid solar cell, there is 8% photoelectric conversion efficiency.
Embodiment 3
The first, TiO 2the preparation of nano-crystal film: by commercially available TiO 2nano-crystalline granule 2kg is dispersed in the 2L deionized water, adds 0.2kg polyethylene glycol (molecular weight is 20,000), after grinding evenly, the fin oxide condutire that is coated in doped with fluorine is on glass, after 80 ℃ of oven dry, be placed in 450～500 ℃ of Muffle furnaces and dry 0.5h, form 0.1-0.8 micron thick film.
Second step, at TiO 2deposition lead halide mixture in nano-crystal film: at first by 38g (CH 3cOO) 2pb is dissolved in 1L acetic acid, forms 0.1M Pb 2+acetum; Secondly by Na +x M NaI, the Y M NaBr that total ion concentration is 0.1M and the alcohol-water mixed solution of Z M NaCl (ethanol/water volume ratio 10/1-10/5, X+Y+Z=0.1); Finally, by TiO 2nano-crystal film is placed in Pb 2+30S in solion, be placed in above-mentioned halogen Ar ion mixing solution 30S after cleaning in ethanol again, then clean in ethanol, completes primary ions exchange deposition, can control the lead halide mixture thickness of generation by controlling the ion-exchange frequency of depositing.
The 3rd step, CH 3nH 3the preparation of I solution: the hydroiodic acid that the ethanolic solution 125mL that is the 25wt% methylamine by commercially available mass concentration and mass concentration are 50wt% is mixing and stirring at room temperature, and decompression distillation obtains CH 3nH 3i salt, clean three times with absolute ethyl alcohol, in isopropyl alcohol and cyclohexane solution that to be dissolved into volume ratio after oven dry be 1/6, forms CH 3nH 3the I saturated solution.
The 4th step, the infusion process original position generates CH 3nH 3pbCl 20Zbr 20Yi 1+20Xperovskite-like: the TiO that will deposit the lead halide mixture 2nano-crystal film immerses the CH of the 3rd step preparation 3nH 3in I isopropyl alcohol-cyclohexane saturated solution, the standing 0.5-1h of room temperature, CH in lead halide and solution 3nH 3the I reaction generates CH gradually 3nH 3pbCl 20Zbr 20Yi 1+20Xperovskite-like, obtain CH 3nH 3pbCl 20Zbr 20Yi 1+20Xthe light anode of perovskite-like sensitization.
Finally, obtain the light anode for the organic-inorganic perovskite-like sensitization of hybrid solar cell, by regulating I, Br, the ratio of Cl in perovskite-like, can obtain the photoelectric conversion efficiency of 8-15%.
Pass through said method, can obtain the light anode for the organic-inorganic perovskite-like sensitization of hybrid solar cell, photoelectric conversion efficiency with 8-15%, simultaneously, by adjusting lead halide component, organic amine component or hydrogen halides component, can obtain the serial organic-inorganic perovskite-like sensitizer with different photoelectric properties.
The sensitization of the perovskite-like for the hydridization solar cell light anode that adopts this method to prepare, can conveniently control the key parameter such as component, particle diameter, thickness of organic-inorganic perovskite-like, thereby control its spectral response wave band and photoelectric properties, for the development of the high-performance hydridization solar cell that consists of the perovskite-like sensitizer provides condition, make the practical possibility that becomes of this novel solar cell.In addition, the product that prepared by the present invention also can be applicable to the fields such as electroluminescence and electrochromism.
Although more than described the specific embodiment of the present invention; but being familiar with those skilled in the art is to be understood that; our described specific embodiment is illustrative; rather than for the restriction to scope of the present invention; those of ordinary skill in the art are in modification and the variation of the equivalence of doing according to spirit of the present invention, all should be encompassed in the scope that claim of the present invention protects.

Claims (8)

1. the preparation method of the sensitization of the perovskite-like for a hydridization solar cell light anode, it is characterized in that: described preparation method is as follows:
At first the sub-micron thick film that preparation consists of the wide bandgap semiconductor oxide-based nanomaterial on transparent conductive substrate then deposits lead halide PbCl by ion-exchange in film 2or PbBr 2or PbI 2in at least one, finally by infusion process, the lead halide of deposition react with the organic halogenation ammonium salt, at film situ generation organic-inorganic perovskite-like, the light anode of acquisition perovskite-like sensitization.
2. the preparation method of a kind of sensitization of the perovskite-like for hydridization solar cell light anode as claimed in claim 1 is characterized in that: by ion-exchange by lead halide PbCl 2or PbBr 2or PbI 2in at least one deposit in wide bandgap semiconductor oxide-based nanomaterial film, Pb wherein 2+ion is by (CH 3cOO) 2pb or Pb (NO 3) 2acetum provide, Cl -, Br -or I -ethanol or alcohol-water mixed solution by NaCl, NaBr or NaI provides respectively; By described Pb 2+with Cl -or Br -or at least one in I-be adsorbed onto in film successively, generate the lead halides of indissolubles after two kinds of ions contacts.
3. the preparation method of a kind of sensitization of the perovskite-like for hydridization solar cell light anode as claimed in claim 1, it is characterized in that: described organic halogenation ammonium salt reacts generation by the organic substance of kiber alkyl amine or amino-contained with HCl, HBr or HI.
4. the preparation method of a kind of sensitization of the perovskite-like for hydridization solar cell light anode as claimed in claim 1, it is characterized in that: described infusion process is as follows:
First the organic halogenation ammonium salt is dissolved in the polar-nonpolar mixed organic solvents and forms saturated solution, the film that is attached with lead halide is immersed in this saturated solution, make lead halide react with the organic halogenation ammonium salt, generate the organic-inorganic perovskite-like at the film situ, obtain the light anode of perovskite-like sensitization; Wherein, described non-polar organic solvent is the non-solvent of generated organic-inorganic perovskite-like, and polar solvent is the polar solvent of soluble organic halogenation ammonium salt; And the organic-inorganic perovskite-like that described polar-nonpolar mixed organic solvents indissoluble solution generates.
5. the preparation method of a kind of sensitization of the perovskite-like for hydridization solar cell light anode according to claim 4, it is characterized in that: described non-polar organic solvent is at least one in benzene, toluene, cyclohexane, and described polar solvent is at least one in methyl alcohol, ethanol, isopropyl alcohol, methyl-sulfoxide, 1-METHYLPYRROLIDONE.
6. according to the preparation method of the described a kind of sensitization of the perovskite-like for the hydridization solar cell light anode of claim 4 or 5, it is characterized in that: the volume ratio of described polar organic solvent and non-polar organic solvent is 1/3～1/10.
7. the preparation method of a kind of sensitization of the perovskite-like for hydridization solar cell light anode as claimed in claim 1, it is characterized in that: described wide bandgap semiconductor oxide-based nanomaterial is TiO 2, SnO 2or ZnO.
8. the preparation method of a kind of sensitization of the perovskite-like for hydridization solar cell light anode as claimed in claim 1 is characterized in that: the sub-micron thick film that described wide bandgap semiconductor oxide-based nanomaterial forms is specially 0.1～1 micron thick.
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CN103996749A (en) * 2014-06-04 2014-08-20 山西大学 In-situ preparation method of perovskite solar battery photo-anode
CN105655447A (en) * 2016-04-01 2016-06-08 合肥工业大学 Large-area preparation method of perovskite films suitable for various substrate shapes
CN104332560B (en) * 2014-09-04 2017-01-11 武汉大学 Preparation method of chlorine-bromine-iodine-mixing perovskite light absorption layer material
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CN103996749A (en) * 2014-06-04 2014-08-20 山西大学 In-situ preparation method of perovskite solar battery photo-anode
CN106573791A (en) * 2014-08-05 2017-04-19 韩国化学研究院 Method for preparing inorganic/organic hybrid perovskite compound film
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CN110270485A (en) * 2019-06-11 2019-09-24 南京邮电大学 A kind of preparation method of perovskite nano particle thick film
CN110473972A (en) * 2019-06-27 2019-11-19 南京工业大学 A kind of preparation method and its photovoltaic applications based on the translucent perovskite thin film of anion exchange
CN110649161A (en) * 2019-09-16 2020-01-03 北京航空航天大学 Method for preparing high-purity and high-flatness perovskite film by using mixed solvent
JP2020107912A (en) * 2020-04-06 2020-07-09 株式会社東芝 Method for manufacturing photoelectric conversion film and method for manufacturing photoelectric conversion element
JP2022176313A (en) * 2020-04-06 2022-11-25 株式会社東芝 Method for manufacturing photoelectric conversion film and method for manufacturing photoelectric conversion element
CN112186110A (en) * 2020-09-28 2021-01-05 中山大学 Preparation method of organic-inorganic hybrid perovskite methylamine lead iodide surface in-situ growth organic passivation film
CN112186110B (en) * 2020-09-28 2022-11-25 中山大学 Preparation method of organic-inorganic hybrid perovskite methylamine lead iodide surface in-situ growth organic passivation film
CN113703242A (en) * 2021-08-04 2021-11-26 燕山大学 Electrochemical color-changing device

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