CN103440988B - A kind of preparation method of the perovskite-like sensitization light anode for hydridization solar cell - Google Patents
A kind of preparation method of the perovskite-like sensitization light anode for hydridization solar cell Download PDFInfo
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Abstract
The present invention provides the preparation method of a kind of perovskite-like sensitization light anode for hydridization solar cell, described preparation method is as follows: first prepares the sub-micron thick film being made up of wide bandgap semiconductor oxide-based nanomaterial on transparent conductive substrate, then deposits lead halide PbCl by ion-exchange in the film2Or PbBr2Or PbI2In at least one, finally make the lead halide of deposition and organic halogenation ammonium salt react by infusion process, in-situ preparation organic-inorganic perovskite-like in the film, it is thus achieved that the light anode of perovskite-like sensitization.The present invention can conveniently control the key parameters such as the component of organic-inorganic perovskite-like, particle diameter, thickness, thus controls its spectral response wave band and photoelectric properties.
Description
[technical field]
The present invention relates to the preparation method of a kind of perovskite-like sensitization light anode for hydridization solar cell.
[background technology]
Dyestuff or quantum dot sensitized solar cell are the novel solar cells of one that the nineties is developed, tool
Have the performances such as low cost, easy preparation technology and good Environmental compatibility, have good should
Use prospect.The hydridization solar cell of the organic-inorganic perovskite-like sensitization occurring in recent years is above-mentioned battery
Derivation, has low cost, the advantage of easily preparation equally, and simultaneously this kind of cell photoelectric conversion efficiency is rapidly
Improving, high-photoelectric transformation efficiency has reached 15% at present, is expected to become having of silica-based solar cell
Power competitor.The key component of the hydridization solar cell of organic-inorganic perovskite-like sensitization is organic-inorganic class
Perovskite sensitizer, traditional preparation method is to be spun to its solution be received by wide bandgap semiconductor oxide
In the light anode that rice material film is constituted, but this method is difficult in the film the uniformly organic mineral-type calcium of coating
Titanium ore, is also difficult to control the key parameters such as its particle diameter, pattern, thickness simultaneously, thus cannot be to its photoelectricity
Performance carries out Effective Regulation.
In view of this, this process is on the basis of through a series of research and test, develops one
Planting the preparation method of the perovskite-like sensitization light anode for hydridization solar cell, this case thus produces.
[content of the invention]
The technical problem to be solved in the present invention, is to provide a kind of perovskite-like for hydridization solar cell
The preparation method of sensitization light anode, can conveniently control the component of organic-inorganic perovskite-like, particle diameter, thickness
Deng key parameter, thus control its spectral response wave band and photoelectric properties.
The present invention is achieved in that
A kind of preparation method of the perovskite-like sensitization light anode for hydridization solar cell, described preparation side
Method is as follows:
First on transparent conductive substrate, prepare the Asia being made up of wide bandgap semiconductor oxide-based nanomaterial
Micron thick film, then deposits lead halide PbCl in the film by ion-exchange2Or PbBr2Or PbI2
In at least one, finally make the lead halide of deposition and organic halogenation ammonium salt react, at film by infusion process
Situ generates organic-inorganic perovskite-like, it is thus achieved that the light anode of perovskite-like sensitization.
Further, by ion-exchange by lead halide PbCl2Or PbBr2Or PbI2In at least one
Deposit in wide bandgap semiconductor oxide-based nanomaterial film, wherein Pb2+Ion is by (CH3COO)2Pb
Or Pb (NO3)2Acetum provide, Cl-、Br-Or I-Respectively by the second of NaCl, NaBr or NaI
Alcohol or alcohol-water mixed solution provide;By described Pb2+With Cl-Or Br-Or I-In at least one inhale successively
It is attached in film, after two kinds of contacted with ions, generate the lead halide of indissoluble.
Further, described organic halogenation ammonium salt is by the organic matter of kiber alkyl amine or amino-contained and HCl, HBr
Or HI reaction generates.
Further, described infusion process is as follows:
First organic halogenation ammonium salt is dissolved in polar-nonpolar mixed organic solvents formation saturated solution,
The film being attached with lead halide is immersed in this saturated solution so that lead halide is anti-with organic halogenation ammonium salt
Should, in-situ preparation organic-inorganic perovskite-like in the film, obtain the light anode of perovskite-like sensitization;Its
In, described non-polar organic solvent is the non-solvent of generated organic-inorganic perovskite-like, polar solvent
It is the polar solvent of soluble organic halogenation ammonium salt;And described polar-nonpolar mixed organic solvents indissoluble
Solve generated organic-inorganic perovskite-like.
Further, described non-polar organic solvent is benzene, toluene, at least one in hexamethylene, institute
State polar solvent be methyl alcohol, ethanol, isopropanol, dimethyl sulfoxide, in 1-METHYLPYRROLIDONE at least one
Kind.
Further, described polar organic solvent and the volume ratio of non-polar organic solvent are
1/3~1/10.
Further, described wide bandgap semiconductor oxide-based nanomaterial is TiO2、SnO2Or ZnO.
Further, the sub-micron thick film that described wide bandgap semiconductor oxide-based nanomaterial is constituted, tool
Body is 0.1~1 micron of thickness.
Present invention have the advantage that
The perovskite-like sensitization light anode for hydridization solar cell using this method to prepare, can conveniently control
It is formed with the key parameters such as the component of machine mineral-type perovskite, particle diameter, thickness, thus control its spectral response
Wave band and photoelectric properties, the development of the High-performance hybrid solar cell for being made up of perovskite-like sensitizer carries
For condition, make this novel solar cell be practical to be possibly realized.Additionally, product prepared by the present invention is also
Can be applicable to the field such as electroluminescent and electrochromism.
[detailed description of the invention]
The present invention relates to the preparation method of a kind of perovskite-like sensitization light anode for hydridization solar cell,
Described preparation method is as follows:
First on transparent conductive substrate, prepare the Asia being made up of wide bandgap semiconductor oxide-based nanomaterial
Micron thick film, then deposits lead halide PbCl in the film by ion-exchange2Or PbBr2Or PbI2
In at least one, finally make the lead halide of deposition and organic halogenation ammonium salt react, at film by infusion process
Situ generates organic-inorganic perovskite-like, it is thus achieved that the light anode of perovskite-like sensitization.
By ion-exchange by lead halide PbCl2Or PbBr2Or PbI2In at least one deposit to wide taboo
In band conductor oxidate nano material film, wherein Pb2+Ion is by (CH3COO)2Pb or Pb (NO3)2
Acetum provide, Cl-、Br-Or I-Respectively by ethanol or the alcohol-water of NaCl, NaBr or NaI
Mixed solution provides;By described Pb2+With Cl-Or Br-Or I-In at least one be adsorbed onto successively in film,
The lead halide of indissoluble is generated after two kinds of contacted with ions.
Described organic halogenation ammonium salt is anti-with HCl, HBr or HI by the organic matter of kiber alkyl amine or amino-contained
Should generate.
Described infusion process is as follows:
First organic halogenation ammonium salt is dissolved in polar-nonpolar mixed organic solvents formation saturated solution,
The film being attached with lead halide is immersed in this saturated solution so that lead halide is anti-with organic halogenation ammonium salt
Should, in-situ preparation organic-inorganic perovskite-like in the film, obtain the light anode of perovskite-like sensitization;Its
In, described non-polar organic solvent is the non-solvent of generated organic-inorganic perovskite-like, polar solvent
It is the polar solvent of soluble organic halogenation ammonium salt;And described polar-nonpolar mixed organic solvents indissoluble
Solve generated organic-inorganic perovskite-like.
Described non-polar organic solvent is benzene, toluene, at least one in hexamethylene, described polar solvent
For at least one in methyl alcohol, ethanol, isopropanol, dimethyl sulfoxide, 1-METHYLPYRROLIDONE.
Described polar organic solvent is 1/3~1/10 with the volume ratio of non-polar organic solvent.
Described wide bandgap semiconductor oxide-based nanomaterial is TiO2、SnO2Or ZnO.
The sub-micron thick film that described wide bandgap semiconductor oxide-based nanomaterial is constituted, specially 0.1~1
Micron is thick.
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
First, TiO2The preparation of nano-crystal film: by commercially available TiO2Nano-crystalline granule 2kg is dispersed in 2
In L deionized water, add 0.2kg polyethylene glycol (molecular weight is 20,000), after grinding uniformly, coating
It on the fin oxide condutire glass of doped with fluorine, after 80 DEG C dry, is placed in 450~500 DEG C of baking 0.5h in Muffle furnace,
Form 0.1-0.8 micron thick film.
Second step, at TiO2Nano-crystal film deposits lead iodide: first by 38g (CH3COO)2Pb is molten
Solution, in 1L acetic acid, forms 0.1M Pb2+Acetum;Secondly 15g NaI is dissolved in 1L second
In alcohol, form 0.1M I-Isoionic alcoholic solution;Finally, by TiO2Nano-crystal film is placed in Pb2+From
30S in sub-solution, is placed in I after cleaning in ethanol again-30S in solion, then clean in ethanol,
Completing primary ions exchange deposition, the lead iodide that be can control generation by control ion exchange frequency of depositing is thick
Degree.
3rd step, CH3NH3The preparation of Cl solution: by the second that commercially available mass concentration is 25wt% methylamine
Alcoholic solution 125mL and mass concentration are the concentrated hydrochloric acid at room temperature mixing and stirring of 36wt%, decompression
Distillation obtains CH3NH3Cl salt, with washes of absolute alcohol three times, being dissolved into volume ratio after drying is 1/6
Isopropanol and cyclohexane solution in, formed CH3NH3Cl saturated solution.
4th step, infusion process in-situ preparation CH3NH3PbI2Cl perovskite-like: deposition is had lead iodide
TiO2Nano-crystal film immerses the CH of the 3rd step preparation3NH3In Cl isopropanol-hexamethylene saturated solution,
Room temperature stands 0.5-1h, lead iodide and CH in solution3NH3Cl reaction increasingly generates CH3NH3PbI2Cl
Perovskite-like, it is thus achieved that CH3NH3PbI2The light anode of Cl perovskite-like sensitization.
Finally, it is thus achieved that for the light anode of the organic-inorganic perovskite-like sensitization of hybrid solar cell, tool
There is the photoelectric transformation efficiency of 10%.
Embodiment 2
First, TiO2The preparation of nano-crystal film: by commercially available TiO2Nano-crystalline granule 2kg is dispersed in 2
In L deionized water, add 0.2kg polyethylene glycol (molecular weight is 20,000), after grinding uniformly, coating
It on the fin oxide condutire glass of doped with fluorine, after 80 DEG C dry, is placed in 450~500 DEG C of baking 0.5h in Muffle furnace,
Form 0.1-0.8 micron thick film.
Second step, at TiO2Nano-crystal film deposits lead bromide: first by 38g (CH3COO)2Pb is molten
Solution, in 1L acetic acid, forms 0.1M Pb2+Acetum;Secondly 15g NaBr is dissolved in 1L
In ethanol, form 0.1M Br-Isoionic alcoholic solution;Finally, by TiO2Nano-crystal film is placed in Pb2+
30S in solion, is placed in Br after cleaning in ethanol again-30S in solion, more in ethanol
Clean, complete primary ions exchange deposition, be can control the bromine of generation by control ion exchange frequency of depositing
Change lead thickness.
3rd step, CH3NH3The preparation of I solution: by the ethanol that commercially available mass concentration is 25wt% methylamine
Solution 125mL and mass concentration are the hydroiodic acid at room temperature mixing and stirring of 50wt%, and decompression is steamed
Evaporate acquisition CH3NH3I salt, with washes of absolute alcohol three times, be dissolved into after drying volume ratio be 1/6 different
In propyl alcohol and cyclohexane solution, form CH3NH3I saturated solution.
4th step, infusion process in-situ preparation CH3NH3PbBr2I perovskite-like: deposition is had lead bromide
TiO2Nano-crystal film immerses the CH of the 3rd step preparation3NH3In I isopropanol-hexamethylene saturated solution, room
The gentle and quiet .5-1h that sets to 0, lead bromide and CH in solution3NH3I reaction increasingly generates CH3NH3PbBr2I class calcium
Titanium ore, it is thus achieved that CH3NH3PbBr2The light anode of I perovskite-like sensitization.
Finally, it is thus achieved that for the light anode of the organic-inorganic perovskite-like sensitization of hybrid solar cell, tool
There is the photoelectric transformation efficiency of 8%.
Embodiment 3
First, TiO2The preparation of nano-crystal film: by commercially available TiO2Nano-crystalline granule 2kg is dispersed in 2
In L deionized water, add 0.2kg polyethylene glycol (molecular weight is 20,000), after grinding uniformly, coating
It on the fin oxide condutire glass of doped with fluorine, after 80 DEG C dry, is placed in 450~500 DEG C of baking 0.5h in Muffle furnace,
Form 0.1-0.8 micron thick film.
Second step, at TiO2Nano-crystal film deposits lead halide mixture: first by 38g
(CH3COO)2Pb is dissolved in 1L acetic acid, forms 0.1M Pb2+Acetum;Secondly by Na+
Total ion concentration is that the alcohol-water mixing of the X M NaI of 0.1M, Y M NaBr and Z M NaCl is molten
Liquid (ethanol/water volume ratio 10/1-10/5, X+Y+Z=0.1);Finally, by TiO2Nano-crystal film
It is placed in Pb2+30S in solion, is placed in above-mentioned halogen Ar ion mixing solution after cleaning in ethanol again
30S, then clean in ethanol, complete primary ions exchange deposition, by control ion exchange deposition time
The controllable lead halide mixture thickness generating of number.
3rd step, CH3NH3The preparation of I solution: by the ethanol that commercially available mass concentration is 25wt% methylamine
Solution 125mL and mass concentration are the hydroiodic acid at room temperature mixing and stirring of 50wt%, and decompression is steamed
Evaporate acquisition CH3NH3I salt, with washes of absolute alcohol three times, be dissolved into after drying volume ratio be 1/6 different
In propyl alcohol and cyclohexane solution, form CH3NH3I saturated solution.
4th step, infusion process in-situ preparation CH3NH3PbCl20ZBr20YI1+20XPerovskite-like: deposition is had
The TiO of lead halide mixture2Nano-crystal film immerses the CH of the 3rd step preparation3NH3I isopropanol-hexamethylene
In saturated solution, room temperature stands 0.5-1h, lead halide and CH in solution3NH3I reaction increasingly generates
CH3NH3PbCl20ZBr20YI1+20XPerovskite-like, it is thus achieved that CH3NH3PbCl20ZBr20YI1+20XPerovskite-like
The light anode of sensitization.
Finally, it is thus achieved that for the light anode of the organic-inorganic perovskite-like sensitization of hybrid solar cell, logical
Overregulate I, Br, Cl ratio in perovskite-like, the photoelectric transformation efficiency of 8-15% can be obtained.
It by said method, is available for the organic-inorganic perovskite-like sensitization of hybrid solar cell
Light anode, has a photoelectric transformation efficiency of 8-15%, meanwhile, by adjusting lead halide component, organic
Amine component or hydrogen halides component, can obtain that to have the serial organic-inorganic perovskite-like of different photoelectric properties quick
Agent.
The perovskite-like sensitization light anode for hydridization solar cell using this method to prepare, can conveniently control
It is formed with the key parameters such as the component of machine mineral-type perovskite, particle diameter, thickness, thus control its spectral response
Wave band and photoelectric properties, the development of the High-performance hybrid solar cell for being made up of perovskite-like sensitizer carries
For condition, make this novel solar cell be practical to be possibly realized.Additionally, product prepared by the present invention is also
Can be applicable to the field such as electroluminescent and electrochromism.
It although the foregoing describing the detailed description of the invention of the present invention, but is familiar with the technology people of the art
Member it should be appreciated that we are merely exemplary described specific embodiment, rather than for this
The restriction of bright scope, those of ordinary skill in the art are in the equivalence made according to the spirit of the present invention
Modify and change, all should cover in the scope of the claimed protection of the present invention.
Claims (7)
1. it is used for a preparation method for the perovskite-like sensitization light anode of hydridization solar cell, its feature
It is: described preparation method is as follows:
First on transparent conductive substrate, prepare the Asia being made up of wide bandgap semiconductor oxide-based nanomaterial
Micron thick film, then deposits lead halide PbCl in the film by ion-exchange2Or PbBr2Or PbI2
In at least one, finally make the lead halide of deposition and organic halogenation ammonium salt react, at film by infusion process
Situ generates organic-inorganic perovskite-like, it is thus achieved that the light anode of perovskite-like sensitization;
By ion-exchange by lead halide PbCl2Or PbBr2Or PbI2In at least one deposit to wide taboo
In band conductor oxidate nano material film, wherein Pb2+Ion is by (CH3COO)2Pb or Pb (NO3)2
Acetum provide, Cl-、Br-Or I-Respectively by ethanol or the alcohol-water of NaCl, NaBr or NaI
Mixed solution provides;By described Pb2+With Cl-Or Br-Or I-In at least one be adsorbed onto successively in film,
The lead halide of indissoluble is generated after two kinds of contacted with ions.
2. a kind of perovskite-like sensitization light anode for hydridization solar cell as claimed in claim 1
Preparation method, it is characterised in that: described organic halogenation ammonium salt is by the organic matter of kiber alkyl amine or amino-contained
React generation with HCl, HBr or HI.
3. a kind of perovskite-like sensitization light anode for hydridization solar cell as claimed in claim 1
Preparation method, it is characterised in that: described infusion process is as follows:
First organic halogenation ammonium salt is dissolved in polar-nonpolar mixed organic solvents formation saturated solution,
The film being attached with described lead halide is immersed in this saturated solution so that described lead halide and organic halogenation
Ammonium salt reacts, in-situ preparation organic-inorganic perovskite-like in the film, obtains the light sun of perovskite-like sensitization
Pole;Wherein, described non-polar organic solvent is the non-solvent of generated organic-inorganic perovskite-like, pole
Property solvent is the polar solvent of soluble organic halogenation ammonium salt;And the mixing of described polar-nonpolar is organic molten
The organic-inorganic perovskite-like that agent indissoluble solution is generated.
4. a kind of perovskite-like sensitization light sun for hydridization solar cell according to claim 3
The preparation method of pole, it is characterised in that: described non-polar organic solvent be benzene, toluene, in hexamethylene
At least one, described polar solvent is methyl alcohol, ethanol, isopropanol, dimethyl sulfoxide, N-crassitude
At least one in ketone.
5. a kind of perovskite-like sensitization for hydridization solar cell according to claim 3 or 4
The preparation method of light anode, it is characterised in that: the body of described polar organic solvent and non-polar organic solvent
Long-pending ratio is 1/3~1/10.
6. a kind of perovskite-like sensitization light anode for hydridization solar cell as claimed in claim 1
Preparation method, it is characterised in that: described wide bandgap semiconductor oxide-based nanomaterial is TiO2、SnO2
Or ZnO.
7. a kind of perovskite-like sensitization light anode for hydridization solar cell as claimed in claim 1
Preparation method, it is characterised in that: described wide bandgap semiconductor oxide-based nanomaterial constitute sub-micron
Thick film, specially 0.1~1 micron thickness.
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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 |
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 |
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