CN109545977A - Crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette - Google Patents
Crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette Download PDFInfo
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Abstract
Crystallization preparation method in situ is climbed in the liquid film thickening suppression that the present invention discloses a kind of uniform perovskite film of flannelette, comprising: the first step prepares perovskite precursor sol or solution containing thickener；Second step, the uniform coating of perovskite liquid film；Third step, the drying process of perovskite liquid film；4th step, perovskite thin film go solvent heat treatment: the perovskite thin film through being dried being carried out to the annealing of 10~120min at 90~150 DEG C, removes residual solvent；5th step, perovskite thin film go thickener to be heat-treated: the 4th step treated perovskite thin film being carried out to the annealing of 10~120min at 100~180 DEG C, removal thickener simultaneously makes crystal grain grow up, finally obtains and imitate the uniform perovskite thin film of pyramidal flannelette.The present invention does not carry out polishing to silicon pyramid flannelette and polishes processing, and the preparation of the uniform profiling perovskite thin film of all standing in the pyramid flannelette substrate that micro-meter scale rises and falls is realized using solution-deposition method, maintains the efficient advantage of silicon solar cell.
Description
Technical field
The invention belongs to area of solar cell, in particular to the preparation method of a kind of uniform perovskite film of flannelette.
Background technique
2009, organic inorganic hybridization perovskite light absorbent was used in solar battery for the first time, obtained 3.8% light
Electrotransformation efficiency, then its efficiency rapidly rises in a few years.Up to now, by National Renewable Energy laboratory
The peak efficiency of certification reaches 23.4%.Perovskite solar battery is with the hybridized metal halogenation with perovskite crystal structure
Object AMX3(A is usually CH3NH3 +、HC(NH2)2 +Deng M is usually Pb2+、Sn2+Deng X is usually Cl-、Br-、I-Deng) it is light absorption
A kind of novel solar battery of layer, have photoelectric conversion efficiency it is high, can solwution method the advantages such as inexpensively prepare.However unijunction calcium titanium
The photoelectric conversion efficiency of mine solar battery can not be more than Xiao Keli-Kui Yise limit theory efficiency.Multijunction solar cell, i.e.,
Laminated cell is made of the solar subcells with different band gap, is a kind of mature effective breakthrough pole Xiao Keli-Kui Yise
The mode for limiting theoretical efficiency, has been widely used for traditional silicon, gallium arsenide solar cell.Silicon solar cell is to account at present
According to the maximum mainstream photovoltaic technology of the market share.The band gap of monocrystalline silicon is about 1.1eV, is the sub- battery of ideal narrow band gap.It is organic
Inorganic hybridization perovskite material and full-inorganic perovskite material have the characteristics that band gap is continuously adjusted (1.25~2.0eV).It is based on
These characteristics, New high-efficient low-cost silicon-perovskite both ends stacked solar cell, cascade solar cell is photovoltaic cell technology frontier development and certainty
Trend.
Commercialization High-efficiency silicon solar battery generallys use pyramid flannelette light trapping structure.Silicon pyramid flannelette rises and falls high
Degree is usually at 1~20 μm, it can effectively increase light capture ability, to improve the short-circuit current density of battery.However, at this
The complicated surface texture structure of kind is difficult to the uniform perovskite film of deposition thickness.Calcium titanium with solwution method deposition thickness less than 1 μm
When mine film, solution gathers in the paddy between " pyramid ", so that being not covered with liquid on pyramidal pinnacle of a pagoda, this be will lead to
Pyramidal apex angle and rib can not be completely covered in final perovskite thin film.This phenomenon will lead to battery short circuit, and then reduce
Perovskite/crystal silicon lamination solar cell photoelectric conversion efficiency.In order to avoid this problem, gold of the prior art to silion cell
Word tower flannelette has carried out polishing and has polished processing.However, compared with the silion cell with pyramid flannelette light trapping structure, silicon solar
Photoelectric conversion efficiency after battery polishing can be reduced to about the 50% of original value.Therefore, this technical solution exists following insufficient:
First, polishing is carried out to silicon pyramid flannelette and polishes the photoelectric conversion efficiency that processing significantly reduces silicon solar cell；Second,
Increased polishing polishes the production cost that processing improves lamination solar cell, increases process and time, reduces production
Efficiency.Therefore, how micro-meter scale rise and fall pyramid flannelette substrate on preparation the uniform profiling perovskite thin film of all standing at
To realize high-efficiency and low-cost silicon-perovskite both ends lamination photovoltaic cell technology core problem.
Summary of the invention
The purpose of the present invention is to provide a kind of thickening suppressions of the liquid film of the uniform perovskite film of flannelette to climb crystallization preparation side in situ
Method, to solve the above technical problems.
To achieve the goals above, the present invention adopts the following technical scheme:
Crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette, comprising the following steps:
The first step prepares perovskite precursor sol or solution containing thickener: solvent, perovskite and thickener are mixed
Afterwards, perovskite precursor sol or solution that viscosity is not less than 2.5mPas are obtained；
The uniform coating of perovskite liquid film: second step the perovskite precursor sol of first step configuration or solution is coated
In the substrate with pyramid flannelette pattern, formation a layer thickness is less than the uniform imitative of the 60% of pyramid average characteristics height
Shape perovskite liquid film；Pyramid average characteristics altitude range is 5~20 μm；
Third step, the drying process of perovskite liquid film: being rapidly completed the drying process to perovskite liquid film, to obtain equal
Pyramid perovskite thin film is imitated in even all standing；
4th step, perovskite thin film go solvent heat treatment: by the perovskite thin film through being dried 90~150 DEG C into
The annealing of 10~120min of row removes residual solvent；
5th step, perovskite thin film go thickener to be heat-treated: by the 4th step treated perovskite thin film 100~
The annealing of 180 DEG C of 10~120min of progress removes thickener and crystal grain is made to grow up, and finally obtains all standing and imitates pyramid
The uniform perovskite thin film of flannelette.
Further, the drying process to perovskite liquid film is rapidly completed, specially in the outer normal direction solid phase in edges and corners part
Minimum thickness can be born not less than the outer normal direction perovskite thin film in edges and corners part with the ratio between the total amount of solute in liquid phase and design flow
With before the ratio between design thickness, the drying process of perovskite liquid film is completed；The total amount of solute includes shape in the solid phase and liquid phase
Still uncrystallized perovskite in the solid phase perovskite and liquid phase of crystalline nucleation.Design thickness is not less than 50nm；The minimum that can be born
The ratio between thickness and design thickness are not less than 10%；
Further, the solid phase perovskite of the forming core crystallization includes solid phase perovskite and existing for complex form
Perovskite.
Further, described be dried is degassing method or ventilation-degassing method.
Further, the mass percent of perovskite is 35~40% in perovskite precursor sol or solution.
Further, the thickener is hydrophilic macromolecular compounds；It is thickened in perovskite precursor sol or solution
The mass percent of agent is 1~30%.
Further, thickener is Sodium Polyacrylate, ethylene glycol or acrylic thickener.
Further, the thickener can volatilize removal during perovskite thin film is heat-treated, and not with calcium titanium
Mine and solvent react.
Further, the substrate of the pyramid flannelette pattern is silicon pyramid flannelette.
Further, the substrate of the pyramid flannelette pattern is the silicon pyramid flannelette coated with profiling tunnel layer, painting
It is covered with the silicon pyramid flannelette of profiling hole transmission layer or the silicon pyramid flannelette coated with profiling electron transfer layer.
Further, the chemical general formula of the perovskite is ABX3, wherein A is selected from alkylamine, alkali metal or combinations thereof, B
Selected from lead, tin or combinations thereof, X is selected from Br, Cl, I or combinations thereof.
Further, the quick finger is completed after the completion of first step coating, in 8s to the rapid draing of perovskite liquid film
Reason.It after having coated, is transferred in multithread air knife equipment within time-consuming about 5s, in additional gas knife dry 3s, total time-consuming about 8s.
Compared with the existing technology, the invention has the following advantages:
(1) present invention improves the viscosity of perovskite solution by addition thickener, and liquid film is inhibited to creep, fast using degassing method
Rapid-curing cutback is dry, completes film preparation.It avoids in the prior art, when perovskite thin film with solwution method deposition thickness less than 1 μm, solution
It is gathered in paddy between " pyramid ", so that the technical issues of being not covered with liquid on pyramidal pinnacle of a pagoda.
(2) present invention can be existed using solwution method under conditions of not carrying out polishing to silicon pyramid flannelette and polishing processing
The uniform profiling perovskite thin film of all standing is prepared in the pyramid flannelette substrate that micro-meter scale rises and falls, is able to maintain silicon solar
The advantage of battery-efficient rate realizes silicon-perovskite both ends lamination solar cell technology that photoelectric conversion efficiency is greater than 35%；
(3) polishing that the present invention eliminates silicon pyramid flannelette polishes processing, reduces silicon-perovskite laminate solar electricity
The production cost in pond, reduces waste of time, improves actual production speed.
Specific embodiment
Implementation method of the present invention is described further combined with specific embodiments below.
Embodiment 1
The preparation method of the uniform perovskite film of flannelette, comprising:
(1) preparation of the perovskite precursor sol containing thickener: using DMF as solvent, PbI2And CH3NH3I is solute, is matched
Perovskite colloidal sol processed, Sodium Polyacrylate are thickener, and three is uniformly mixed and obtains highly viscous perovskite precursor sol；Height is viscous
The perovskite precursor sol viscosity of degree is greater than in 2.5mPas；CH in highly viscous perovskite precursor sol3NH3PbI3's
Mass percentage concentration is 40%, and the mass percentage concentration of Sodium Polyacrylate is 10%；
(2) the uniform coating of perovskite liquid film: perovskite precursor sol is coated in by the way of banister brush coating
On silicon solar cell with pyramid flannelette pattern, one layer of flaxen uniform profiling perovskite with a thickness of 2 μm is formed
Liquid film.The thickness of profiling perovskite liquid film is less than the 60% of pyramid average characteristics height.
(3) it the drying process of perovskite liquid film: is completed in 3s using multithread air knife perovskite liquid film quickly drying method
Drying process to perovskite liquid film imitates pyramid perovskite thin film to obtain with a thickness of the uniform all standing of 400nm.
(4) perovskite thin film goes solvent heat treatment: the perovskite thin film through being dried is carried out 10min's at 90 DEG C
Annealing removes residual solvent.
(5) perovskite thin film goes thickener to be heat-treated: perovskite thin film is carried out to the annealing of 10min at 100 DEG C,
Removal thickener simultaneously makes crystal grain grow up, and finally obtain fine and close all standing imitates the uniform perovskite thin film of pyramidal flannelette.
Embodiment 2
The preparation method of the uniform perovskite film of flannelette, comprising:
(1) preparation of the perovskite precursor sol containing thickener: using DMSO as solvent, PbI2With FAI be solute, poly- third
Olefin(e) acid sodium is thickener, and three is uniformly mixed and obtains highly viscous perovskite precursor sol；Highly viscous perovskite presoma
Colloidal sol viscosity is greater than in 2.5mPas；FAPbI in highly viscous perovskite precursor sol3Mass percentage concentration be 35%,
The mass percentage concentration of Sodium Polyacrylate is 20%；
(2) the uniform coating of perovskite liquid film: perovskite precursor sol is coated in by the way of banister brush coating
On silicon solar cell with pyramid flannelette pattern, one layer of flaxen uniform profiling perovskite with a thickness of 4 μm is formed
Liquid film.The thickness of profiling perovskite liquid film is less than the 60% of pyramid average characteristics height.
(3) it the drying process of perovskite liquid film: is completed in 3s using pumping-ventilation perovskite liquid film quickly drying method
Drying process (pumping chamber air pressure: 300Pa is evacuated duration: 3s) to perovskite liquid film, to obtain with a thickness of the equal of 800nm
Pyramid perovskite thin film is imitated in even all standing.
(4) perovskite thin film goes solvent heat treatment: the perovskite thin film through being dried is carried out 10min's at 90 DEG C
Annealing removes residual solvent.
(5) perovskite thin film goes thickener to be heat-treated: perovskite thin film is carried out to the annealing of 10min at 100 DEG C,
Removal thickener simultaneously makes crystal grain grow up, and finally obtain fine and close all standing imitates the uniform perovskite thin film of pyramidal flannelette.
Embodiment 3
The preparation method of the uniform perovskite film of flannelette, comprising:
(1) preparation of the perovskite precursor sol containing thickener: using GBL as solvent, PbI2With FAI be solute, poly- third
Olefin(e) acid sodium is thickener, and three is uniformly mixed and obtains highly viscous perovskite precursor sol；Highly viscous perovskite presoma
Colloidal sol viscosity is greater than in 2.5mPas；FAPbI in highly viscous perovskite precursor sol3Mass percentage concentration be 35%,
The mass percentage concentration of Sodium Polyacrylate is 5%；
(2) the uniform coating of perovskite liquid film: perovskite precursor sol is coated in by the way of banister brush coating
On silicon solar cell with pyramid flannelette pattern, one layer of flaxen uniform profiling perovskite with a thickness of 3 μm is formed
Liquid film.The thickness of profiling perovskite liquid film is less than the 60% of pyramid average characteristics height.
(3) it the drying process of perovskite liquid film: is completed in 3s using pumping-ventilation perovskite liquid film quickly drying method
Drying process (pumping chamber air pressure: 50Pa is evacuated duration: 3s) to perovskite liquid film, to obtain with a thickness of the uniform of 500nm
Pyramid perovskite thin film is imitated in all standing.
(4) perovskite thin film goes solvent heat treatment: by the perovskite thin film through being dried in 120 DEG C of progress 60min
Annealing, remove residual solvent.
(5) perovskite thin film goes thickener to be heat-treated: perovskite thin film is carried out to the annealing of 30min at 130 DEG C,
Removal thickener simultaneously makes crystal grain grow up, and finally obtain fine and close all standing imitates the uniform perovskite thin film of pyramidal flannelette.
Embodiment 4
The preparation method of the uniform perovskite film of flannelette, comprising:
(1) preparation of the perovskite precursor sol containing thickener: using DMF as solvent, PbI2And CH3NH3I is solute, is matched
Perovskite colloidal sol processed, Sodium Polyacrylate are thickener, and three is uniformly mixed and obtains highly viscous perovskite precursor sol；Height is viscous
The perovskite precursor sol viscosity of degree is greater than in 2.5mPas；CH in highly viscous perovskite precursor sol3NH3PbI3's
Mass percentage concentration is 40%, and the mass percentage concentration of Sodium Polyacrylate is 10%；
(2) the uniform coating of perovskite liquid film: perovskite precursor sol is coated in by the way of banister brush coating
On silicon solar cell with pyramid flannelette pattern, one layer of flaxen uniform profiling perovskite with a thickness of 2 μm is formed
Liquid film.The thickness of profiling perovskite liquid film is less than the 60% of pyramid average characteristics height.
(3) it the drying process of perovskite liquid film: is completed in 3s using multithread air knife perovskite liquid film quickly drying method
Drying process to perovskite liquid film imitates pyramid perovskite thin film to obtain with a thickness of the uniform all standing of 400nm.
(4) perovskite thin film goes solvent heat treatment: by the perovskite thin film through being dried in 150 DEG C of progress 110min
Annealing, remove residual solvent.
(5) perovskite thin film goes thickener to be heat-treated: perovskite thin film is carried out to the annealing of 50min at 180 DEG C,
Removal thickener simultaneously makes crystal grain grow up, and finally obtain fine and close all standing imitates the uniform perovskite thin film of pyramidal flannelette.
In conclusion the above is only highly preferred embodiment of the present invention, it is all according to claims of the present invention and explanation
Equivalent modifications made by book belong to the range that the invention patent covers.
Claims (10)
1. crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette, which comprises the following steps:
The first step prepares perovskite precursor sol or solution containing thickener: after solvent, perovskite and thickener are mixed,
Obtain perovskite precursor sol or solution that viscosity is not less than 2.5mPas；
The uniform coating of perovskite liquid film: the perovskite precursor sol of first step configuration or solution are coated in tool by second step
In the substrate for having pyramid flannelette pattern, the 60% uniform profiling calcium that a layer thickness is less than pyramid average characteristics height is formed
Titanium ore liquid film；
Third step, the drying process of perovskite liquid film: being rapidly completed the drying process to perovskite liquid film, to obtain uniformly complete
Cover imitative pyramid perovskite thin film；
4th step, perovskite thin film go solvent heat treatment: the perovskite thin film through being dried is carried out 10 at 90~150 DEG C
The annealing of~120min removes residual solvent；
5th step, perovskite thin film go thickener to be heat-treated: by the 4th step treated perovskite thin film at 100~180 DEG C
The annealing of 10~120min is carried out, thickener is removed and crystal grain is made to grow up, all standing is finally obtained and imitates pyramidal suede
The uniform perovskite thin film in face.
2. crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette according to claim 1, special
Sign is, the drying process to perovskite liquid film is rapidly completed, specially molten in the outer normal direction solid phase in edges and corners part and liquid phase
The ratio between the total amount of matter and design flow can bear minimum thickness and design thickness not less than the outer normal direction perovskite thin film in edges and corners part
The ratio between before, complete perovskite liquid film drying process；The total amount of solute includes consolidating for forming core crystallization in the solid phase and liquid phase
Still uncrystallized perovskite in phase perovskite and liquid phase.
3. crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette according to claim 2, special
Sign is, the solid phase perovskite of the crystallization of forming core includes solid phase perovskite and with perovskite existing for complex form.
4. crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette according to claim 1, special
Sign is that described be dried is degassing method or ventilation-degassing method.
5. crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette according to claim 1, special
Sign is that the thickener is hydrophilic macromolecular compounds；The quality hundred of thickener in perovskite precursor sol or solution
Divide than being 1~30%.
6. crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette according to claim 1, special
Sign is that thickener is Sodium Polyacrylate, ethylene glycol or acrylic thickener.
7. crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette according to claim 1, special
Sign is, the thickener can volatilize removal during perovskite thin film is heat-treated, and not with perovskite and solvent hair
Raw reaction.
8. crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette according to claim 1, special
Sign is that the substrate of the pyramid flannelette pattern is silicon pyramid flannelette.
9. crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette according to claim 1, special
Sign is, the substrate of the pyramid flannelette pattern is silicon pyramid flannelette coated with profiling tunnel layer, to be coated with profiling empty
The silicon pyramid flannelette of cave transport layer or silicon pyramid flannelette coated with profiling electron transfer layer.
10. crystallization preparation method in situ is climbed in the liquid film thickening suppression of the uniform perovskite film of flannelette according to claim 1, special
Sign is that the chemical general formula of the perovskite is ABX3, wherein A be selected from alkylamine, alkali metal or combinations thereof, B be selected from lead, tin or
A combination thereof, X are selected from Br, Cl, I or combinations thereof.
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| CN110578174A (en) * | 2019-08-09 | 2019-12-17 | 北京工业大学 | Perovskite single crystal growth method capable of reducing nucleation number |
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