CN110635050A - Method for preparing high-quality perovskite thin film with assistance of pressure - Google Patents

Method for preparing high-quality perovskite thin film with assistance of pressure Download PDF

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CN110635050A
CN110635050A CN201910821531.XA CN201910821531A CN110635050A CN 110635050 A CN110635050 A CN 110635050A CN 201910821531 A CN201910821531 A CN 201910821531A CN 110635050 A CN110635050 A CN 110635050A
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thin film
perovskite
perovskite thin
pressure
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CN110635050B (en
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罗军生
贾春阳
万中全
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University of Electronic Science and Technology of China
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    • H—ELECTRICITY
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    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/80—Manufacture or treatment specially adapted for the organic devices covered by this subclass using temporary substrates
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    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells

Abstract

A method for preparing a high-quality perovskite thin film with pressure assistance belongs to the technical field of photoelectric thin film preparation. Firstly, preparing a perovskite precursor film on a substrate; then, oppositely placing the two substrates with the perovskite precursor films to enable the perovskite precursor films to be tightly attached together, applying pressure above the top film, heating and annealing the bottom film, and slowly growing perovskite crystals; and after the annealing is finished, taking down the substrate with the perovskite thin film on the top, thus obtaining the high-quality bottom perovskite thin film. The perovskite thin film prepared by the method has micron-sized grains, microsecond-level carrier life, high crystallinity, few crystal boundaries and low defect state density, effectively improves the photoelectric property and long-term stability of the perovskite thin film, and correspondingly improves the device performance.

Description

Method for preparing high-quality perovskite thin film with assistance of pressure
Technical Field
The invention belongs to the technical field of photoelectric film preparation, and particularly relates to a method for preparing a high-quality perovskite film under the assistance of pressure.
Background
In recent years, organic-inorganic hybrid perovskite materials (ABX)3，A＝CH3NH3 +、NHCHNH3 +、Cs+、Ru+、K+Etc., B ═ Pb2+And Sn2+Etc., X ═ Cl-、Br-And I-Etc.) are receiving attention from researchers by virtue of their advantages of high light absorption coefficient, adjustable band gap, long carrier diffusion length, solution-soluble processing flow, etc., and have been widely used in the fields of solar cells, light emitting diodes, photodetectors, etc. The preparation method of the perovskite thin film plays a decisive role in the parameters of crystallinity, compactness, grain size and the like, and correspondingly influences the performance of the device. At present, the preparation method of the perovskite thin film mainly comprises a one-step spin coating method, a two-step solution method, a vapor deposition method, a vapor auxiliary solution method and the like. However, since the perovskite thin film has a faster crystallization rate, the perovskite thin film prepared by the simple method generally has smaller crystal grains and more crystal boundaries, and accordingly causes defects of the crystal and the crystal boundaries, resulting in the recombination of current carriers and weakening the performance of the device.
Disclosure of Invention
The invention aims to provide a method for preparing a perovskite thin film with high crystallinity, large crystal grains and low defect state density under the assistance of pressure aiming at the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing a high-quality perovskite thin film through pressure assistance is characterized by comprising the following steps:
step 1, preparing a perovskite precursor film on a substrate;
step 2, reversely buckling the substrate A with the perovskite precursor film to the substrate B with the perovskite precursor film to enable the perovskite precursor film to be tightly attached together;
step 3, transferring the composite structure obtained in the step 2 to a heating table, applying pressure above the top thin film, annealing, and slowly growing a perovskite crystal;
and 4, after the annealing is finished, taking down the substrate A with the perovskite thin film, and obtaining the high-quality perovskite thin film on the substrate B.
Further, when the annealing treatment is carried out in the step 3, the pressure applied to the substrate A with the perovskite precursor thin film on the top is not more than 10000 Pa.
Further, the chemical general formula of the perovskite precursor thin film in the step 1 is ABX3Wherein A is CH3NH3 +(MA+)、NH2＝CHNH2 +(FA+)、C4H9NH3 +、Cs+、Rb+、K+B is Pb2+，Sn2+、Ge2+Etc., X is Cl-、Br-、I-And the like.
Further, the substrate in the step 1 is glass, flexible plastic, ITO conductive PEN, ITO conductive PET, FTO conductive glass, ITO conductive glass, AZO conductive glass, silver nanowire modified conductive glass, graphene modified conductive glass or carbon nanotube layer modified conductive glass, and the like.
Further, before preparing the perovskite precursor thin film in the step 1, an electron transport layer (TiO) can be deposited on the substrate2、SnO2ZnO, C60, PCBM, etc.) or hole transport layer (NiO)xPEDOT PSS, PTAA, etc.).
Further, the perovskite precursor film in the step 1 is prepared by adopting a one-step spin coating method, a two-step solution method, a vapor deposition method, a vapor auxiliary solution method, spraying, blade coating, roll-to-roll printing, slit coating, screen printing or other methods.
Further, the annealing temperature in the step 3 is 60-300 ℃, and the annealing time is 5-120 min.
The invention also provides application of the high-quality perovskite thin film obtained by the method in solar cells, light-emitting diodes or photodetectors. Preferably, applied to the light-absorbing layer of a perovskite solar cell.
Compared with the prior art, the invention has the beneficial effects that:
the perovskite thin film prepared by the method has micron-sized grains, microsecond-sized carrier life, high crystallinity, few crystal boundaries and low defect state density, the photoelectric property and the long-term stability of the perovskite thin film are effectively improved, and the performance of a device is correspondingly improved.
Drawings
FIG. 1 is a SEM morphology of the surface of a perovskite thin film prepared in a comparative example;
FIG. 2 is a schematic representation of the pressure-assisted production of high quality perovskite thin films of the present invention;
FIG. 3 is SEM topography of the surface of the perovskite thin film prepared in example 1;
FIG. 4 is SEM topography of the surface of the perovskite thin film prepared in example 2;
FIG. 5 is SEM topography of the surface of the perovskite thin film prepared in example 3;
FIG. 6 is SEM topography of the surface of the perovskite thin film prepared in example 4;
FIG. 7 is the 2D-GIXD results for perovskite thin films; wherein, (a) the perovskite thin film prepared in the comparative example; (b) the perovskite thin film prepared in example 3;
FIG. 8 shows the results of fluorescence tests of perovskite thin films prepared in comparative example and example 3 on a glass substrate; wherein (a) steady state fluorescence; (b) transient fluorescence;
FIG. 9 is a cross-sectional SEM of the application of perovskite thin films prepared in comparative example (a) and example 3(b) in a solar cell;
FIG. 10 is a graph of the performance of perovskite thin films prepared in comparative example and example 3 in solar cell applications; wherein (a) J-V performance, (b) long term air stability;
FIG. 11 is a schematic flow diagram of a pressure-assisted process for preparing high quality perovskite thin films in accordance with the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples.
Comparative example (one-step spin coating anti-solvent method)
The perovskite thin film is prepared by a one-step spin coating anti-solvent method, and the preparation method comprises the following specific steps:
(1) preparing a solution A: 103.92mg of CsI was dissolved in 200uL of DMSO and stirred well to give a solution A;
(2) preparing a solution B: 548.6mg of PbI277.07mg of PbBr2190.12mg of NH2＝CHNH2I (FAI), 21.84mg of CH3NH3Br (MABr) is dissolved in 1mL of mixed solvent of DMSO and DMF (the volume ratio of the DMF to the DMSO is 4: 1), and the solution is fully stirred to obtain a solution B;
(3) preparing a perovskite precursor solution: adding 34uL of the solution A obtained in the step 1 into the solution B obtained in the step 2, and fully stirring to obtain a perovskite precursor solution;
(4) spreading the perovskite precursor solution obtained in the step (3) on glass/FTO/TiO2And (3) respectively spin-coating the surface of the substrate for 10s and 45s at the rotation speeds of 1300 revolutions and 5000 revolutions, dripping 200uL of chlorobenzene antisolvent 12s before the second step of spin-coating is finished, heating and annealing at 110 ℃ for 80min after the spin-coating is finished, and growing perovskite crystals to obtain the perovskite thin film.
FIG. 1 shows SEM morphology of the surface of a perovskite thin film prepared by a comparative example, and the average grain size of the perovskite thin film is 288 nm.
Example 1
Referring now to FIG. 2, the perovskite thin film is prepared under 1250Pa by the following steps:
spreading the perovskite precursor solution prepared in the step (3) of the comparative example on glass/FTO/TiO2Respectively spin-coating the surface of the substrate for 10s and 45s at the rotation speeds of 1300 revolutions and 5000 revolutions, dropwise adding a chlorobenzene antisolvent 12s before the second step of spin-coating is finished, and obtaining a perovskite precursor film after the spin-coating is finished; the two perovskite precursor films obtained by the method are oppositely placed, then transferred to a heating table, and the pressure of 1250Pa is applied above the top film for annealing treatment, wherein the annealing temperature is 110 ℃, the time is 80min, and high-quality perovskite crystals are slowly grown; and after the annealing is finished, taking down the top film to obtain the bottom perovskite film with high quality.
FIG. 3 is an SEM surface morphology of the perovskite thin film prepared in example 1(1250Pa), and the average grain size is 770 nm.
Example 2
Referring now to FIG. 2, the perovskite thin film is prepared under 2500Pa pressure by the following steps:
spreading the perovskite precursor solution prepared in the step (3) of the comparative example on glass/FTO/TiO2Respectively spin-coating the surface of the substrate for 10s and 45s at the rotation speeds of 1300 revolutions and 5000 revolutions, dropwise adding a chlorobenzene antisolvent 12s before the second step of spin-coating is finished, and obtaining a perovskite precursor film after the spin-coating is finished; the two perovskite precursor films obtained by the method are oppositely placed, then transferred to a heating table, and the pressure of 2500Pa is applied to the upper part of the top film for annealing treatment, wherein the annealing temperature is 110 ℃, the time is 80min, and high-quality perovskite crystals are slowly grown; and after the annealing is finished, taking down the top film to obtain the bottom perovskite film with high quality.
FIG. 4 is an SEM topography of the surface of the perovskite thin film prepared in example 2(2500Pa), and the average grain size is 1000 nm.
Example 3
Referring now to FIG. 2, the perovskite thin film is prepared under 5000Pa pressure by the following steps:
spreading the perovskite precursor solution prepared in the step (3) of the comparative example on glass/FTO/TiO2Respectively spin-coating the surface of the substrate for 10s and 45s at the rotation speeds of 1300 revolutions and 5000 revolutions, dropwise adding a chlorobenzene antisolvent 12s before the second step of spin-coating is finished, and obtaining a perovskite precursor film after the spin-coating is finished; the two perovskite precursor films obtained by the method are oppositely placed, then transferred to a heating table, and the pressure of 5000Pa is applied to the upper part of the top film for annealing treatment, wherein the annealing temperature is 110 ℃, the time is 80min, and high-quality perovskite crystals are slowly grown; and after the annealing is finished, taking down the top film to obtain the bottom perovskite film with high quality.
FIG. 5 is an SEM image of the surface of the perovskite thin film prepared in example 3(5000Pa), and the average grain size is 1100 nm.
Example 4
Referring now to FIG. 2, the perovskite thin film is prepared under 12500Pa pressure by the following steps:
will be paired withSpreading the perovskite precursor solution prepared in the proportion step (3) on glass/FTO/TiO2Respectively spin-coating the surface of the substrate for 10s and 45s at the rotation speeds of 1300 revolutions and 5000 revolutions, dropwise adding a chlorobenzene antisolvent 12s before the second step of spin-coating is finished, and obtaining a perovskite precursor film after the spin-coating is finished; the two perovskite precursor films obtained by the method are oppositely placed, then transferred to a heating table, and the pressure of 12500Pa is applied to the upper part of the top film for annealing treatment, wherein the annealing temperature is 110 ℃, the time is 80min, and high-quality perovskite crystals are slowly grown; and after the annealing is finished, removing the top thin film to obtain a bottom perovskite thin film with larger grains and fragment defects at the grain boundary.
FIG. 6 is an SEM image of the surface of the perovskite thin film prepared in example 4(12500Pa), wherein the average grain size is 2000nm, but the grain boundary has fragment defects.
Example 5
By replacing the top perovskite precursor thin films of examples 1-4 with glass or FTO, otherwise unchanged, the resulting bottom perovskite thin films have large grains, but have more pinholes and relatively poor overall quality.
FIG. 7 is the 2D-GIXD results for perovskite thin films; wherein, (a) the perovskite thin film prepared in the comparative example; (b) the perovskite thin film prepared in example 3; it can be seen from the figure that the perovskite diffraction peaks (110), (220) and (310) of example 3 are significantly enhanced, indicating that the perovskite thin film prepared by example 3 has more excellent crystallinity. FIG. 8 shows the results of fluorescence measurements on glass substrates of perovskite thin films prepared in comparative example and example 3, respectively, as comparative and pressure, (a) steady state fluorescence; (b) transient fluorescence; it can be seen from the figure that both the steady-state fluorescence intensity and the transient fluorescence lifetime of the latter are significantly enhanced, indicating that the perovskite thin film prepared in example 3 has fewer defect states. In particular, the transient fluorescence lifetime of the perovskite thin film prepared in example 3 reaches microsecond level (1119 ns). According to the test results of the comparative example and the example 3, the perovskite thin film prepared by pressure assistance has the advantages of micron-sized grains, microsecond-sized carrier life, high crystallinity, few grain boundaries, low defect state density and the like, and is beneficial to improving the performance of the perovskite thin film and a corresponding device.
Example 6
The perovskite thin films prepared in the comparative example and the example 3 are respectively applied to the solar cell, and the method specifically comprises the following steps:
(1) solution preparation: compact TiO 22Preparing a precursor solution: firstly, 2.53mL of ethanol is added into a No. 1 reagent bottle, and 369 mu L of tetraisopropyl titanate is added dropwise under the condition of stirring and is continuously stirred; then, 2.53mL of ethanol was added to reagent bottle No. 2, followed by 35. mu.L of 2M HCl aqueous solution with constant stirring; finally, the solution in the No. 2 reagent bottle is added into the No. 1 reagent bottle drop by drop, stirred for a plurality of hours and filtered by a filter head with the diameter of 0.22 mu m to obtain clear and transparent compact TiO2A precursor liquid. Mesoporous TiO 22Preparing a dispersion liquid: diluting 18NR-T and ethanol according to the mass ratio of 1:7, and continuously stirring and ultrasonically dispersing 18NR-T in ethanol uniformly. Preparing a hole transport layer solution: 15mg of PTAA and a quantity of LAD were dissolved in 1mL of toluene with a LAD/PTAA molar ratio (relative to the monomers of PTAA) of 5% and then stirred overnight.
(2) Cleaning conductive glass: and ultrasonically cleaning the conductive glass FTO in deionized water containing detergent, a saturated ethanol solution of KOH, ethanol, acetone and deionized water for 30 minutes, blow-drying by using nitrogen, and treating the FTO substrate in ultraviolet ozone for 30 minutes to remove organic residues on the surface.
(3) Compact TiO 22Layer preparation: compact TiO prepared in the step 12The precursor solution is spin-coated on a conductive glass substrate, then is heated for 15min at the temperature of 150 ℃, and then is annealed for 30min at the temperature of 500 ℃ in a muffle furnace and is slowly cooled to the room temperature.
(4) Mesoporous TiO 22Layer preparation: the mesoporous TiO prepared in the step 12The dispersion is spin-coated on the dense TiO prepared in step 32On the layer, it was then heated at 125 ℃ for 10min and at 500 ℃ for 30min, respectively.
(5) Preparing a perovskite layer: mesoporous TiO prepared in step 42The perovskite layer was prepared on the layer in the same manner as in comparative example or example 3, and the corresponding cells were marked respectivelyFor comparison or pressure.
(6) And (3) preparing a hole transport layer, namely spin-coating the hole transport layer solution prepared in the step (1) on the perovskite layer prepared in the step (5), wherein the rotation speed and the time of the spin-coating are 3000rpm and 30s respectively.
(7) And (3) gold-plated electrode evaporation: and (5) evaporating a gold electrode on the hole transport layer prepared in the step (6) by using a resistance evaporation vacuum coating instrument to finish the preparation of the battery.
FIG. 9 is a cross-sectional SEM of the application of perovskite thin films prepared in comparative example (a) and example 3(b) in a solar cell; from the SEM sectional view, it can be clearly seen that the multilayer structure of the perovskite solar cell and the perovskite thin film prepared based on example 3 have the characteristics of compactness and large crystal grains, and the perovskite layer is composed of single-layer perovskite crystals in the vertical direction. The large-grain perovskite thin film is beneficial to reducing the defect state density of the perovskite thin film, so that the efficient and stable perovskite solar cell is prepared.
FIG. 10(a) is a graph of the J-V performance of perovskite thin films prepared in comparative example and example 3 in solar cell applications; cells based on the perovskite thin film prepared in example 3 were exposed to a standard simulated sunlight (100mW cm)-2) Photoelectric conversion efficiency (J) of 20.74% was obtainedSC＝23.15mA cm-2,VOC1.12V, FF 0.80) which is significantly higher than the cell performance based on the comparative perovskite thin film (PCE 18.11%, JSC＝22.73mA cm-2,VOC1.06V, FF 0.75). FIG. 10(b) is a graph showing long-term environmental stability of perovskite thin films prepared in comparative example and example 3 applied to a solar cell; the two were separately left in an atmospheric environment for 60 days (room temperature, 50-85% relative humidity), and the cell efficiency of the perovskite thin film prepared based on example 3 remained the initial 91%, while the perovskite thin film cell prepared based on the comparative example remained only the initial 35%. The high-quality perovskite thin film prepared based on pressure assistance is beneficial to improving the photovoltaic performance and long-term stability of the solar cell.
The above description is only illustrative of the present invention and is not intended to limit the scope of the present invention. Any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the scope of the technical solution of the present invention.

Claims (7)

1. A method for preparing a high-quality perovskite thin film through pressure assistance is characterized by comprising the following steps: firstly, preparing a perovskite precursor film on a substrate; then, oppositely placing the two substrates with the perovskite precursor films to enable the perovskite precursor films to be tightly attached together, applying pressure on the substrate with the perovskite precursor film at the top, and heating and annealing the film at the bottom; and after the annealing is finished, taking down the substrate with the perovskite thin film on the top, and thus obtaining the high-quality perovskite thin film.
2. A method for pressure-assisted production of high quality perovskite thin films according to claim 1, characterized in that the annealing treatment is carried out by applying a pressure of not more than 10000Pa to the substrate with the perovskite precursor thin film on top.
3. The pressure-assisted preparation method of a high-quality perovskite thin film according to claim 1, wherein the annealing temperature is 60-300 ℃ and the annealing time is 5-120 min.
4. The method of pressure-assisted production of high quality perovskite thin film according to claim 1, wherein the substrate is glass, flexible plastic, ITO conductive PEN, ITO conductive PET, FTO conductive glass, ITO conductive glass, AZO conductive glass, silver nanowire modified conductive glass, graphene modified conductive glass or carbon nanotube layer modified conductive glass.
5. A method for pressure-assisted production of high quality perovskite thin film according to claim 1, characterized in that an electron-transporting layer or a hole-transporting layer is deposited on the substrate before producing the perovskite precursor thin film.
6. The method for pressure-assisted preparation of a high-quality perovskite thin film according to claim 1, wherein the perovskite precursor thin film is prepared by a one-step spin coating method, a two-step solution method, a vapor deposition method, a vapor-assisted solution method, spray coating, blade coating, roll-to-roll printing, slit coating or screen printing method.
7. Use of a high quality perovskite thin film obtained by the method of any one of claims 1 to 6 in solar cells, light emitting diodes or photodetectors.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112002814A (en) * 2020-07-29 2020-11-27 隆基绿能科技股份有限公司 Preparation method of perovskite solar cell based on solid-phase reaction
CN113540270A (en) * 2021-06-30 2021-10-22 杭州电子科技大学 Method for obtaining flat, uniform and compact perovskite film
CN116004229A (en) * 2023-01-04 2023-04-25 吉林大学 Chlorophyll-modified CsPbCl3: yb3+ perovskite film and preparation method and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109888110A (en) * 2017-12-06 2019-06-14 中国科学院大连化学物理研究所 A kind of preparation method of laminated type perovskite solar battery

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109888110A (en) * 2017-12-06 2019-06-14 中国科学院大连化学物理研究所 A kind of preparation method of laminated type perovskite solar battery

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112002814A (en) * 2020-07-29 2020-11-27 隆基绿能科技股份有限公司 Preparation method of perovskite solar cell based on solid-phase reaction
CN113540270A (en) * 2021-06-30 2021-10-22 杭州电子科技大学 Method for obtaining flat, uniform and compact perovskite film
CN113540270B (en) * 2021-06-30 2023-06-30 杭州电子科技大学 Method for obtaining flat, uniform and compact perovskite film
CN116004229A (en) * 2023-01-04 2023-04-25 吉林大学 Chlorophyll-modified CsPbCl3: yb3+ perovskite film and preparation method and application thereof
CN116004229B (en) * 2023-01-04 2023-12-05 吉林大学 Chlorophyll-modified CsPbCl3: yb3+ perovskite film and preparation method and application thereof

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