Method for preparing perovskite thin film by dynamic spin coating

A perovskite and spin-coating technology, applied in semiconductor/solid-state device manufacturing, semiconductor devices, electrical components, etc., can solve the problem of a large number of pinholes in the microscopic appearance of perovskite films, affecting battery conversion efficiency and stability, and perovskite Problems such as uneven distribution of ore precursor liquid, to achieve high photoelectric conversion efficiency, reduced recombination probability, and excellent photoelectric performance

Active Publication Date: 2018-10-12
NANJING UNIV OF SCI & TECH
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Problems solved by technology

However, there are many problems in the quality of its film formation.
[0004] Snaith et al. used the static spin coating method to prepare CH 3 NH 3 PB 3-x Cl x Perovskite film, the microscopic morphology of the film mainly has a large number of pinholes, low coverage, and uneven grain size, so the obtained cell efficiency is only 4.41% (CarnieM J.A one-step low temperature processing route for organolead halideperovskite solar cells [J].Chemical Communications,2013,49(72):7893.)
Zhao et al. used the same method to prepare FAPbI 3-x Cl x Perovskite thin film, due to its low crystallinity, low coverage, and pinholes, has a large density of defect states, so that the conversion efficiency of the prepared solar cell is only 7.51% (Lv S, et al. One-step, solution -processed formamidinium lead trihalide (FAPbI (3-x) Cl (x) )formesoscopic perovskite-polymer solar cells.[J].Physical ChemistryChemicalPhysics Pccp,2014,16(36):19206-19211.)
Therefore, due to the uneven distribution of the perovskite precursor solution in the process of preparing the film by the static spin coating method, a large number of pinholes and other defects appear in the microscopic morphology of the perovskite film, resulting in poor photoelectric performance and affecting the conversion efficiency of the battery. and stability

Method used

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  • Method for preparing perovskite thin film by dynamic spin coating
  • Method for preparing perovskite thin film by dynamic spin coating
  • Method for preparing perovskite thin film by dynamic spin coating

Examples

Experimental program
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Effect test

Embodiment 1

[0027] 1) Ultrasonic cleaning of the glass with detergent, deionized water, absolute ethanol, and acetone, followed by ultraviolet and ozone cleaning;

[0028] 2) Combine MAI and PbI 2 According to the ratio of 1:1, it was dissolved in the mixed solution of DMF and DMSO with a volume ratio of 4:1, stirred and reacted at 70°C for 12 hours, and 1M MAPbI was prepared. 3 Perovskite precursor;

[0029] 3) Put the washed glass slide on the spin coater, add 200μm dense layer solution dropwise, spin coat at 1000rpm for 10s, then spin coat at 3500rpm for 35s, then place the slide on a heating plate at 125°C for 5min and anneal Take it off, wait for cooling to room temperature for the second spin coating;

[0030] 4) Place the glass substrate after the second spin coating on a heating plate at 125°C, raise the temperature by 25°C every 2 minutes, and keep it at 500°C for 1.5-2h;

[0031] 5) Set the parameters of the spin coater, high speed 5000rmp, 15s; low speed 3500rmp, 45s;

[00...

Embodiment 2

[0038] 1) Ultrasonic cleaning of the glass with detergent, deionized water, absolute ethanol, and acetone, followed by ultraviolet and ozone cleaning;

[0039] 2) CsI, FAI and PbI 2 According to the ratio of 1:9:10, it was dissolved in the mixed solution of DMF and DMSO with a volume ratio of 4:1, and stirred and reacted for 12 hours at 70 degrees to prepare 1M Cs 0.1 FA 0.9 PB 3 Perovskite precursor;

[0040] 3) Put the washed glass slide on the spin coater, add 200μm dense layer solution dropwise, spin coat at 1000rpm for 10s, then spin coat at 3500rpm for 35s, then place the slide on a heating plate at 125°C for 5min. Take it off, wait for cooling to room temperature for the second spin coating;

[0041] 4) Place the glass substrate after the second spin coating on a heating plate at 125°C, raise the temperature by 25°C every 2 minutes, and keep it at 500°C for 1.5-2h;

[0042] 5) Set the parameters of the spin coater, high speed 6000rmp, 15s; low speed 4000rmp, 45s; ...

Embodiment 3

[0047] This embodiment is basically the same as Embodiment 1, the only difference is that the rotational speed of the high-speed spin coating is 4000 rpm. The film prepared in this embodiment, its SEM picture is as follows figure 2 As shown in (c), the microscopic morphology of the perovskite film is observed to have uniform grains, no pinholes, and complete coverage.

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Abstract

The invention discloses a method for preparing a perovskite thin film by dynamic spin coating. According to the method, a perovskite APbX<3> precursor liquid is directly spin coated on a substrate with a clean surface at high-speed rotation of 4,500-6,000rmp; then an anti solvent is dropwise added to the high-speed spin coated thin film surface at low-speed rotation of 3,000-4,000rmp to obtain a lead halide thin film; and finally, annealing treatment is preformed at a temperature of 80-110 DEG C for 10-30min to obtain the APbX<3> perovskite thin film. The perovskite thin film is prepared by adopting the dynamic spin coating method in the invention; compared with a static spin coating method, the method disclosed in the invention is high in repeatability, simple in operation, high in controllability and wide in applicable range; and the prepared perovskite thin film is high in degree of crystallinity, large in grain size, high in uniformity, free of pin holes, high in coverage rate, lowers trap density for promoting carrier recombination, excellent in photoelectric performance, and has wide application prospect in commercial preparation of a perovskite solar cell.

Description

technical field [0001] The invention belongs to the field of solar cell device preparation, and relates to a method for preparing a perovskite thin film by dynamic spin coating. Background technique [0002] Perovskite material (structural formula ABX 3 ) has been used in solar cells, electroluminescent diodes, photodetectors and semiconductor Fields such as lasers show great application potential. [0003] In just seven years, the conversion efficiency of perovskite solar cells has risen from 3.8% to 22.7%. Although the conversion efficiency of perovskite solar cells has made great breakthroughs, there are still some problems to be solved in the device, such as stability, large-area preparation, low toxicity and repeatability. Since high-quality perovskite films are the key to high-performance devices, perovskite films with high crystallinity, high uniformity, and low defect density are prerequisites for obtaining devices with high stability and high conversion efficienc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01L51/42H01L51/48H01L51/46
CPCH10K71/12H10K85/30H10K30/00Y02E10/549
Inventor 曾秋桂胡延强邱婷白帆阮伟张树芳
Owner NANJING UNIV OF SCI & TECH
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