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Pinhole-free large-area controllable growth perovskite film forming process

A large-area, perovskite technology, applied in sustainable manufacturing/processing, climate sustainability, final product manufacturing, etc., can solve the problems of uncontrollable evaporation and reaction rates of organic and inorganic sources, rough surface of thin films, cavity The body is easy to cause pollution and other problems, and achieves the effect of controllable large-area dense film-forming technology without pinholes, improving film quality and avoiding shrinkage.

Active Publication Date: 2020-09-25
ZHEJIANG ZHENENG TECHN RES INST +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] 1) The ETL layer cannot match the polarity of the perovskite and the substrate to achieve the purpose of reducing the activation energy of nucleation and accelerating nucleation, and the polarity mismatch in the local area leads to obvious shrinkage
[0013] 2) Due to uncontrollable crystal nucleation and growth, the underlying PbI 2 The rough surface of the film makes the two-step spin coating unfavorable for the subsequent morphology control of perovskite film formation
[0014] 3) The one-step spin coating method reacts faster, and the high-boiling point mixed solvent DMF and DMSO have inconsistent volatilization speeds in different regions due to the increase in area during the stripping process, making it difficult to control the nucleation rate during the crystallization process, resulting in the inability to release internal stress and form Pore ​​structure defects such as pinholes; mixed solvent atmosphere during spin coating may affect the crystallization process of perovskite
[0015] 4) In the one-step spin coating method, the requirements on the dropping time and the dropping process of the stripping agent are relatively strict, especially in the process of area enlargement, the process window is narrower, and it is greatly affected by the operation of the operator
[0016] 5) Under the same vacuum degree, co-evaporation cannot control the evaporation rate and reaction rate of organic and inorganic sources, and it is easy to cause pollution to the cavity

Method used

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  • Pinhole-free large-area controllable growth perovskite film forming process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] According to the ratio of N:Sn=0.02:1, weigh 9.57mg of hexadecyldimethylbenzyl ammonium chloride raw material and dissolve it in 13mL of deionized water, filter it for 30min after ultrasonication, and then use a pipette Pipette 80 μL of liquid and drop it vertically on the ETL layer SnO 2 Above, rotate at 4000rpm / 30s after the liquid is spread, anneal at 100°C for 10min after rotation, and the film thickness of the obtained low surface energy material substrate is about 20nm.

[0041] Place the low surface energy material substrate sample obtained above in a thermal evaporation, the sample is installed in the middle of the turntable, the turntable speed is set to 1krpm / min, and about 1.30g of PbI is placed in the cavity 2 Powder, in a vacuum of 4*10 －6 torr pressure, for Pb I 2 The film is pre-steamed, the thermal evaporation power supply voltage is adjusted to 0.82V, the current is 125A, the pre-steaming rate is controlled to 0.05nm / s, and it is reset to zero after t...

Embodiment 2

[0044] According to the ratio of N:Sn=0.04:1, weigh 19.14mg of hexadecyldimethylbenzyl ammonium chloride raw material, dissolve it in 3mL deionized water, filter it after ultrasonic for 30min, and then use a pipette Pipette 80 μL of liquid and drop it vertically on the ETL layer SnO 2 Above, rotate at 4000rpm / 30s after the liquid is spread, anneal at 100°C for 10min after rotation, and the film thickness of the obtained low surface energy material substrate is about 20nm. Place the low surface energy material substrate sample obtained above in a thermal evaporation, the sample is installed in the middle of the turntable, the turntable speed is set to 1krpm / min, and about 1.30g of PbI is placed in the cavity 2 Powder, in a vacuum of 4*10 － 6 torr pressure, for PbI 2 The film is pre-steamed, the thermal evaporation power supply voltage is adjusted to 0.82V, the current is 125A, the pre-steaming rate is controlled to 0.05nm / s, and it is reset to zero after the pre-steaming rea...

Embodiment 3

[0047] 2 mg of 4,4'-((methyl(4-sulfonyl)amino)bis(propane-3,1-diyl))bis(dimethyl-ammoniumdiyl)bis-(butane-1- Sulfonate) (MSAPBS) was dissolved in 1 mL of MeOH and AcOH with a volume ratio of 0.97:0.03, sonicated for 30 min and then filtered for use. Then pipette 80 μL of liquid and drop it vertically on the ETL layer SnO 2 Above, after the liquid is spread, the spin coating speed is 4000rpm / 30s, the annealing temperature is set at 100°C and the annealing time is 10min, and the film thickness of the low surface energy amphoteric small molecule material substrate is 8-9nm.

[0048] Place the substrate sample obtained above in a thermal evaporation, the sample is installed in the middle of the turntable, the turntable speed is set at 1krpm / min, and about 1.30g of PbI is placed in the cavity 2 Powder, thermal evaporation power supply voltage adjusted to 0.82V, current to 125A, in a vacuum of 4*10 －6 torr pressure, for PbI 2 The film is pre-steamed, the pre-steaming rate is contr...

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Abstract

The invention relates to a pinhole-free large-area controllable growth perovskite film forming process. The process comprises the following steps: step 1, preparing a low-surface-energy material substrate; step 2, depositing a PbI2 layer by adopting thermal evaporation; and step 3, spin-coating an isopropanol solution of MAI / FAI on the PbI2 thin film by adopting a spin-coating method. The method has the beneficial effects that the low-surface-energy material for large-area thermal evaporation and improvement of the quality of the film is provided, and deposition of a PbI2 layer is enhanced while nucleation activation energy is reduced. The reaction is completely carried out by adopting a spin-coating process, and the bottom uneven surface can be covered better. The low surface energy additive is used for better matching the polarity of the substrate and the polarity of the perovskite layer, the shrinkage cavity phenomenon caused by the change of local hydrophilicity and hydrophobicityis effectively avoided, the crystal quality is effectively regulated and controlled while the film forming quality is improved, and a controllable large-area compact pinhole-free film forming technology is realized.

Description

technical field [0001] The invention relates to the field of perovskite solar cells, and in particular includes a large-area controllable growth perovskite film-forming process without pinholes. Background technique [0002] At present, the highest certified efficiency of small-area organic-inorganic hybrid perovskite solar cells reaches 25.2%, and the rapid rise of its efficiency has attracted widespread attention. Despite the rapid development of perovskite solar cells, most of them are based on small-scale laboratory research results, which is not conducive to their commercial development. At present, the key problem facing the area enlargement of perovskite solar cells is to prepare high-quality perovskite films. Due to the existence of substrate impurities in the film-forming process, the local hydrophilicity and hydrophobicity of the substrate surface change, which often causes shrinkage cavities. The introduction of defects such as pinholes and protrusions seriously ...

Claims

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Application Information

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IPC IPC(8): H01L51/48H01L51/42
CPCH10K71/15H10K71/16H10K71/12H10K30/15Y02P70/50
Inventor 寿春晖盛江赵敏闫宝杰闫锦张永强杨伟创叶继春丁莞尔
Owner ZHEJIANG ZHENENG TECHN RES INST
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