Columnar Grain Growth of Lead-Free Double Perovskite Using Mist Deposition Method for Sensitive X-ray Detectors

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For Table of Contents Use Only

“Columnar Grain Growth of Lead-Free Double Perovskite using Mist Deposition Method for

Sensitive X-ray Detectors”

Yuki Haruta, Shinji Wada, Takumi Ikenoue, Masao Miyake, and Tetsuji Hirato

TOC GRAPHICS

Synopsis

Cs2AgBiBr6 films with columnar grain structures are fabricated via the mist deposition method. In

this method, the re-dissolution capability of the precursor solution is a key factor promoting the

grain growth on the film surface, leading to columnar growth. An X-ray detector based on the

Cs2AgBiBr6 thick films with columnar grains exhibits a high sensitivity of 487 μC Gyair−1 cm−2.

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Supporting Information

Columnar Grain Growth of Lead-Free Double Perovskite

Using Mist Deposition Method for Sensitive X-ray Detectors

Yuki Haruta, Shinji Wada, Takumi Ikenoue*, Masao Miyake, and Tetsuji Hirato

Graduate School of Energy Science, Kyoto University, Kyoto 606-8501, Japan

*E-mail: ikenoue.takumi.4m@kyoto-u.ac.jp

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Experimental

Preparation of MAPbBr3 Films

To prepare the MAPbBr3 precursor solution, MABr (Sigma-Aldrich, 99%) and PbBr2

(Sigma-Aldrich, 98%) were dissolved in DMF, so that the MAPbBr3 concentration was 120 mM.

The MAPbBr3 films were deposited on glass substrates via the mist deposition method. The

fabrication conditions are shown in Table S1.

Table S1. Fabrication conditions for MAPbBr3

Solution concentration

120 mM MAPbBr3

Solvent

DMF

Substrate temperature

120 °C

Carrier gas

N2, 0.6 L min−1

Dilution gas

N2, 4.4 L min−1

Stage

1.00 mm s−1 × 30 cycles

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Figure S1. (a) A photograph and (b) XRD pattern of the prepared Cs2AgBiBr6 powders. (c–e)

Saturation test by adding (c) 4 mL, (d) 5 mL, and (e) 6 mL DMSO-DMF solvent to 1.16 mmol

Cs2AgBiBr6 powders.

To investigate the saturation concentration of Cs2AgBiBr6 for the solvent mixture of DMSO

and DMF (1:1, v/v), we added the solvent to 1.16 mmol Cs2AgBiBr6 powders (Figure S1a, b). As

shown in Figures S1c and S1d, white precipitates remained even after 3 hours of stirring. The

white precipitates seemed to be CsBr. After adding a total solvent amount of 6 mL, complete

dissolution was confirmed (Figure S1e). Based on the above results, the saturation concentration

was identified to be 193–232 mM. These experiments were performed at 20±5 °C.

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Figure S2. EDX spectrum and the corresponding atomic ratio of the Cs2AgBiBr6 film.

Figure S3. Histogram of thicknesses measured at randomly selected points in the 1.9-μm-thick

Cs2AgBiBr6 film.

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Figure S4. (a) Schematic of the mist droplets reaching the substrate. (b) SEM images of the

precipitation formed from a mist droplet.

To observe the precipitation formed from a mist droplet, we focused on the edge on the

substrate, which is only reached by few mist droplets (Figure S4a), and found an isolated circular

precipitation (Figure S4b). The SEM observation revealed that the diameter was approximately 7

μm, and the grain size was less than 100 nm.

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Figure S5. Cross-sectional SEM images of the Cs2AgBiBr6 films prepared at the substrate

temperatures of (a) 130, (b) 160, (c) 170, and (d) 190 °C.

Figure S6. Surface SEM images of the Cs2AgBiBr6 films prepared at the substrate temperatures

of (a) 110, (b) 130, (c) 150, (d) 160, (e) 170, and (f) 190 °C.

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Figure S7. XRD patterns of the Cs2AgBiBr6 films prepared at 110–210 °C.

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Figure S8. Correlation between (100)-orientation/(111)-orientation and substrate temperature.

The crystal orientation of (hkl) plane was quantified using the orientation factor F(hkl) defined by

the following equation:

𝐹(ℎ𝑘𝑙) =

𝐼(ℎ𝑘𝑙)

⁄𝐼

(220) sample

𝐼(ℎ𝑘𝑙)

⁄𝐼

(220) reference

where I(hkl) is the intensity of the peak derived from the (hkl) plane.

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Figure S9. (a, b) surface and (c, d) cross-sectional SEM images of the Cs2AgBiBr6 film prepared

from the 2.5 mM solution. The other fabrication conditions are summarized in Table S2.

Table S2. Fabrication conditions for Cs2AgBiBr6 film

Substrate temperature

150 °C

Carrier gas

N2, 0.4 L min−1

Dilution gas

N2, 4.6 L min−1

Stage

0.16 mm s−1 × 200 cycles

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Figure S10. (a) Cross-sectional SEM image and (b) XRD pattern of the MAPbBr3 film and the

reference pattern of cubic MAPbBr31.

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