Growth mechanism, phase transition and optical properties of large-size and high-quality perovskite CH3NH3PbCl3 single crystal

Nan Rui-Hua; Wu Chun-Yan; Liu Teng; Luo Jia-Xin; Wei Yong-Xing; Jian Zeng-Yun

doi:10.7498/aps.72.20230097

Abstract

According to the phenomenon that the solubility of CH₃NH₃PbCl₃ decreases with the increase of temperature in different solvents, CH₃NH₃PbCl₃ perovskite single crystal with a maximum dimension of 11 mm × 11 mm × 2 mm is grown by introducing a high-quality seed crystal via the seed-induced inverse temperature crystallization method in this work. X-ray diffraction and Rietveld refinements show that the full widths at half maximum (FWHM) of CH₃NH₃PbCl₃ single crystal diffraction peaks are 0.1527°, 0.1353°, 0.2295° and 0.3452°, corresponding to the crystal plane indices of (100), (200), (300) and (400), respectively. And there are no miscellaneous peaks, indicating a good crystal quality. As a result, CH₃NH₃PbCl₃ single crystal is of cubic phase at room temperature, its space group belongs to Pm

$ \bar{3} $

m, and the lattice constant is a = 0.56877 nm. The surface morphology and growth mechanism of CH₃NH₃PbCl₃ crystal are investigated by using a polarizing microscope. It is found that its growth mechanism follows the step horizontal growing mechanism of smooth interface, and its growth direction (that is, step movement direction) is along the outward normal direction of the step. The structural symmetry of CH₃NH₃PbCl₃ crystal is studied by variable temperature Raman spectroscopy, which reveals an orthogonal-tetragonal phase transition at 160 K. But the tetragonal phase structure is not stable, and its temperature range is very narrow. As temperature rises gradually, the tetragonal phase again transforms into a cubic phase (Pm

$\bar{3}$

m). Results of UV-Vis-NIR absorption and photoluminescence spectra show that the absorption cutoff of CH₃NH₃PbCl₃ crystal is about 442 nm, and the photoluminescence peak is 450 nm. Thereupon, its band gap is obtained to be about 2.93 eV by a linear fit of Tauc formula, which is slightly higher than the theoretical value of 2.55 eV calculated by first principles simulation. We believe that it is related to the seed crystal, which is introduced into the crystal growth process as the core of heterogeneous nucleation and thus making the lattice more distorted. The lower the lattice symmetry of CH₃NH₃PbCl₃, the larger the band gap is, that is, the lattice symmetry determines the degree of distortion for inorganic PbCl₆ octahedral frameworks, resulting in an increase of band gap for CH₃NH₃PbCl₃.

Keywords:

Authors and contacts

Shaanxi Key Laboratory of Optoelectronic Functional Materials and Devices, School of Materials and Chemical Engineering, Xi’an Technological University, Xi’an 710021, China

Corresponding author: Nan Rui-Hua, nanrh@xatu.edu.cn

Funds: Project supported by the Natural Science Basic Research Plan in Shaanxi Province of China (Grant No. 2022JM212).

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References

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Cited By

图 1 籽晶诱导逆温差结晶法生长CH₃NH₃PbCl₃单晶　(a)原理示意图; (b) CH₃NH₃PbCl₃在DMF和DMSO混合溶剂中的溶解度曲线

Figure 1. CH₃NH₃PbCl₃ single crystal grown by seed-induced inverse temperature crystallization method: (a) Schematic diagram of principle; (b) temperature-dependent solubility curve of CH₃NH₃PbCl₃ in DMF+DMSO mixed solution.

DownLoad: Full-Size Img PowerPoint

图 2 CH₃NH₃PbCl₃单晶生长　(a)单晶生长温度工艺曲线; (b)单晶宏观形貌图(尺寸为11 mm × 11 mm × 2 mm)

Figure 2. CH₃NH₃PbCl₃ single crystal growth: (a) Temperature control curve of single crystal growth; (b) macroscopic morphology of single crystal (Size: 11 mm × 11 mm × 2 mm).

DownLoad: Full-Size Img PowerPoint

图 3 籽晶诱导逆温差结晶法生长CH₃NH₃PbCl₃单晶　(a) 单晶XRD图谱; (b)粉末XRD与Material studio模拟的标准XRD图谱; (c) 粉末XRD Rietveld精修结果(R_p = 12.6%, R_wp = 18.5%)

Figure 3. CH₃NH₃PbCl₃ single crystal grown by seed-induced inverse temperature crystallization method: (a) XRD pattern of single crystal; (b) powder XRD and standard XRD pattern simulated by Material studio; (c) Rietveld result of powder XRD pattern (R_p = 12.6%, R_wp = 18.5%).

DownLoad: Full-Size Img PowerPoint

图 4 CH₃NH₃PbCl₃单晶的偏光显微形貌图　(a)单晶整体; (b)单晶局部放大图

Figure 4. Polarizing micromorphology of CH₃NH₃PbCl₃ single crystal: (a) Whole crystal; (b) partial magnification of single crystal.

DownLoad: Full-Size Img PowerPoint

图 5 (a) CH₃NH₃PbCl₃单晶的UV-Vis-NIR吸收光谱和PL光谱; (b) 通过拟合得到的帯隙值(蓝色散点是实验数据, 黑色实线是拟合结果E_g = 2.93 eV)

Figure 5. (a) UV-Vis-NIR absorption and PL spectra of CH₃NH₃PbCl₃ single crystal; (b) band gap obtained by fitting (Blue scatter dots are the experimental data, and the black solid line is the fitting result of E_g = 2.93 eV).

DownLoad: Full-Size Img PowerPoint

图 6 CH₃NH₃PbCl₃单晶的变温拉曼光谱　(a), (b) 80—300 K; (c), (d) 150—170 K; (e) 158 K; (f) 160 K; (g) 不同温度下CH₃NH₃PbCl₃晶体结构(立方/四方/正交)的拉曼谱

Figure 6. Temperature-dependent Raman spectra of CH₃NH₃PbCl₃ single crystal: (a), (b) 80–300 K; (c), (d) 150–170 K; (e) 158 K; (f) 160 K; (g) Raman spectra of CH₃NH₃PbCl₃ crystal structures (cubic/tetragonal/orthogonal) at different temperatures.

DownLoad: Full-Size Img PowerPoint

图 7 第一性原理计算CH₃NH₃PbCl₃的能带结构和态密度(a) 能带图谱; (b) 总态密度图; (c) 分波态密度图

Figure 7. Energy band structure and DOS for CH₃NH₃PbCl₃ calculated by first-principles simulation: (a) Energy band structure diagram; (b) total DOS diagram; (c) partial DOS diagram.

DownLoad: Full-Size Img PowerPoint

[1]	Turedi B, Lintangpradipto M N, Sandberg O J, Yazmaciyan A, Matt G J, Alsalloum A Y, Almasabi K, Sakhatskyi K, Yakunin S, Zheng X, Naphade R, Nematulloev S, Yeddu V, Baran D, Armin A, Saidaminov M I, Kovalenko M V, Mohammed O F, Bakr O M 2022 Adv. Mater. 34 2202390 Google Scholar
[2]	Xing G, Mathews N, Sun S, Lim S S, Lam Y M, Grätzel M, Mhaisalkar S, Sum T C 2013 Science 342 344 Google Scholar
[3]	Wang S, Yang F, Zhu J, Cao Q, Zhong Y, Wang A, Du W, Liu X 2020 Sci. China Mater. 63 1438 Google Scholar
[4]	Stranks S D, Eperon G E, Grancini G, Menelaou C, Alcocer M J P, Leijtens T, Herz L M, Petrozza A, Snaith H J 2013 Science 342 341 Google Scholar
[5]	Zhang Y, Liu Y, Liu S 2022 Adv. Funct. Mater. 32 2210335 Google Scholar
[6]	Chen H, Ye F, Tang W, He J, Yin M, Wang Y, Xie F, Bi E, Yang X, Grätzel M, Han L 2017 Nature 550 92 Google Scholar
[7]	Li M, Zhao C, Wang Z, Zhang C, Lee H K H, Pockett A, Barbé J, Tsoi W C, Yang Y, Carnie M J, Gao X, Yang W, Durrant J R, Liao L, Jain S M 2018 Adv. Energy Mater. 8 1801509 Google Scholar
[8]	Wang Y, Chen W, Wang L, Tu B, Chen T, Liu B, Yang K, Koh C W, Zhang X, Sun H, Chen G, Feng X, Woo H Y, Djurišic´ A B, He Z, Guo X 2019 Adv. Mater. 31 1902781 Google Scholar
[9]	Quan L N, García de Arquer F P, Sabatini R P, Sargent E H 2018 Adv. Mater. 30 1801996 Google Scholar
[10]	Cao Y, Wang N, Tian H, Guo J, Wei Y, Chen H, Miao Y, Zou W, Pan K, He Y, Cao H, Ke Y, Xu M, Wang Y, Yang M, Du K, Fu Z, Kong D, Dai D, Jin Y, Li G, Li H, Peng Q, Wang J, Huang W 2018 Nature 562 249 Google Scholar
[11]	Zhang Q, Su R, Liu X, Xing J, Sum T C, Xiong Q 2016 Adv. Funct. Mater. 26 6238 Google Scholar
[12]	Wang K, Wang S, Xiao S, Song Q 2018 Adv. Optical Mater. 6 1800278 Google Scholar
[13]	Li D, Cheng H, Wang Y, Zhao Z, Wang G, Wu H, He Q, Huang Y, Duan X 2017 Adv. Mater. 29 1601959 Google Scholar
[14]	Yu W, Li F, Yu L, Niazi M R, Zou Y, Corzo D, Basu A, Ma C, Dey S, Tietze M L, Buttner U, Wang X, Wang Z, Hedhili M N, Guo C, Wu T, Amassian A 2018 Nat. Commun. 9 5354 Google Scholar
[15]	Tian W, Zhou H, Li L 2017 Small 13 1702107 Google Scholar
[16]	Pan W, Wei H, Yang B 2020 Front. Chem. 8 268 Google Scholar
[17]	Andričević P, Frajtag P, Lamirand V P, Pautz A, Kollár M, Náfrádi B, Sienkiewicz A, Garma T, Forró L, Horváth E 2021 Adv. Sci. 8 2001882 Google Scholar
[18]	Ma L, Yan Z, Zhou X, Pi Y, Du Y, Huang J, Wang K, Wu K, Zhuang C, Han X 2021 Nat. Commun. 12 2023 Google Scholar
[19]	Shen H, Nan R, Jian Z, Li X 2019 J. Mater. Sci. 54 11596 Google Scholar
[20]	Wang W, Meng H, Qi H, Xu H, Du W, Yang Y, Yi Y, Jing S, Xu S, Hong F, Qin J, Huang J, Xu Z, Zhu Y, Xu R, Lai J, Xu F, Wang L, Zhu J 2020 Adv. Mater. 32 2001540 Google Scholar
[21]	Ryu S, Noh J H, Jeon N J, Kim Y C, Yang W S, Seoa J, Seok S I 2014 Energy Environ. Sci. 7 2614 Google Scholar
[22]	Cheng X, Jing L, Zhao Y, Du S, Ding J, Zhou T 2018 J. Mater. Chem. C 6 1579 Google Scholar
[23]	Zheng E, Yuh B, Tosado G A, Yu Q 2017 J. Mater. Chem. C 5 3796 Google Scholar
[24]	Liu Y, Yang Z, Cui D, Ren X, Sun J, Liu X, Zhang J, Wei Q, Fan H, Yu F, Zhang X, Zhao C, Liu S 2015 Adv. Mater. 27 5176 Google Scholar
[25]	Ding J, Cheng X, Jing L, Zhou T, Zhao Y, Du S 2018 ACS Appl. Mater. Interfaces 10 845 Google Scholar
[26]	Mosconi E, Amat A, Nazeeruddin M K, Grätzel M, Angelis F D 2013 J. Phys. Chem. C 117 13902 Google Scholar
[27]	Zhang F, Zhong H, Chen C, Wu X, Hu X, Huang H, Han J, Zou B, Dong Y 2015 ACS Nano 9 4533 Google Scholar
[28]	Bernasconi A, Page K, Dai Z, Tan L Z, Rappe A M, Malavasi L 2018 J. Phys. Chem. C 122 28265 Google Scholar
[29]	Songvilay M, Wang Z, Sakai V G, Guidi T, Bari M, Ye Z G, Xu G, Brown K L, Gehring P M, Stock C 2019 Phys. Rev. Mater. 3 125406 Google Scholar
[30]	Ivanovska T, Quarti C, Grancini G, Petrozza A, Angelis F D, Milani A, Ruani G 2016 Chem. Sus. Chem 9 2994 Google Scholar
[31]	Wang H, Nan R, Jian Z, Jin C, Wei Y, Bai Y, Li H 2021 Mater. Sci. Semicond. Process. 135 106107 Google Scholar
[32]	Singleton J, Rabe K M 2002 Phys. Today 55 61 Google Scholar

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Growth mechanism, phase transition and optical properties of large-size and high-quality perovskite CH₃NH₃PbCl₃ single crystal