J. Semicond. > 2022, Volume 43 > Issue 12 > 120201

RESEARCH HIGHLIGHTS

Single crystals of perovskites

Haiyue Dong1, H, Lixiu Zhang2, , Wenhua Zhang3, Jilin Wang1, , Xiaoliang Zhang4, and Liming Ding2,

+ Author Affiliations

 Corresponding author: Jilin Wang, jilinwang@glut.edu.cn; Xiaoliang Zhang, xiaoliang.zhang@buaa.edu.cn; Liming Ding, ding@nanoctr.cn

DOI: 10.1088/1674-4926/43/12/120201

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During last decade, metal halide perovskites (MHPs) have become research hotspot due to their superior optoelectronic properties[1-15]. MHP single crystal was first reported in 1978[16]. Up to now, MHP single crystals with various compositions have been synthesized and characterized. Compared with perovskite polycrystalline films, perovskite single crystals show lower defect density, higher carrier mobility, longer carrier diffusion length. Here, we summarize the growth methods of perovskite single crystals, and discuss their optoelectronic applications, including perovskite solar cells (PSCs), photodetectors (PDs) and light-emitting diodes (LEDs).

A variety of crystallization methods have been developed for preparing high-quality perovskite single crystals[17-21], including inverse temperature crystallization (ITC) method[19], solution temperature-lowering (STL) method[20, 21] and antisolvent vapor-assisted crystallization (AVC) method[22, 23]. ITC method was first proposed by Bakr et al. to grow MAPbX3 (X = Br, I) single crystals in 2015[19] (Fig. 1(a)). This method is applied to precursors with inverse solubility in certain organic solvents (i.e., the solubility decreases as temperature increases). Perovskite molecules in complex can be released by raising the temperature, initiating supersaturation and crystallization. For MAPbI3, MAPbBr3 and MAPbCl3, the applicable solvents for ITC method are GBL, DMF and DMSO, respectively. This method is commonly used because it is very simple and quick. For STL method, the supersaturation is achieved by lowering the temperature of a hot saturated solution[20] (Fig. 1(b)). The solvents have increasing solubility with temperature, e.g., HI-based solution. High-quality single crystals can be obtained by precisely controlling the rate of lowering temperature[21]. However, STL method is quite time-consuming. Bakr et al. reported AVC method to grow sizable MAPbX3 (X = I or Br) single crystals with volumes exceeding 100 mm3[22]. The perovskite solution was sealed in an antisolvent-containing container, and the diffusion of antisolvents induces slow and uniform crystallization without changing the temperature (Fig. 1(c)). Ding et al. utilized this method to grow lead-free perovskite materials (NH4)3Sb2IxBr9–x in ethanol solvent[23].

Fig. 1.  (Color online) Common solution growth methods for perovskite single crystals. (a) Inverse temperature crystallization method. Reproduced with permission[19], Copyright 2015, Springer Nature. (b) Solution temperature-lowering method. Reproduced with permission[20], Copyright 2015, Science (AAAS). (c) Antisolvent vapor-assisted crystallization. Reproduced with permission[22], Copyright 2015, Science (AAAS).

For photovoltaic application, the absence of grain boundary in single crystals lowers the defect density and increases carrier diffusion length, theoretically enabling better device performance. While in practice, it is challenging to obtain single-crystal devices with controllable thickness, negligible surface defects and well-deposited functional layers, which explains their underperformance compared with polycrystalline counterparts. Efforts have been made to thickness control, defect engineering and interface management, pushing the power conversion efficiency (PCE) to over 20%. Bakr et al. used space-limited ITC method to grow size-controllable MAPbI3 single crystal[24]. A PTAA-coated substrate was used to cover another PTAA-coated substrate spread with perovskite precursor on the surface, and the complex was then heated slowly. The growth of crystal film was confined by hydrophobic substrates, and micrometers-thick single-crystal film was obtained. With careful separation of two substrates with a blade, good contact between crystal film and transport layer could be ensured, yielding a PCE of 21.09% with a high fill factor of 84.3%. To reduce surface defects caused by MAI escape at high temperature, Bakr et al. lowered the crystallization temperature by using mixed solvent, propylene carbonate (PC) and GBL[25] (Fig. 2(a)). The addition of PC can let crystallization to occur at <90 °C. The film exhibited a smooth surface with a uniform thickness of ~20 μm (Fig. 2(b)). The PCE was increased to 21.9%. To further broaden near-infrared (NIR) response, mixed-cation FA0.6MA0.4PbI3 single-crystal films were made[26]. The external quantum efficiency (EQE) spectra showed edge redshifted, increasing short-circuit current density to over 26 mA/cm2 while maintaining the open-circuit voltage. A PCE of 22.8% was achieved.

Fig. 2.  (Color online) (a) MAI escape from MAPbI3 films in high-temperature and low-temperature crystallization. (b) Cross-sectional SEM images and device structure for MAPbI3 single-crystal PSC. Reproduced with permission[25], Copyright 2020, American Chemical Society. (c) The planar-type photodetector fabricated on (100) facet of a MAPbI3 single crystal. Reproduced with permission[27], Copyright 2015, Springer Nature. (d) The X-ray image for a key by Cs3Bi2I9 single-crystal detector (1 × 1 mm2). Reproduced with permission[32], Copyright 2020, Springer Nature. (e) Emission intensity vs time plot for an LED operated at 1 mA current. Inset: SEM image for MAPbBr3 micro-platelet and the image of LED at t = 12 h. Reproduced with permission[33], Copyright 2017, American Chemical Society. (f) Normalized PL spectra for (BA)2Csn−1PbnBr3n+1 single crystals. Reproduced with permission[35], Copyright 2020, Science (AAAS).

Perovskite single crystals have been used in PDs. In 2015, Sun et al. first utilized perovskite single crystal to make PDs (Fig. 2(c)), revealing better performance and durability than its polycrystalline counterpart[27]. Under 1 mW/cm2 light illumination, MAPbI3 single-crystal PD showed 100 times higher responsivity and EQE. To further increase the detectivity and lower the noise, Huang et al. made detectors with thin perovskite single crystals, obtaining low dark current, low noise and high detectivity[28]. MAPbBr3 PDs offered a record linear dynamic range of 256 dB, which can be attributed to reduced carrier recombination. In 2016, Huang et al. first explored the application of MAPbBr3 single crystal in X-ray detector, achieving a high mobility-lifetime product of 1.2 × 10–2 cm2/V[29]. Lead-free perovskite single crystals were also used in X-ray detectors. Tang et al. used double perovskite Cs2AgBiBr6 single crystal to make X-ray detectors with a minimum detectable dose rate of 59.7 nGyair/s[30]. Yang et al. reported anisotropic X-ray detectors based on (NH4)3Bi2I9 single crystals with a detection limit as low as 55 nGyair/s[31]. Liu et al. used refinement solution to get rid of extraneous nuclei and grew large Cs3Bi2I9 single crystals[32]. The X-ray detectors showed high sensitivity, low dark current and high thermal stability at 100 °C, being suitable for X-ray imaging (Fig. 2(d)).

Moreover, perovskite single crystal can be a good electroluminescent material. Yu et al. first reported LEDs based on MAPbBr3 single-crystal micro-platelets with a simple structure ITO/PVK/Au[33]. The device emitted green light with a luminance of ~5000 cd/m2, lasting for at least 54 h without degradation (Fig. 2(e)). Then, the electroluminescence blinking behavior of MAPbBr3 single crystal was observed. The device with a structure ITO/MAPbBr3/ITO exhibited a low operation voltage of 2 V and a pure green emission with full width at half maximum of ~20 nm[34]. Nevertheless, the luminescence went through blinking at the crystal edges. The radiative recombination mainly occurred at crystal edges due to spatial confinement effect, but large number of traps and defects also exist at the edges, providing non-radiative paths. The excitons either emitted light or were quenched by the traps at the edges, leading to blinking. Yang et al. prepared a series of 2D Ruddlesden-Popper perovskite single crystals with the formula of (BA)2Csn−1PbnBr3n+1[35]. Blue LEDs with high color purity were made via a micromechanical exfoliation method. The emission can be tuned across blue light range by varying n (Fig. 2 (f)).

Single crystals of perovskites present application potential in solar cells, photodetectors and LEDs by virtue of superior optoelectronic properties. Various growth methods have been developed to obtain large single crystals with high quality. More efforts will focus on size control, interface modification and long-term stability.

Acknowledgements: J. Wang thanks the National Natural Science Foundation of China (51972071), Guangxi Distinguished Experts Special Fund (2019B06) and Guangxi Research Foundation for Science and Technology (AD19245175). L. Ding thanks the open research fund of Songshan Lake Materials Laboratory (2021SLABFK02) and the National Natural Science Foundation of China (21961160720).


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Dang Y Y, Liu Y, Sun Y X, et al. Bulk crystal growth of hybrid perovskite material CH3NH3PbI3. CrystEngComm, 2015, 17, 665 doi: 10.1039/C4CE02106A
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Chen Z L, Turedi B, Alsalloum A Y, et al. Single-crystal MAPbI3 perovskite solar cells exceeding 21% power conversion efficiency. ACS Energy Lett, 2019, 4, 1258 doi: 10.1021/acsenergylett.9b00847
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Alsalloum A Y, Turedi B, Almasabi K, et al. 22.8%-Efficient single-crystal mixed-cation inverted perovskite solar cells with a near-optimal bandgap. Energy Environ Sci, 2021, 14, 2263 doi: 10.1039/D0EE03839C
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Zhuang R Z, Wang X J, Ma W B, et al. Highly sensitive X-ray detector made of layered perovskite-like (NH4)3Bi2I9 single crystal with anisotropic response. Nat Photonics, 2019, 13, 602 doi: 10.1038/s41566-019-0466-7
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Fig. 1.  (Color online) Common solution growth methods for perovskite single crystals. (a) Inverse temperature crystallization method. Reproduced with permission[19], Copyright 2015, Springer Nature. (b) Solution temperature-lowering method. Reproduced with permission[20], Copyright 2015, Science (AAAS). (c) Antisolvent vapor-assisted crystallization. Reproduced with permission[22], Copyright 2015, Science (AAAS).

Fig. 2.  (Color online) (a) MAI escape from MAPbI3 films in high-temperature and low-temperature crystallization. (b) Cross-sectional SEM images and device structure for MAPbI3 single-crystal PSC. Reproduced with permission[25], Copyright 2020, American Chemical Society. (c) The planar-type photodetector fabricated on (100) facet of a MAPbI3 single crystal. Reproduced with permission[27], Copyright 2015, Springer Nature. (d) The X-ray image for a key by Cs3Bi2I9 single-crystal detector (1 × 1 mm2). Reproduced with permission[32], Copyright 2020, Springer Nature. (e) Emission intensity vs time plot for an LED operated at 1 mA current. Inset: SEM image for MAPbBr3 micro-platelet and the image of LED at t = 12 h. Reproduced with permission[33], Copyright 2017, American Chemical Society. (f) Normalized PL spectra for (BA)2Csn−1PbnBr3n+1 single crystals. Reproduced with permission[35], Copyright 2020, Science (AAAS).

[1]
Li L, Chen H Y, Fang Z M, et al. An electrically modulated single-color/dual-color imaging photodetector. Adv Mater, 2020, 32, 1907257 doi: 10.1002/adma.201907257
[2]
Zhao D W, Ding L M. All-perovskite tandem structures shed light on thin-film photovoltaics. Sci Bull, 2020, 65, 1144 doi: 10.1016/j.scib.2020.04.013
[3]
Zuo C T, Ding L M. Drop-casting to make efficient perovskite solar cells under high humidity. Angew Chem Int Ed, 2021, 60, 11242 doi: 10.1002/anie.202101868
[4]
Cheng Y H, Ding L M. Pushing commercialization of perovskite solar cells by improving their intrinsic stability. Energy Environ Sci, 2021, 14, 3233 doi: 10.1039/D1EE00493J
[5]
Xiang H Y, Zuo C T, Zeng H B, et al. White light-emitting diodes from perovskites. J Semicond, 2021, 42, 030202 doi: 10.1088/1674-4926/42/3/030202
[6]
Wang S R, Wang A L, Hao F, et al. Renaissance of tin halide perovskite solar cells. J Semicond, 2021, 42, 030201 doi: 10.1088/1674-4926/42/3/030201
[7]
Liu L, Xiao Z, Zuo C T, et al. Inorganic perovskite/organic tandem solar cells with efficiency over 20%. J Semicond, 2021, 42, 020501 doi: 10.1088/1674-4926/42/2/020501
[8]
Zhang M Q, Zuo C T, Tian J J, et al. Blue perovskite LEDs. J Semicond, 2021, 42, 070201 doi: 10.1088/1674-4926/42/7/070201
[9]
Ma Z W, Xiao G J, Ding L M. Pressure-induced emission from low-dimensional perovskites. J Semicond, 2021, 42, 100203 doi: 10.1088/1674-4926/42/10/100203
[10]
Zhou H, Wang H, Ding L M. Perovskite nanowire networks for photodetectors. J Semicond, 2021, 42, 110202 doi: 10.1088/1674-4926/42/11/110202
[11]
Li M B, Zhou J J, Tan H, et al. Multifunctional succinate additive for flexible perovskite solar cells with more than 23% power-conversion efficiency. The Innovation, 2022, 3, 100310 doi: 10.1016/j.xinn.2022.100310
[12]
Mei L Y, Mu H R, Zhu L, et al. Frontier applications of perovskites beyond photovoltaics. J Semicond, 2022, 43, 040203 doi: 10.1088/1674-4926/43/4/040203
[13]
Pan X Y, Ding L M. Application of metal halide perovskite photodetectors. J Semicond, 2022, 43, 020203 doi: 10.1088/1674-4926/43/2/020203
[14]
Zhang L X, Pan X Y, Liu L, et al. Star perovskite materials. J Semicond, 2022, 43, 030203 doi: 10.1088/1674-4926/43/3/030203
[15]
Wang S Y, Tan L G, Zhou J J, et al. Over 24% efficient MA-free Cs xFA1– xPbX3 perovskite solar cells. Joule, 2022, 6, 1344 doi: 10.1016/j.joule.2022.05.002
[16]
Weber D. CH3NH3SnBr xI3– x (x = 0–3), a Sn(II)-system with cubic perovskite structure. Z Naturforsch B, 1978, 33, 862 doi: 10.1515/znb-1978-0809
[17]
Ke L L, Ding L M. Perovskite crystallization. J Semicond, 2021, 42, 080203 doi: 10.1088/1674-4926/42/8/080203
[18]
Li Y L, Ding L M. Single-crystal perovskite devices. Sci Bull, 2021, 66, 214 doi: 10.1016/j.scib.2020.09.026
[19]
Saidaminov M I, Abdelhady A L, Murali B, et al. High-quality bulk hybrid perovskite single crystals within minutes by inverse temperature crystallization. Nat Commun, 2015, 6, 7586 doi: 10.1038/ncomms8586
[20]
Dong Q F, Fang Y J, Shao Y C, et al. Electron-hole diffusion lengths > 175 µm in solution-grown CH3NH3PbI3 single crystals. Science, 2015, 347, 967 doi: 10.1126/science.aaa5760
[21]
Dang Y Y, Liu Y, Sun Y X, et al. Bulk crystal growth of hybrid perovskite material CH3NH3PbI3. CrystEngComm, 2015, 17, 665 doi: 10.1039/C4CE02106A
[22]
Shi D, Adinolfi V, Comin R, et al. Low trap-state density and long carrier diffusion in organolead trihalide perovskite single crystals. Science, 2015, 347, 519 doi: 10.1126/science.aaa2725
[23]
Zuo C T, Ding L M. Lead-free perovskite materials (NH4)3Sb2- I xBr9– x. Angew Chem Int Ed, 2017, 56, 6528 doi: 10.1002/anie.201702265
[24]
Chen Z L, Turedi B, Alsalloum A Y, et al. Single-crystal MAPbI3 perovskite solar cells exceeding 21% power conversion efficiency. ACS Energy Lett, 2019, 4, 1258 doi: 10.1021/acsenergylett.9b00847
[25]
Alsalloum A Y, Turedi B, Zheng X P, et al. Low-temperature crystallization enables 21.9% efficient single-crystal MAPbI3 inverted perovskite solar cells. ACS Energy Lett, 2020, 5, 657 doi: 10.1021/acsenergylett.9b02787
[26]
Alsalloum A Y, Turedi B, Almasabi K, et al. 22.8%-Efficient single-crystal mixed-cation inverted perovskite solar cells with a near-optimal bandgap. Energy Environ Sci, 2021, 14, 2263 doi: 10.1039/D0EE03839C
[27]
Lian Z P, Yan Q F, Lv Q R, et al. High-performance planar-type photodetector on (100) facet of MAPbI3 single crystal. Sci Rep, 2015, 5, 16563 doi: 10.1038/srep16563
[28]
Bao C X, Chen Z L, Fang Y J, et al. Low-noise and large-linear-dynamic-range photodetectors based on hybrid-perovskite thin-single-crystals. Adv Mater, 2017, 29, 1703209 doi: 10.1002/adma.201703209
[29]
Wei H T, Fang Y J, Mulligan P, et al. Sensitive X-ray detectors made of methylammonium lead tribromide perovskite single crystals. Nat Photonics, 2016, 10, 333 doi: 10.1038/nphoton.2016.41
[30]
Pan W C, Wu H D, Luo J J, et al. Cs2AgBiBr6 single-crystal X-ray detectors with a low detection limit. Nat Photonics, 2017, 11, 726 doi: 10.1038/s41566-017-0012-4
[31]
Zhuang R Z, Wang X J, Ma W B, et al. Highly sensitive X-ray detector made of layered perovskite-like (NH4)3Bi2I9 single crystal with anisotropic response. Nat Photonics, 2019, 13, 602 doi: 10.1038/s41566-019-0466-7
[32]
Zhang Y X, Liu Y C, Xu Z, et al. Nucleation-controlled growth of superior lead-free perovskite Cs3Bi2I9 single-crystals for high-performance X-ray detection. Nat Commun, 2020, 11, 2304 doi: 10.1038/s41467-020-16034-w
[33]
Chen M M, Shan X, Geske T, et al. Manipulating ion migration for highly stable light-emitting diodes with single-crystalline organometal halide perovskite microplatelets. ACS Nano, 2017, 11, 6312 doi: 10.1021/acsnano.7b02629
[34]
Nguyen V C, Katsuki H, Sasaki F, et al. Single-crystal perovskite CH3NH3PbBr3 prepared by cast capping method for light-emitting diodes. Jpn J Appl Phys, 2018, 57, 04FL10 doi: 10.7567/JJAP.57.04FL10
[35]
Chen H, Lin J, Kang J, et al. Structural and spectral dynamics of single-crystalline Ruddlesden-Popper phase halide perovskite blue light-emitting diodes. Sci Adv, 2020, 6, eaay4045 doi: 10.1126/sciadv.aay4045
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1. Lin, R., Dong, K., Zhao, J. et al. Wavelength-Tunable Microlasers Based on Perovskite Sheets Processed from the Solution Saturation-Controlled Method. Journal of Physical Chemistry C, 2024. doi:10.1021/acs.jpcc.4c01149
2. Sun, J., Zhao, D., Li, G. et al. Control spin-orbit coupling through changing the crystal structure of the metal halide perovskites. Applied Physics Reviews, 2023, 10(4): 041410. doi:10.1063/5.0155104
3. Zhang, K., Ding, B., Wang, C. et al. Highly Efficient and Stable FAPbI3 Perovskite Solar Cells and Modules Based on Exposure of the (011) Facet. Nano-Micro Letters, 2023, 15(1): 138. doi:10.1007/s40820-023-01103-8
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    Haiyue Dong, Lixiu Zhang, Wenhua Zhang, Jilin Wang, Xiaoliang Zhang, Liming Ding. Single crystals of perovskites[J]. Journal of Semiconductors, 2022, 43(12): 120201. doi: 10.1088/1674-4926/43/12/120201
    H Y Dong, L X Zhang, W H Zhang, J L Wang, X L Zhang, L M Ding. Single crystals of perovskites[J]. J. Semicond, 2022, 43(12): 120201. doi: 10.1088/1674-4926/43/12/120201
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    Received: 30 September 2022 Revised: Online: Accepted Manuscript: 30 September 2022Uncorrected proof: 30 September 2022Published: 02 December 2022

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      Haiyue Dong, Lixiu Zhang, Wenhua Zhang, Jilin Wang, Xiaoliang Zhang, Liming Ding. Single crystals of perovskites[J]. Journal of Semiconductors, 2022, 43(12): 120201. doi: 10.1088/1674-4926/43/12/120201 ****H Y Dong, L X Zhang, W H Zhang, J L Wang, X L Zhang, L M Ding. Single crystals of perovskites[J]. J. Semicond, 2022, 43(12): 120201. doi: 10.1088/1674-4926/43/12/120201
      Citation:
      Haiyue Dong, Lixiu Zhang, Wenhua Zhang, Jilin Wang, Xiaoliang Zhang, Liming Ding. Single crystals of perovskites[J]. Journal of Semiconductors, 2022, 43(12): 120201. doi: 10.1088/1674-4926/43/12/120201 ****
      H Y Dong, L X Zhang, W H Zhang, J L Wang, X L Zhang, L M Ding. Single crystals of perovskites[J]. J. Semicond, 2022, 43(12): 120201. doi: 10.1088/1674-4926/43/12/120201

      Single crystals of perovskites

      DOI: 10.1088/1674-4926/43/12/120201
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      • Haiyue Dong:got his BS from Dalian Minzu University in 2020. Now he is a MS student at Guilin University of technology under the supervision of Professor Fei Long and Professor Jilin Wang. His research focuses on perovskite solar cells
      • Lixiu Zhang:got her BS degree from Soochow University in 2019. Now she is a PhD student at University of Chinese Academy of Sciences under the supervision of Prof. Liming Ding. Her research focuses on perovskite solar cells
      • Jilin Wang:received his PhD in 2014 form Wuhan University of Technology under the supervision of Professor Weimin Wang. He joined Guilin University of Technology in 2015. Currently, he is an associate professor in Fei Long Group. His research focuses on optoelectronic materials and devices
      • Xiaoliang Zhang:is a professor at Beihang University. He received his PhD in Materials Physics and Chemistry from Beihang University in 2013. Then, he joined Uppsala University as a postdoc and subsequently was promoted as a Senior Researcher there. He joined Beihang University as a full professor in 2018. His research focuses on semiconducting quantum dots and their application in optoelectronic devices
      • Liming Ding:got his PhD from University of Science and Technology of China (was a joint student at Changchun Institute of Applied Chemistry, CAS). He started his research on OSCs and PLEDs in Olle Inganäs Lab in 1998. Later on, he worked at National Center for Polymer Research, Wright-Patterson Air Force Base and Argonne National Lab (USA). He joined Konarka as a Senior Scientist in 2008. In 2010, he joined National Center for Nanoscience and Technology as a full professor. His research focuses on innovative materials and devices. He is RSC Fellow, and the Associate Editor for Journal of Semiconductors
      • Corresponding author: jilinwang@glut.edu.cnxiaoliang.zhang@buaa.edu.cnding@nanoctr.cn
      • Received Date: 2022-09-30
        Available Online: 2022-09-30

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