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Communication

Chiral Lead Halide Perovskite Nanowires for Second-Order Nonlinear Optics

Chunqing Yuan, Xinyue Li, Sergey Semin, Yaqing Feng, Theo Rasing, and Jialiang Xu

Nano Lett., Just Accepted Manuscript • DOI: 10.1021/acs.nanolett.8b01616 • Publication Date (Web): 13 Aug 2018

Downloaded from http://pubs.acs.org on August 14, 2018

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polarization ratios and chiroptical NLO effects. Such a chiral perovskite skeleton could provide a

new platform for future engineering of optoelectronic functionalities of hybrid perovskite

materials.

KEYWORDS: chiral perovskite, nanowire, nonlinear optics, second harmonic generation.

Introduction

Hybrid organic/inorganic lead halide perovskites (LHPs), featuring intrinsic chemical variability

and structural diversity,

have recently emerged as extremely promising photonic materials

2-4

for

diverse optoelectronic device applications in light emitting diodes,

5,6

solar cells,

7,8

photoelectrolysis,

photodetectors,

10,11

and optically pumped lasers.

The nonlinear optical

(NLO) effects are fundamentals for realizing some very important optical devices such as optical

parametric generators and oscillators (OPGs and OPOs respectively), all optical switches, optical

limiters, etc.

13,14,15

Meanwhile, the NLO materials are also widely applied in advanced

techniques such as high resolution optical lithography

and microscopy.

Perovskite-type

materials such as niobates,

18,19

borates,

titanates,

21,22

germanium iodides,

etc. have been

widely explored as NLO materials for their versatile chemical structures and large NLO

coefficients. In particular, the hybrid organic/inorganic LHPs allow for enormous opportunities

to fine tune the structural scaffolds and electronic bandgaps of perovskite materials by varying

the organic and inorganic components. Along with the merits of low-cost and processability,

they are therefore very promising for applications in NLO materials. The third- and higher-order

NLO properties of LHP materials have been extensively investigated

and widely applied in

optical devices such as up-conversion lasers.

24-27

However, for electro-optical and frequency

doubling/mixing applications, second-order NLO effects are required.

For second-order NLO

responses such as second harmonic generation (SHG), a strict structural non-centrosymmetry is

Page 2 of 22

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Nano Letters

required.

Although weak, presumably surface related SHG signals have been detected from

micro-domains of tetragonal CH

PbI

based LHP films,

strong second-order NLO

responses have been hardly observed from the bulk of the ordinary LHP materials, consistent

with their centrosymmetric crystal space groups.

25,31

In addition, second-order optical

nonlinearities are often accompanied with some other technologically important effects such as

ferroelectricity, pyroelectricity and piezoelectricity, because these effects also require structural

non-centrosymmetry. A few hybrid LHP materials have indeed been demonstrated to be superior

ferroelectric semiconductors.

32,33

In this context, a rational design and construction of LHPs with

intrinsic non-centrosymmetric geometries and bulk second-order optical nonlinearities is of

particular importance, not only for advancing their applications in the next generation integrated

photonic circuits, but also for providing a prototype for developing new LHP functional

materials and devices. In particular, the elongated one-dimensional nanostructure of these LHP

materials makes them potential building blocks for nanowire photonics.

34,

Recently, two-dimensional (2D) hybrid LHP materials with relatively bulky organic motifs have

attracted broad interests for their improved stability under ambient conditions. The bulky organic

site has provided a versatile platform for the functionalization of these 2D perovskite materials

by introducing diverse ammonium groups for superior optoelectronic properties.

36-39

Billing

and Moon

have also demonstrated the feasibility of introducing chirality into LHP materials by

employing chiral amine as the organic component. Inspired by these pioneering works, we report

here the construction of a new chiral LHP material and the observation of strong bulk second-

order NLO responses from nanowires of this chiral perovskite material. Chiral β-

methylphenethylamine (MPEA) was used as the organic component to direct the non-

centrosymmetric assembly of the 2D inorganic layers and perovskite crystals into a chiral P1

Page 3 of 22

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Nano Letters

space group, by anti-solvent vapor-assisted crystallization (AVC)

using a ternary solvent

system. The structure of the dimethylsulfoxide (DMSO) solvent engineered 2D perovskite

intermediate phase was determined to be a new type of perovskite material in which DMSO

molecules axially coordinated with Pb

in the partially edge-shared octahedrons with a formula

of (MPEA)

1.5

PbBr

3.5

(DMSO)

0.5

. Nanowires from this chiral perovskite material were fabricated

and strong SHG signal was observed from the nanowires with high polarization ratios and NLO

circular dichroism. This chiral perovskite skeleton offers a new platform for future engineering

of the optoelectronic and other functionalities of hybrid perovskite materials.

Results and Discussion

The chiral perovskite materials were obtained by incorporating the bulky (R)-(+)- or (S)-(-)- β-

methylphenethylammonium cation (R- or S- MPEA) into the 2D perovskite scaffolds. We

followed the AVC technique for the growth of the chiral perovskite single crystals with

chloroform (CHCl

) as the anti-solvent and N,N-dimethylformamide (DMF) as the good

solvent

(see details in the Supporting Information). The slow diffusion of CHCl

vapor into the

mixed solution of PbBr

and MPEA

precursors in DMF results in the growth of white

needle-like single crystals (Supplementary Figure S1). However, these needle crystals are small

and of poor quality, which makes them unsuitable for single crystal X-ray diffraction (SCXRD)

analysis. We therefore sought a ternary solvent system in which a mixture of DMF and DMSO

was utilized as the good solvent instead of pure DMF.

The employment of DMSO indeed

improved the crystal size and the optical quality of the as-formed single crystals (Supplementary

Figure S1), which made SCXRD measurements possible. Scheme 1 shows the crystallographic

structures of the perovskite single crystals grown from the R- and S- MPEA

with PbBr

precursors in this ternary solvent system (referred to as the α-phase), respectively. We identified

that the structure of as-formed perovskite materials grown from the ternary solvent system is

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