Multicomponent Organic Metal Halide Hybrid with White Emissions

Article abstract of DOI:10.1002/anie.202006064

Zero-dimensional (0D) organic metal halide hybrids, in which organic and metal halide ions cocrystallize to form neutral species, are a promising platform for the development of multifunctional crystalline materials. Herein we report the design, synthesis, and characterization of a ternary 0D organic metal halide hybrid, (HMTA)₄PbMn_0.69Sn_0.31Br₈, in which the organic cation N-benzylhexamethylenetetrammonium (HMTA⁺, C₁₃H₁₉N₄⁺) cocrystallizes with PbBr₄^2?, MnBr₄^2?, and SnBr₄^2?. The wide band gap of the organic cation and distinct optical characteristics of the three metal bromide anions enabled the single-crystalline “host–guest” system to exhibit emissions from multiple “guest” metal halide species simultaneously. The combination of these emissions led to near-perfect white emission with a photoluminescence quantum efficiency of around 73 percent. Owing to distinct excitations of the three metal halide species, warm- to cool-white emissions could be generated by controlling the excitation wavelength.

Full text of DOI:10.1002/anie.202006064

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Accepted Article
Title: Multicomponent Organic Metal Halide Hybrid with White
Emissions
Authors: Liang-Jin Xu, Sujin Lee, Xinsong Lin, Logan Ledbetter,
Michael Worku, Haoran Lin, Chenkun Zhou, He Liu, Anna
Plaviak, and Biwu Ma
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To be cited as: Angew. Chem. Int. Ed. 10.1002/anie.202006064
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10.1002/anie.202006064
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Multicomponent Organic Metal Halide Hybrid with White
Emissions
Liang-Jin Xu,[a] Sujin Lee,[a] Xingsong Lin,[a] Logan Ledbetter,[b] Michael Worku,[c] Haoran Lin,[a]
Chenkun Zhou,[a] He Liu,[a] Anna Plaviak[a] and Biwu Ma* [a, c]
when wide bandgap organic cations are used. To date, various
combinations of organic and metal halides have been used to
synthesize 0D organic metal halide hybrids, which could exhibit
highly efficient emissions with tunable colors covering the whole
visible spectrum.[2a, 3] Other remarkable properties and applications,
such as thermometry,[1f] scintillation,[4] and ferroelectric,[5] have also
been observed in these materials.
Abstract: Multicomponent single crystals have received great
research attention for their capability of realizing multifunctionalities in
a single phase material. Zero-dimensional (0D) organic metal halide
hybrids are an emerging class of ionically bonded crystalline materials,
in which organic and metal halide ions co-crystallize to form neutral
species. The rich choices of organic and metal halide components
make 0D organic metal halide hybrids a highly promising platform for
the development of multifunctional crystalline materials, which
however are very much unexplored to date. Here we report the design,
synthesis, and characterization of a ternary 0D organic metal halide
hybrid, (HMTA)4PbMn0.69Sn0.31Br8, in which an organic cation HMTA+
(HMTA+: N-benzyl hexamethylenetetramium, C13H19N4+) co-
crystallizes with multiple metal halide anions, i.e. PbBr42-, MnBr42-, and
SnBr42-. The wide bandgap of the organic cation and distinct optical
characteristics of three metal bromide anions enable a single
crystalline “host-guest” system to exhibit emissions from multiple
“guest” metal halide species simultaneously. The combination of
these emissions could lead to a near-perfect white emission, with
Commission Internationale d’Eclairage (CIE) of (0.32, 0.33), Color
Rendering Index (CRI) of 95, and photoluminescence quantum
efficiency (PLQE) of around 73%. Due to distinct excitations of three
metal halide species, warm to cool white emissions with Correlated
Colour Temperature (CCT) varying from 3237 K to 12730 K could be
realized by controlling the excitation wavelength.
0D organic metal halide hybrids provide an excellent platform for
the development of multifunctional single crystalline materials, in
which multiple metal halide species can be integrated into a single
phase system. With proper synthetic control, several binary organic
metal halide hybrids have been developed recently. Our group
reported a series of highly luminescent binary metal halide hybrids
containing MClx2- (M = Pb, Zn or Sb, and x = 4 or 5) and Pb3Cl15-
clusters.[3a, 3b],[3f] Xia group synthesized binary hybrids with dual-
emissions by integrating MnBr42- and Pb3Br15- species.[1d] Despite
these recent developments, design and synthesis of ternary or higher
component organic metal halide hybrids remain challenging. 0D
organic metal halide hybrids containing three or more distinct metal
halide species have not been reported to date. One reason is that
single component or binary single crystals, instead of
multicomponent single crystals, would form preferentially, when
several components are involved in the crystallization process. Here
we refer 0D organic metal halide hybrids containing one kind of
metal halide species as single component single crystals, and two
kinds of metal halide species as binary single crystals. It is of great
interest to develop ternary or higher component organic metal halide
hybrids, which could provide a new avenue for preparation of
multifunctional materials, e.g. integrating ternary components with
blue, green, and red emissions to achieve white emissions,
assembling strong X-ray absorption and visible light emitting
species for X-ray scintillation, incorporating synergetic catalysts for
catalysis, and so on.
Organic-inorganic metal halide hybrids have recently emerged as
an important class of crystalline materials with unique optical and
electronic properties for various applications.[1] Besides 3D ABX3
metal halide perovskites, organic metal halide hybrids with low
dimensional 2D, corrugated-2D, 1D, and 0D structures have been
developed using appropriate organic and metal halides.[1c, 1g, 2] In 0D
organic metal halide hybrids, anionic metal halide molecular species
or clusters are separate from each other and co-crystallize with
cationic organic species to form periodical structures. The complete
site isolation enables 0D organic metal halide hybrids to exhibit the
intrinsic properties of metal halide molecular species or clusters,
Here we report the design, synthesis, and characterization of a
ternary organic metal halide hybrid, by co-crystallizing delicately
chosen organic and metal halides. Following the design strategy
applied for the preparation of organic cocrystals,[6] HMTA+ was
employed as the organic cation for its bulk steric hindrance; and
PbBr42-, MnBr42-and SnBr42- were chosen for their same charges and
similar sizes, but distinct emissions covering different regions of the
visible spectrum. It was found that these metal halide species can co-
crystallize with HMTA+ to form
a single phase system,
(HMTA)4PbMn0.69Sn0.31Br8, which possess integrated properties
from individual metal halide species. By combining blue emission
from PbBr42-, green emission from MnBr42-, and red emission from
SnBr42- in an appropriate ratio, efficient white emission could be
achieved with CIE of (0.32, 0.33), CRI of 95, and PLQE of around
73 %. As three metal halide species have distinct excitations, the
white emission can be tuned from warm to cool white with
Correlated Color Temperature (CCT) in the range of 3237 to 12730
K using different excitation wavelengths. UV-pumped white LEDs
have been fabricated by using this material as down conversion
phosphor, which exhibited maximum brightness of 6570 cd/m2 at
3.5 V and luminous efficiency of 6.2 lm/w.
[a]
Dr.L.-J. Xu, Dr. X Lin, Dr. Q. He, Prof. B. Ma
Department of Chemistry and Biochemistry, Florida State University
Tallahassee, FL 32306 (USA)
E-mail: bma@fsu.edu
L. Ledbetter
Department of Chemistry and Physics, Troy University, Troy, AL
36082 (USA)
M. Worku, Prof. B. Ma
Materials Science and Engineering Program, Florida State
University
Tallahassee, FL 32306 (USA)
[b]
[c]
Supporting information (Details of materials and synthesis, characterization
methods, structural and photophysical properties of materials, cif file for the
crystal structure of (HMTA)4PbMn0.69Sn0.31Br8 .
Binary 0D organic metal halide hybrids have been synthesized by
selecting appropriate organic cations to enable two inorganic metal
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10.1002/anie.202006064
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halide species to co-crystallize with each other. Simply introducing
a third metal halide species into binary metal halide hybrid
precursors may not lead to the formation of ternary single crystals,
as the formation of single component or binary single crystals could
dominate the crystallization process. To synthesize ternary organic
metal halide single crystals, many parameters, such as geometry and
solubility of metal halides, need to be considered carefully to
and 2.82 Å, respectively. (Details can be found in Table S2 and S3)
The PXRD patterns of ground crystals are identical to the simulated
results from the SCXRD data in Figure S2a, suggesting the purity
and uniformity of as-synthesized single crystals. To further confirm
the phase purity, PXRD patterns for single component hybrids,
HMTA2PbBr4, HMTA2MnBr4, HMTA2SnBr4, were collected,
which were compared to those of 0D (HMTA)4PbMn0.69Sn0.31Br8. It
suspense the formation of single component or binary single crystals, was found that the patterns of each single component hybrid and
while making ternary single crystals as preferred products. A
strategy similar to that used for the synthesis of organic cocrystals
was therefore proposed, as shown in Figure 1. A, B, and C represent
unit cells of single component organic metal halide crystals with the
same organic cation. Binary single crystals cannot be obtained for
the combination of A and B, as packed structures could not form as
easy as single component crystals. However, by introducing a third
building block C, ternary single crystals could form with a structure
more packed than those of single component crystals. After
screening organic cations and metal halides used to date for the
preparation of single component 0D organic metal halide hybrids,
we came up with the combination of HMTA2PbBr4 (A),
HMTA2MnBr4 (B), and HMTA2SnBr4 (C), considering that they
have similar structures containing the same organic ligand HMTA,
but different sizes. (See their structural information in Figure S1 and
Table S1) Moreover, they have the emissions covering different
regions of the visible spectrum, blue from HMTA2PbBr4, green from
HMTA2MnBr4, and red from HMTA2SnBr4. These distinct optical
properties would make it straightforward to characterize the
multifunctionality of a ternary system, which also has the potential
to achieve white emissions for various applications.
their mixtures are significantly different from those of the ternary
hybrid. (Figure S2b) Energy dispersive X-ray fluorescence
(EDXRF) was conducted to characterize the molar ratio of different
elements, which suggested the ratio of Pb /Mn /Sn /Br at
1/0.67/0.35/7.77, agreeing well with the SCXRD result. (See more
details in supporting information Figure S4 and Table S4) Thermal
gravimetric analysis (TGA) was used to characterize the thermal
stability of (HMTA)4PbMn0.69Sn0.31Br8, which exhibits good
thermal stability without weight loss until 211oC (Figure S3).
Figure 2. (a) The illustration of the crystal growing. (b) The images
of (HMTA)4PbMn0.69Sn0.31Br8 single crystals under ambient light
(up) and UV light (down). (c) View of the single crystal structure of
(HMTA)4PbMn0.69Sn0.31Br8. (d) the building blocks (PbBr42- purple
tetrahedrons, MnBr42- green tetrahedrons; SnBr42- brown
tetrahedrons; and organic cation HMTA+; Pb, red; Mn, green; Sn,
brown; N, blue; C, gray; Hydrogen atoms are hidden for clarity).
The photophysical properties of (HMTA)4PbMn0.69Sn0.31Br8 were
investigated
using
UV-Vis
absorption,
steady
state
photoluminescence spectroscopy, as well as time-resolved
photoluminescence spectroscopy. As illustrated in Figure 3a, the
solid-state UV–Vis spectrum (purple solid line) shows an a very
intense maximum absorption centered at 292 nm and a shoulder
peak at 350 nm. Upon irradiation at λex = 296 nm, white light
emission with distinguishable peaks at 460 nm, 550 nm and 645 nm,
can be observed with PLQE of around 73%, CRI of 95, and CIE of
(0.32, 0.33). The excitation spectra (Figure 3a) and emission decay
lifetimes were recorded for three emission peaks at 460 nm, 550 nm
and 645nm, which show completely different characteristics (Figure
3b). PL decay lifetimes for three emission peaks were measured at
85 ns, 426.7 µs, and 3.4 µs, respectively. Based on the photophysical
properties of single component 0D organic metal halide hybrids
(Figure S5), we can attribute the blue emission at 460 nm to PbBr42-
species,[3g] the green emission at 550nm to MnBr42- species,[1h] and
the red emission at 645 nm to SnBr42- species.[3c] The similar
photophysical properties of individual metal halide species in this
ternary single crystal ((HMTA)4PbMn0.69Sn0.31Br8) and their single
Figure 1. Scheme for the design of ternary single crystals based on
organic metal halides hybrids. A, B, and C represent unit cells of
single component organic metal halide crystals with the same
organic cation.
Following the design strategy, we grew single crystals by slowly
diffusing diethyl ether into a DMF precursor solution containing
HMTA, PbBr2, MnBr2 and SnBr2. (see Figure 2a and Scheme S1)
By optimizing the ratio of different components (see supporting
information on the experimental details), high-quality crystals were
successfully prepared, which are white under ambient light and
become strongly white emissive under UV light irradiation (Figure
2b). The crystal structure was solved by single crystal X-ray
diffraction (SCXRD) (Figure 2c-d), which gave the material a
chemical formula of (HMTA)4PbMn0.69Sn0.31Br8. The metal halide
species are isolated from each other by HMTA+ cations, among
which PbBr42- polyhedron adopts a seesaw-shaped geometry with an
average Pb-Br bond length of 2.87 Å, similar to that in previously
reported 0D HMTA2PbBr4.[3g] Both MnBr42- and SnBr42- have
distorted tetrahedral structures, which are positioned in the same
lattice points with a occupancy of 69 % for MnBr42- and 31 % for
SnBr42-. The average bond lengths for Mn-Br and Sn-Br are 2.50 Å
component crystals
(HMTA2PbBr4,
HMTA2MnBr4
and
HMTA2SnBr4) suggest little-to-no interactions among three metal
halide species. This is not surprising as three metal halide species
are completely separate from each other and there is no overlap
between their emissions and absorptions, resulting in no energy
transfer. Overall, this ternary orgainc metal halide hybrid, a
multifunctional single phase system, exhibits combined optical
properties from individual building blocks. The stability of
(HMTA)4PbMn0.69Sn0.31Br8 against moisture was characterized,
which exhibited little-to-no change of PLQE after exposure in
ambient atmosphere for two months. (Figure S6)
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Figure 3. Optical properties of (HMTA)4PbMn0.69Sn0.31Br8 at room
temperature. (a) Absorption, excitation and emission spectra of
(HMTA)4PbMn0.69Sn0.31Br8. (b) Emission decay curves of
(HMTA)4PbMn0.69Sn0.31Br8 monitored at 460 nm, 550 nm, and 645
nm, respectively.
The photoluminescence of this single phase ternary hybrid also
shows a strong dependence on the excitation, as the three emitting
species, blue emitting PbBr42-, green emitting MnBr42-, and red
emitting SnBr42-, have distinct excitations. Figure 4a shows the
excitation-dependent PLs with excitation shifting from 290 to 310
nm, with emission intensities at 460 nm and 550 nm increasing,
while decreasing at 645nm. This excitation-dependence enables
color tuning of the white emission from (HMTA)4PbMn0.69Sn0.31Br8,
with CCT varying from 3237 (warm white) to 12730 K (cool white)
upon excitation from 290 to 380 nm. Variant CIEs with high CRIs
of up to 97 and PLQEs as high as 82% (exictated at 350 nm) could
be achieved, as shown in Figure 4b, Figure S7 and Table S5.
Considering its high stability and strong white emissions,
(HMTA)4PbMn0.69Sn0.31Br8 could serve as down conversion
phosphor for UV pumped white LEDs. A simple device was
fabricated by embedding the grounded (HMTA)4PbMn0.69Sn0.31Br8
powders into polydimethylsiloxane (PDMS) polymer matrix. The
resulting composite thin films were then attached to a commercial
UV-LED (360 nm). As shown in Figure 4c, a UV pumped LED
displays bright white emission with a maximum brightness of 6570
cd/m2 at 3.5 V and luminous power efficiency of 6.2 lm/w. The
relative low power efficiency is due to the use of a UV LED with
low efficiency and mismatching of excitation wavelength (deep UV
nm excitation sources in the range 290-310 nm are not readily
available), a single device architecture, and only front emission
being counted in measurement. This UV pumped LED exhibited
excellent color stability at different driving currents, as shown in
Figure 4d.
Figure 4. (a) The excitation-dependent PL with the excitation
wavelength ranging from 290 to 380 nm. (b) CIE 1931 diagram
showing the chromaticity points of emissions when the material was
excited from 290 to 380 nm. (c) voltage versus brightness and
luminous efficiency of a UV-pumped LED (Inset shows the image
of a UV pumped LED) (d) Emission spectra of a UV-pumped LED
at different driving currents.
Acknowledgements
The authors acknowledge the supports from the National
Science Foundation (DMR-1709116), the Air Force Office of
Scientific Research (AFOSR-17RT0906), and the Florida
State University Office of Research.
In summary, a ternary orgainc metal halide hybrid with excitation
dependent white emissions has been prepared, by carefully choosing
organic and metal halides with appropriate geometries and
comprising emissions to cover blue, green, and red regions. This is
by far the first single phase 0D organic metal halide hybrid
containing three distinct metal halide species. With this
multicomponent single crystal as down conversion phosphor, a UV
pumped white LED was demonstrated. Our work enriches the family
of multicomponent single crystals based on organic metal halide
hybrids, and provides a versatile approach to design and prepare
multifunctional materials based on ionically bonded systems.
Keywords: multicomponent • organic metal halide hybrid •
single crystal • white emission • light emitting diode
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Entry for the Table of Contents (Please choose one layout)
COMMUNICATION
A ternary organic metal halide hybrid
(HMTA)4PbMn0.69Sn0.31Br8 has been
developed, which contains three
distinct metal halide species with
emissions covering blue, green, and
Liang-Jin Xu, Sujin Lee,
Xingsong Lin, Logan Ledbetter,
Michael Worku, Haoran Lin,
Chenkun Zhou, He Liu, Anna
Plaviak and Biwu Ma*
red
spectral
regions.
This
multicomponent single crystalline
material exhibits highly efficient
excitation dependent emissions,
with near-perfect white emissions
Page No. – Page No.
Title
obtained
under
appropriate
excitation wavelengths.
Multicomponent Organic Metal
Halide hybrid with White
Emissions
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