Two-Dimensional Metal-Organic Layers as a Bright and Processable Phosphor for Fast White-Light Communication

Article abstract of DOI:10.1002/chem.201702037

A metal–organic layer (MOL) is a new type of 2D material that is derived from metal–organic frameworks (MOFs) by reducing one dimension to a single layer or a few layers. Tetraphenylethylene-based tetracarboxylate ligands (TCBPE), with aggregation-induced emission properties, were assembled into the first luminescent MOL by linking with Zr₆O₄(OH)₆(H₂O)₂(HCO₂)₆ clusters. The emissive MOL can replace the lanthanide phosphors in white light emitting diodes (WLEDs) with remarkable processability, color rendering, and brightness. Importantly, the MOL-WLED exhibited a physical switching speed three times that of commercial WLEDs, which is crucial for visible-light communication (VLC), an alternative wireless communication technology to Wi-Fi and Bluetooth, by using room lighting to carry transmitted signals. The short fluorescence lifetime (2.6 ns) together with high quantum yield (50 %) of the MOL affords fast switching of the assembled WLEDs for efficient information encoding and transmission.

Full text of DOI:10.1002/chem.201702037

A Journal of
Accepted Article
Title: Two-dimensional Metal-Organic Layers as A Bright and
Processable Phosphor for Fast White-Light Communication
Authors: Xuefu Hu, Zi Wang, Bangjiang Lin, Cankun Zhang, Lingyun
Cao, Tingting Wang, Jingzheng Zhang, Cheng Wang, and
Wenbin Lin
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To be cited as: Chem. Eur. J. 10.1002/chem.201702037
Link to VoR: http://dx.doi.org/10.1002/chem.201702037
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Two-dimensional Metal–Organic Layers as A Bright and
Processable Phosphor for Fast White-Light Communication
Xuefu Hu[a], Zi Wang[a], Bangjiang Lin*[b], Cankun Zhang[a], Lingyun Cao[a], Tingting Wang[a], Jingzheng
Zhang[a], Cheng Wang*[a], Wenbin Lin*[a,c]
Abstract: Metal-organic layer (MOL) is a new type of 2D material
that is derived from metal-organic frameworks (MOFs) by reducing
one dimension to a single layer or a few layers. We assembled
tetraphenylethylene-based tetracarboxylate ligands (TCBPE) with
aggregation-induced emission property into the first luminescent
MOL by linking with Zr6O4(OH)6(H2O)2(HCO2)6 clusters. The
emissive MOL can replace the lanthanide phosphors in white light
emitting diodes (WLEDs) with remarkable processability, color
rendering, and brightness. Importantly, the MOL-WLED exhibited a
physical switching speed three times that of commercial WLEDs,
which is crucial for visible-light communication (VLC), an alternative
wireless communication technology to Wifi and Bluetooth by using
room lighting to carry transmitted signals. The short fluorescence
lifetime (2.6 ns) together with high quantum yield (50%) of the MOL
affords fast switching of the assembled WLEDs for efficient
information encoding and transmission.
fast switching of WLEDs to encode signals.[5] As compared to
radio-frequency based technologies such as Wi-Fi and Bluetooth,
VLC can transmit information with higher speed, higher security,
lower radio interference, lower cost, more bandwidth and more
desirable bio-friendliness.[5b]
Although the theoretical upper limit of modulation frequency
for data transmission in the visible-light range is up to hundreds
of THz, commercial WLEDs have limited physical response
frequency[6] of only hundreds of kHz as a result of slow response
of the lanthanide phosphors such as Ce-doped yttrium aluminum
garnet (YAG-Ce).[7] The luminescence of YAG-Ce has an
emitting lifetime of 200 ns, leading to an intrinsic modulation
frequency of less than 0.8 MHz.[8] Even with such a slow
response rate, the modulation frequency in VLC based on
commercial WLEDs has been pushed to hundreds of MHz by
resorting to regions of small signals using advanced detection
and signal equalizing circuits. The transmission rate can be
further boosted to over Gbit/s by using spectrally efficient
Metal-organic layer (MOL) is a new type of 2D material that
is derived from metal-organic frameworks (MOFs) by reducing
one dimension to a single layer or a few layers.[1] Similar to
MOFs, MOLs serve as a versatile platform to organize functional
molecular building blocks.[2] Introducing fluorescent ligands into
MOLs can afford luminescent material that is more processable
than their MOF counterparts for LED lighting[3] and other
fluorescence-related applications.[4] The network structure of
MOL immobilizes fluorescent struts, which not only prevents
their self-aggregation but also restricts their internal motions,
both of which enhance quantum yields and suppress unwanted
photochemistry. The MOLs as ultrathin nano-sheets also
alleviate the scattering and non-uniform absorption of back light
by bulk solid phosphors in LED construction.
[9]
modulation techniques.
We envision that if we can improve
the intrinsic physical response frequencies of WLEDs, we will be
able to further increase the capability of the VLC technology.
Molecular phosphors exhibit fluorescence lifetimes down to
ns with high quantum yields, and are thus suitable replacements
for YAG-Ce in fast VLCs. MOLs provide an ideal platform to
organize the molecular phosphors into luminescent materials
with theoretical response frequency of hundreds of MHz, and
can thus remove the rate limit imposed by the phosphor in
current WLEDs.
In this work, we assembled a MOL-based WLED and
achieved an intrinsic physical modulation frequency of 1.7 MHz
at 3dB attenuation of the received oscillating signal, as
compared to 0.6 MHz for a commercial WLED. The frequency
response of the MOL-based WLED is the same as that of the
underlying LED circuits, demonstrating the ability to overcome
the limitation of phosphor response rate by using a novel
fluorescent MOL.
Luminescent MOLs assembled from fluorescent molecules
are particularly suitable for constructing white light emitting
diodes (WLEDs) for visible-light communication (VLC). VLC is a
wireless communication technology that uses everyday lighting
for information transmission and is motivated by the possible
[a]
X. Hu, Dr. C. Zhang, Z. Wang, L. Cao, T. Wang, J. Zhang, Prof. C.
Wang, Prof. W. Lin
Collaborative Innovation Center of Chemistry for Energy Materials,
State Key Laboratory of Physical Chemistry of Solid Surfaces,
Department of Chemistry, College of Chemistry and Chemical
Engineering, Xiamen University, Xiamen, Fujian, 361005, P.R.
China
E-mail: wangchengxmu@xmu.edu.cn
Prof. B. Lin
Quanzhou Institute of Equipment Manufacturing, Haixi Institutes,
Chinese Academy of Sciences, Quanzhou, Fujian, 362200, P.R.
China
[b]
[c]
E-mail: linbangjiang@fjirsm.ac.cn
Prof. W. Lin
Department of Chemistry, University of Chicago, 929 E 57th Street,
Chicago, IL 60637, USA
E-mail: wenbinlin@uchicago.edu
Figure 1. Schematic showing the construction of visible-light communication
(VLC) devices using a fluorescent MOL as the phosphor.
Supporting information for this article is given via a link at the end of
the document.((Please delete this text if not appropriate))
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We utilized a tetraphenyl ethylene-based ligand 4',4'',4''',4''''-
(ethene-1,1,2,2-tetrayl)tetrakis([1,1'-biphenyl]-4-carboxylic acid)
(H4TCBPE)[10] (Figure S1-S4) as the fluorescent phosphor with
the aggregation-induced emission (AIE) property.[11] Li[10] and
other groups[12] have used this ligand and related derivatives to
construct MOFs for LEDs and WLEDs with remarkable color
(Figure 3b). Fourier-transformed maps of these images also
gave an averaged value of 2.44 nm which matched these
distances (Figure 3b). The TEM images of larger area show
pleated films of 300 nm to 500 nm in size for the MOL (Figure 3c,
S5). This pleat feature is typical for ultrathin 2D materials.
rendering and brightness. We successfully obtained
fluorescent 2D MOL (Zr-TCBPE-MOL) based
a
on
[Zr6O4(OH)6(H2O)2(HCO2)6]4+ secondary building units (SBUs) by
reacting H4TCBPE with ZrCl4 in the presence of formic acid and
water in DMF (Figure 2). The MOL was obtained as a result of
SBU super-saturation, a strategy we previously adopted for the
synthesis of 2D MOLs based on tricarboxylate ligands.[1f]
Both the TCBPE ligands and SBUs are 4-connected in Zr-
TCBPE-MOL. Each carboxylate on the ligand bridges two Zr4+
ions on the same SBU. The four benzoate arms of the same
ligand lie on the same plane with 120o and 60o angles between
them. These directions match four of the twelve connections on
the [Zr6O4(OH)6(H2O)2(HCO2)6]4+ SBU, leading to 4,4-connected
2D MOL with a sql topology (Figure 2c). The rest of the Zr sites
on the SBUs are capped by formate groups that are added as a
modulator in the synthesis.
Figure 3. a) Experimental (red line at the top) and simulated (black line at the
bottom) PXRD patterns of Zr-TCBPE-MOL; b) HRTEM and corresponding FFT
images of Zr-TCBPE-MOL; c) TEM image of Zr-TCBPE-MOL; d) HAADF
image of Zr-TCBPE-MOL.
Third, the thickness of the Zr-TCBPE-MOL was measured by
atomic force microscopy (AFM) (Figure 4) to be 2.43 nm,
corresponding to the van der Waals thickness of a bilayer of the
proposed structure. Thicker films with averaged thickness of 5.0
nm were also observed, consistent to four layers of the
proposed structure. (Figure S6).
Figure 2. a) Structrues of the H4TCBPE ligand and Zr6 clusters; b) The
structure of Zr-TCBPE-MOL; c) The sql topology of Zr-TCBPE-MOL; d) Ball-
and-stick model of the Zr6 cluster.
This 2D structural model of Zr-TCBPE-MOL was confirmed
by a number of experimental evidences. First, the Bragg peaks
in the powder X-ray diffraction (PXRD) pattern of Zr-TCBPE-
MOL could all be indexed to (hk0) reflections, which is a unique
feature for 2D materials (Figure 3a top).[1f] The experimental
PXRD pattern also matched the simulated one using the 2D
atomic model of Zr-TCBPE-MOL (Figure 3a bottom).
Second, the arrangement of the SBUs in two dimensions as
revealed in scanning transmission electron microscope high-
angle annular dark-field (STEM-HAADF) images (Figure 3d)
nicely fit the structural model of the sql topology (Figure 2c). The
distances between adjacent SBUs in the model (2.46 nm) were
corroborated by both the distances between adjacent white dots
of 2.50 nm in STEM-HAADF images (Figure 3d) and the
distances between the lattice fringes of 2.38 nm in High
Resolution Transmission electron microscopy (HRTEM) images
Figure 4. a) AFM image; b) the height profile of Zr-TCBPE-MOL.
Fourth, the chemical composition of Zr-TCBPE-MOL was
determined by a combination of thermogravimetric analysis
(TGA) and NMR spectroscopy. TGA gave the metal/ligand ratio
(Figure S7) whereas 1H-NMR of the digested sample afforded
the ratio between the capping formates and the TCBPE ligand
(Figure
S8).
The
resultant
formula
of
[Zr6O4(OH)6(H2O)2(HCO2)6(TCBPE)] is consistent with that of the
structural model shown in Figure 2. Hydroxides and water
molecules in the formula were assigned based on the charge
balance requirement.
Fifth, we used preformed [Zr6O4(OH)4]12+ clusters capped by
methacrylates as the Zr source in the synthesis, and obtained
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the same Zr-TCBPE-MOL based on PXRD patterns (Figure S9).
The direct assembly of Zr6 SBU to MOL structure further
supports our assignment of the SBUs.
optical head to give a uniform white light field. The emission
power of this WLED exhibited a linear dependence on the
working current (Figure S12), a desirable feature for VLC. The
spectrum of the white emission from the MOL-WLED (Figure 5b)
corresponds to (0.37, 0.41) on the CIE coordinates, representing
a warm-white light that is comfortable to human eyes (Figure 5d,
S13).The MOL-WLED was continuously operated over 168
hours to test its stability. A 30% drop of the output power was
detected at the end of the test (Fig. S14), possibly due to
decomposition of the TCBPE ligand under intense light in the
presence of oxygen. We believe that this stability can be further
improved by sealing the optical cavity in air-tight assemblies.
A VLC system was constructed to test the frequency
response of the WLED in communication. An arbitrary waveform
generator (AWG) was used to generate a high frequency signal
to drive the WLED in a coupled mode of alternating current (AC)
and direct current (DC). The WLED received a voltage signal
with a DC background of 3.3 V that drove the device and an AC
overlay of 3 V that modulated the light flux at high frequency.
This intensity-modulated light was received by a PIN photodiode
and then converted back to electric signals which were analyzed
by an oscilloscope.
Photophysical property of Zr-TCBPE-MOL was measured
before assembling WLEDs. Zr-TCBPE-MOL gives yellow
fluorescence with a broad emission spectrum centered at 560
nm [full width at half maximum (FWHM) = 100 nm] when excited
at 450 nm, the peak wavelength of commercial blue LED based
on GaInN (Figure 5a). This fluorescence spectrum closely
represents that of YAG-Ce[13] and corresponds to a coordinate of
(0.42, 0.54) on the Commission Internationale de L'Eclairage
(CIE) map (Figure 5b). This result is very similar to MOFs built
from the same ligand reported by Li and coworkers.[10] The blue
emission of the GaInN LED can be drawn at (0.15, 0.05) on the
CIE map (Figure 5b). Any combination of these blue and yellow
emissions should fall on the line connecting the two end points
on the CIE map. The white light point (0.33, 0.33) locates right
on the line, indicating the possibility of constructing WLEDs
using Zr-TCBPE-MOL and GaInN LED.
The amplitudes of the received AC signals were recorded at
different input frequencies with the same input driving voltage.
When the input frequency was too high, the system could not
fully follow the oscillation, and the transmitted signal dropped in
amplitude. The frequency at which the transmitted signal drops
to -3dB with respect to the amplitude at zero frequency is
defined as the maximum usable frequency in communication. As
shown in Figure 6a, the normalized transmission amplitude of
the MOL-WLED showed
a linear dependence over the
frequency range of 0-4 MHz, with an intrinsic modulation
frequency of 1.7 MHz at -3dB. In comparison, a similar system
constructed from
a commercial WLED gave an intrinsic
modulation frequency of only 0.6 MHz.
This VLC system was further examined in data transmission
tests. A random binary signal was encoded with on-off keying
(OOK) by the AWG and transmitted at different bit rates. The bit
error rate (BER), defined as the number of error bits divided by
the total number of transmitted bits, is a measure of the reliability
of the system at the specific bit rate. A BER of over 1×10-3 is
regarded unsuitable for wireless communication. The MOL-
WLED could transmit the testing signal at a speed of 3.5 Mbps
with a nearly negligible BER (Figure 6b), while the commercial
one (c-WLED) only worked below 1.2 Mbps. This bit rate
difference of ~three times between the MOL-WLED and the c-
WLED is similar to their difference in intrinsic modulation
frequency.
Figure 5. a) Emission spectra of Zr-TCBPE-MOL (orange line) and 450 nm
LED (blue line) and the MOL-WLED (black line); b) The coordinates of the
MOL-WLED on CIE map (red square: Zr-TCBPE-MOL, yellow triangle: 450 nm
LED, blue star: MOL-WLED); c) The fluorescence decay curves of Zr-TCBPE-
MOL (line and triangles) and commercial WLED (line and squares); d) The
photo of the MOL-WLED.
The fluorescence lifetime of Zr-TCBPE-MOL was determined
to be 2.6 ns as shown in Figure 5c, significantly shorter than that
of YAG-Ce (Figure 5c, S10). We thus hypothesize that Zr-
TCBPE-MOL can give a WLED that is turned on/off much faster
than commercial ones. This fast response rate can support an
on/off frequency of over 60 MHz in VLC. The quantum yield of
Zr-TCBPE-MOL is as high as 50%, suitable for the construction
of efficient LEDs.
To assemble the WLED, a suspension of Zr-TCBPE-MOL
was filled into an optical cavity just above the GaInN LED chip
and dried in air. (Fig. S11) The yellow emission from Zr-TCBPE-
MOL and the transmitted blue light were redistributed by the
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Figure 6. a) The modulation frequency of the VLC system (line and squares
for the c-BLED, line and dots for the c-WLED, line and triangles for the MOL-
WLED); b) The BER of the data transmission (line and dots for the c-WLED
and line and squares for the MOL-WLED).
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In summary, we have synthesized a new 2D MOL based on
an AIE ligand and Zr6 cluster. This MOL with thickness down to
a bilayer exhibits intense yellow fluorescence and remarkable
processibility. A WLED constructed using this new phosphor is
at least three times faster than the commercial ones in visible-
light communication, thanks to the much shorter fluorescence
lifetime of the MOL as compared to lanthanide emitters in
commercial WLEDs. The MOL-WLED achieved three times data
transmission speed over commercial WLEDs with simple OOK
modulation in VLC. This work illustrates the opportunities in
designing and assembling new functional molecules into hybrid
nanomaterials for advanced information technology.
Experimental Section
Synthesis of 2D Zr-TCBPE-MOL: H4TCBPE (2 mg 0.0025 mmol) was
dissolved in 0.2 mL of DMF, and ZrCl4 (3.5 mg 0.015 mmol) was
dissolved in a mixed solvent of 0.3 mL of DMF, 0.1 mL of formic acid and
0.2 mL of H2O. The two solutions were combined and kept at 120 °C for
48 h to obtain a white suspension. The Zr-TCBPE-MOL solid was
obtained through centrifugal separation.
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[6] For a given device, the response to oscillating input signals drop in
intensity as a function of the frequency of this signal. This physical
response frequency is defined as the frequency at which half the
intensity of zero frequency is preserved.
[7] In commercial WLEDs, blue light from GaInN-based emitting
diodes excites YAG-Ce to give yellow light from the 4f-5d transition
of Ce3+. The combination of blue and yellow in a proper ratio looks
white to human eyes.
[8] Although short-pass filters have been installed before the receiver to
remove the slow yellow light and recover fast data transmission
rate,[a] the reduction in light intensity presents a challenge to the
signal receiver part, especially considering that commercial Si-based
PIN and avalanche photodiode (APD) detectors are usually more
sensitive to yellow light. [a]: see ref [S. Wang, F. Chen, L. Liang, S.
He, Y. Wang, X. Chen, W. Lu, IEEE. Wirel. Commun. 2015, 22,
61.]
Acknowledgements
We acknowledge funding support from the National Natural
Science Foundation and Ministry of Science and Technology of
the P. R. China (NNSFC21671162, 2016YFA0200700,
NNSFC21471126, NNSFC61601439), the National Thousand
Talents Program of the P. R. China, the 985 Program of
Chemistry and Chemical Engineering Disciplines of Xiamen
University, and the U.S. National Science Foundation (DMR-
1308229).
[9] X. Huang, Z. Wang, J. Shi, Y. Wang, N. Chi, Opt. Express 2015, 23,
22034.
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Banerjee, D. Zhang, J. Li, Chem. Commun. 2015, 51, 3045-3048.
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Keywords: metal-organic layers (MOLs); white light emitting
diode (WLED); visible-light communication (VLC); metal-organic
frameworks (MOFs); aggregation-induced emission (AIE)
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Entry for the Table of Contents (Please choose one layout)
Layout 1:
COMMUNICATION
A new two-dimensional metal-organic
layer, constructed from zirconium
clusters and fluorescent ligands, is
used as a fast phosphor to increase
the response rate of white light LED
for visible-light communication. The
use of molecular phosphors increases
the data transfer rate by three times,
illustrating the opportunity in using
Xuefu Hu, Cankun Zhang, Bangjiang
Lin*, Zi Wang, Lingyun Cao, Tingting
Wang, Jingzheng Zhang, Cheng Wang*,
Wenbin Lin*
Page No.1– Page No.5
Two-dimensional Metal–Organic
Layers as A Bright and Processable
Phosphor for Fast White-Light
Communication
nano-assemblies
for
advanced
information technology.
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