FlatChem 24 (2020) 100193

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FlatChem
journal homepage: www.elsevier.com/locate/flatc

Ultra-thin two-dimensional nanosheets for in-situ NIR light-triggered T

fluorescence enhancement
Cong Wang, Lan Zhang, Jia-Ying Wang, Shan Su, Xiao-Wei Jin, Pei-Jing An, Bai-Wang Sun,
Yang-Hui Luo
⁎

School of Chemistry and Chemical Engineering, Southeast University, Nanjing 211189, PR China

ABSTRACT

Ultra-thin two-dimensional (2D) nanosheets of Zn-based metal -organic framework (MOF) were prepared from the precursor [Zn(bpydc) (H2O)·H2O]n (bpydc = 2,2′-
bipyridine-5,5′-dicarboxylate), by using a liquid phase ultrasonic stripping technique. The atomic thickness and the abundant oxygen atoms making the nanosheets
are well dispersed in various solvents, exhibiting unique fluorescence responses to solvents of different polarities. Adding on, by loading on the ytterbium ion (Yb3+)-
sensitized hexagonal phase up-converting nanoparticles (UCNPs, sodium yttrium fluoride (NaYF4): 20 mol% Yb3+, 1 mol% erbium (Er3+ ions)) on the surfaces of
nanosheets, the in-situ near infrared (NIR) light (980 nm) triggered luminescence enhancement has been observed, suggesting the favorable application foreground
in biomedical science, super-capacitors, and electronic devices.

1. Introduction
Stimuli-responsive fluorescent materials have attracted considerable
attention for fundamental investigation and intelligent applications
during the last few decades [1–6]. Light [7], heat [8], pH [9] and
mechanical force [10] are the typical stimuli utilized to tune the
fluorescent behaviors of these materials. Stimuli-responsive fluorescent
materials have the merits of simple synthesis, fast response speed and
repeatable response, which play an important role in the fields of
fluorescent sensors, anti-counterfeiting paper, optical coding, optical
switches, data storage and biological imaging [11,12]. Thus, searching
for new types of stimuli-responsive fluorescent materials is of sig-
nificant importance.
One promising approach to obtain multiple stimuli-responsive
fluorescent materials is fluorescent variation via simple, noninvasive
and effective stimuli under ambient conditions. Light is an attractive
external stimuli for fluorescent materials, because it has the advantage
of relatively high local precision and remote controllability [13,14].
However most of the fluorescent materials were driven by high-energy
ultraviolet (UV) or visible light, which suffers the drawbacks of limited
penetration and invasiveness [15,16]. Compared with UV, the non-
toxic near infrared (NIR) light is more suitable for biological applica-
tions, especially for three-dimensional (3D) light scanning simulation
and information storage applications. In light-control system for the
biological field, NIR light plays an irreplaceable role [17–20]. But the
energy of NIR light is often too low to trigger most fluorescent varia-
tions. Lanthanide ions doped up-conversion nanoparticles (UCNPs) are
capable of efficiently converting low energy photons in the NIR region
to high-energy photons in the visible region. The transition between the
energy levels of the rare earth ions is a forbidden f-f transition with a
longer lifetime to achieve a two-photon or multiphoton effect [21–25].
Besides a deeper tissue penetration and lower biological tissue damage
featured by the NIR light, the advantages of UCNPs include high photo-
stability, adjustable luminescence spectra and relatively good bio-
compatibility. Thus, the combination of UCNPs with stimuli-responsive
materials may represent an attractive target for NIR light-triggered
application.
To demonstrate the above-mentioned promising aspects, the hy-
bridization between ultra-thin two-dimensional (2D) metal–organic
frameworks (MOFs) fluorescent nanomaterials with UCNPs, to achieve
the NIR light-triggered fluorescent variations have been proposed.
MOFs are classical porous materials that have been applicated in pho-
toluminescence, sorption, magnetism. Molecular recognition, and so on
[26–38]. Ultra-thin 2D MOFs nanosheets possess the merits of large
surface area and highly accessible active sites, which thus can act as a
versatile nano-platform for various chemical-physical process [29–31].
Here in this work, we have prepared ultra-thin 2D fluorescent na-
nosheets of Zn-based MOF from the 3D bulk precursor [Zn(bpydc)
(H2O)·H2O]n (bpydc = 2,2′-bipyridine-5,5′-dicarboxylate), by using a
facile-operating ultrasonic force-assisted liquid exfoliation technology.
Note that, this 2D fluorescent nanosheets can be well dispersed in
various solvents, and have shown interesting solvent polarity-depen-
dent fluorescent properties. More interestingly, by loading ytterbium
(Yb3+) ion sensitized UCNPs (NaYF4: 20 mol% Yb3+, 1 mol% Er3+

⁎
Corresponding author.
E-mail address: luoyh2016@seu.edu.cn (Y.-H. Luo).

https://doi.org/10.1016/j.flatc.2020.100193
Received 8 July 2020; Received in revised form 11 August 2020; Accepted 28 August 2020
Available online 11 September 2020
2452-2627/ © 2020 Elsevier B.V. All rights reserved.
C. Wang, et al. FlatChem 24 (2020) 100193

Scheme 1. Schematic illustration of Zn-MOF@UCNPs hybrid system, and the mechanism of in-situ NIR light-triggered fluorescence enhancement.

[32]) on the 2D surfaces (Scheme 1), the obtained hybrid species Zn-
MOF@UCNPs have shown NIR (980 nm) light triggered fluorescent
enhancement, attributing to the energy match between up-conversion
luminescence (UCL) for UCNPs and ligand-to-metal charge transfer
(LMCT), from the pπ*-orbitals of ligands to 4sσ-orbitals of the Zn ions,
for 2D nanosheets. These results are expected to provide new solutions
for further application of in-situ NIR triggered molecular conversion
[33–38].
2. Results and discussion
2.1. Preparation of ultra-thin 2D nanosheets
The 3D bulk precursor [Zn(bpydc)(H2O)·H2O]n, which was initially
synthesized by Seong Huh et al., [33] exhibits a layered crystalline
structure and shows potential to be exfoliated into ultrathin 2D na-
nosheets. Within the 2D layered structure, the coordination geometry
around zinc ions is a distorted octahedral comprised by two nitrogen
atoms from bipyridine, two oxygen atoms of a carboxylate, one oxygen
atom of the other carboxylate, and one oxygen atom from the co-
ordinated water molecular (Fig. 1a). In addition, another solvated
water molecule was dissociated in the lattice, and occupied the cavity
(Fig. 1a, 1b), which was stabilized via O-H…O hydrogen bonding
contacts between water molecules and carboxylate groups (Fig. S1).
To be exfoliated from the 3D bulk precursor into ultra-thin 2D na-
nosheets, by using the top-down strategy, one should break the inter-
layer interactions (van der Waals forces, pi-pi, etc.). Note that, the 2D
layered structures are mainly supported by van der Waals bonds, as
have been revealed by the 3D Hirshfeld surface and 2D fingerprint plot
analysis, where, H…O contacts account for 19.3% of the total interlayer
interactions (Figs. S2 and S3). Thus, the materials exhibited the po-
tential to exfoliated into nanoscale sheets of atomic thickness. The
layered bulk crystals were dispersed in ethanol and treated with soni-
cation, which resulted in white-colored powdered samples of 2D na-
nosheets (Fig. 1c). notably, the obtained nanosheets can be re- dis-
persed in ethanol to stand for at least one month without sedimentation
at room temperature, accompanied by a distinct Tyndall effect
(Fig. 1d), suggesting the high stability of this kind of ultrathin 2D

Fig. 1. (a) Molecular structure of the Zn(bpydc)(H2O)·H2O unit; (b) A diagram of the 2D nanosheets along the c-axis; (c) Image of the powder samples of bulk
precursor; (d) Tyndall effect of colloidal suspension; (e) TEM image of the bulk precursor; (f, g) TEM images of the 2D nanosheets.

2
C. Wang, et al.
Fig. 2. (a) IR and (b) PXRD patterns of 2D nanosheets, bulk and the stimulation map; (c) UV–vis absorption spectra of the colloidal suspension in the different
solvents; (d) the emission spectra of the aqueous colloidal suspension of 2D in the different kinds of solvents at room temperature upon excitation at 350 nm; (e) TEM
image of UCNPs and Zn-MOF@UCNPs; (f) emission spectra (λex = 980 nm, 33.8 W cm−2).
nanosheets. To further demonstrate the successful preparation of 2D
ultra-thin nanosheets by using an ultrasonic force-assisted liquid ex-
foliation technology, the obtained ultra-thin 2D nanosheets was also
characterized by the transmission electron microscopy (TEM). The TEM
image of the 3D bulk precursor has suggested the layered structure with
nanosheets that were stacked together (Fig. 1e). While the TEM images
of 2D nanosheets have revealed the random stacked giant ultra-thin
nanosheets with unambiguous outlines and somewhat curling edges,
with lateral size was found to be larger than 1 µm. (Fig. 1f, g and Fig.
S4). These results have suggested clearly the successful preparation of
ultra-thin 2D nanosheets.
One thing should be stressed was that, the ethanol solution was
removed to collect white powder 2D nanosheets, and the single layer of
2D nanometers was re-stacked together via weak van der Waals forces
into bulk precursor, which was demonstrate by the almost identical
PXRD, IR, Raman as well as UV–vis absorption spectroscopy of the 2D
nanosheets and 3D bulk precursors (Fig. 2a, b and Fig. S5). Shown in
Fig. 2a was the IR spectra, which was dominated by an intense and wide
peak centered at 3380 and 3200 cm−1 in the high-frequency region,
which was arise from ν(O–H) stretching modes of lattice water mole-
cules. The νasym and νsym stretching of –COO– groups is at
1629 cm−1 and 1135 cm−1. The bands for pyridyl rings are as-
signed to the peaks of 1376 cm−1, and the peak of coordination water is
in 720–460 cm−1 range. PXRD patterns of both 3D bulk and 2D na-
nosheets match well the simulated one, indicating that they have ex-
actly the same frame structure (Fig. 2b). Hence, these results have de-
monstrated that the 2D nanosheets stack or aggregate together to form
3D bulk precursors during the process of solvent removal via a rotary
evaporation (temperature of 55 °C).
2.2. Fluorescent properties in different solutions
As have been mentioned previously, the large surface area of the
ultra-thin 2D nanosheets and the abundant oxygen atoms with high
electronegativity arrayed on the surfaces, may make the sample be well
3
FlatChem 24 (2020) 100193
dispersed in various solvents. As we have expected, this ultra-thin 2D
nanosheets can be suspended in all kinds of solvents with a significant
Tyndall effect. Adding on, the dispersion of the 2D nanosheets in polar
solvents (H2O, EtOH, MeOH) can cause the red shift of the UV–vis
absorption peak of the π → π* transitions (Fig. 2c), which can be at-
tributed to the effective hydrogen- bonding contacts between the pro-
tonic solvents and oxygen atoms on the surfaces of 2D nanosheets.
More importantly, each solvent has shown a unique effect on the
optical properties of the colloidal suspensions, as have been revealed by
the fluorescence spectroscopy (Fig. 2d). The fluorescence peak at the
higher wavelength changed significantly with the variation of solvent
polarity, the double emission peaks were increased with the decrease of
solvent polarity, accompanied by shift of maximum emission peak to
the lower wavelength. Moreover, due to the influence of the electron
cloud of polar solvent molecules on the fluorescence molecules, the
electron density within the nanosheets is transferred to the hydrogens
of the protonic solvents. The fluorescence spectra may be accompanied
with the phenomenon of fluorescence intensity decreasing or even
quenching. These results have suggested significantly the ultrahigh
sensitivity of the present 2D nanosheets, as a result, the loading of
UCNPs on the surfaces will certainly make a profound effect on the
fluorescent properties.
2.3. Zn-MOF@UCNPs for NIR light-triggered molecular switching
To verify the above-mentioned promising aspects, the hexagonal
phase ytterbium (Yb3+) ion sensitized UCNPs (NaYF4: 20 mol% Yb3+,
1 mol% Er3+) was selected (Fig. 2e). The latter shows a superior up-
conversion efficiency with green up-conversion UCL in the 500–700 nm
region (Fig. 2f). Note that, the bare groups of the surfaces of the na-
nosheet can ensure effective interactions between the UCNPs and ultra-
thin 2D nanosheets involving the lanthanide ions and oxygen atoms,
giving a stable hybridized system Zn-MOF@UCNPs that can be dis-
persed in aqueous solution to form a clear suspension with distinct
Tyndall effect (Fig. 3a). Note that, this hybridized suspension can stable
C. Wang, et al.
Fig. 3. (a) Optical image of Tyndall effect of an ethanolic colloidal suspension and hybrid systems under 980 nm irradiation of Zn-MOF@UCNP (The red beam comes
from a laser pen and is used to detect the Tyndall effect of the suspension); (b) TEM image of Zn-MOF@UCNPs; (c) UV–vis absorption for Zn-MOF @UCNPs hybrid
systems and UCNPs; (d) the emission spectra of the 2D and Zn-MOF@UCNPs at room temperature upon excitation at 350 nm, as well as UCL of UCNPs; (e and f) the
emission spectra of Zn-MOF@UCNPs in colloidal suspension under a 980 nm laser with different excitation times. (For interpretation of the references to colour in
this figure legend, the reader is referred to the web version of this article.)
at least one month without precipitation, and the green UCL of the
UCNPs was well maintained (Fig. 3a). Adding on, TEM images have
further demonstrated the successful formation of Zn-MOF@UCNPs hy-
bridized system (Fig. 3b and Fig. S6).
To further demonstrate the successful preparation of Zn-MOF@
UCNPs hybrid system, the UV–vis absorption of Zn-MOF@UCNPs and
2D nanosheets have been contrasted (Fig. 3c). The UV–vis absorption
spectrum of Zn-MOF@UCNPs has shown a new shoulder at around
308 nm, which can be attribute to the synergistic effect of UCNPs and
2D nanosheets, that initiated the LMCT (pπ*(ligands)-4sσ(Zn2+)) effects
within 2D nanosheets. Adding on, the fluorescence intensity of Zn-
MOF@UCNPs was decrease in the range of 350–500 nm, because of the
scattering of the emitted light from the incident light by the 2D na-
nosheets (Fig. 3d). However, the fluorescence intensity of Zn-MOF@
UCNPs was higher than 2D nanosheets in the range of 500 nm–600 nm,
owing to the well matching between UCL and LMCT. The results have
verified significantly the synergetic effects between UCNPs and 2D
nanosheets within the 2D@UCNP hybrid systems.
To investigate the NIR-triggered fluorescent properties of Zn-MOF@
UCNPs, the fluorescence spectra of Zn-MOF@UCNPs hybrid systems in
aqueous colloidal suspension was measured under irradiating with a
980 nm CW laser excitation. Zn-MOF@UCNPs has two emission peaks
at 390 nm and 436 nm (Fig. 3e). The fluorescence emission at 390 nm
was caused by LMCT, and the peak at around 436 nm can be assigned to
the charge transitions inside the ligand. There is a clear broad peak, and
the fluorescence intensity gradually decrease with the increase of ir-
radiation time at around 570 nm (Fig. 3f). It is further proved that
UCNPs can initiate LMCT of 2D nanosheets. As can be seen from the
above studies, Zn-MOF@UCNPs shows detectable in-situ NIR light
triggered luminescence enhancement, indicating potential biomedical
applications such as imaging, detection and sensing.
3. Conclusion
In summary, we have preparation ultra-thin 2D nanosheets of Zn-
4
FlatChem 24 (2020) 100193
based MOF, and examined its luminescence properties, response char-
acteristics to solvent polarity and fluorescence sensing mediated by
UCNPs. These results show that the maximum emission wavelength of
2D nanosheets in polar solvents moves to the shorter wavelength, and
the shift of the fluorescence emission spectrum of the 2D nanosheet
dispersed in different solvents is also distinct, especially the difference
between the polar solvent and the non-polar solvent. As the polarity of
the solvent decreases, the double emission peak of the sample becomes
more pronounced. More importantly, Zn-MOF@UCNPs hybrid system
shows detectable in-situ NIR light triggered luminescence enhance-
ment, which shown great potential for biomedical applications.
4. Materials and methods
4.1. Material
All the reactions were carried out at room-temperature, the chem-
icals involved in the experiments were of analytical grade and used
without further purification. Both the raw materials for Ultra-thin 2D
nanosheets [Zn(bpydc)(H2O)·H2O]n-Zn(NO3)2·6H2O, bpydc; and the
raw materials for UCNPs–NaOH, NH4F, ethanol, chloroform, toluene,
cyclohexane, trifluoroacetic acid (CF3COOH), and HCl were all ob-
tained commercially purchased from Sinopharm Chemical Reagent Co.
Ltd (China), Beijing HWRK Chem Co., Ltd. (China), and Sinopharm
Chemical Reagent Co. Ltd (China).
4.2. Characterization
The morphologies of the ultra-thin 2D nanosheets, UCNPs and Zn-
MOF@UCNPs hybridized systems were characterized by using a Field
emission scanning electron microscope transmission electron micro-
scope (TEM; Tecnai-G2 20 E-TWIN 200 KV). Before these microscope
characterizations, the aqueous suspension of the ultra-thin 2D na-
nosheets was dropping onto the holey carbon-coated carbon support
copper grids, Si/SiO2, piranha-cleaned Si/SiO2, and then naturally
C. Wang, et al.
dried. X-ray powder diffraction (PXRD) experiments were performed by
using a Bruker D8 Focus with an X-ray tube with a Cu target. Infrared
spectra were recorded on a Shimadzu IR Prestige-21 FTIR-8400S
spectrometer in the spectral range 4000–500 cm−1, with the samples in
the form of potassium bromide pellets. The emission spectra of Zn-
MOF@UCNPs and 2D colloidal suspensions were excited at 350 nm
with a LS 55 Luminescence Spectrometer. (The solvent of the colloidal
suspension is ethanol solution). And the emission spectra of the Zn-
MOF@UCNPs in colloidal suspension under a 980 nm laser with dif-
ferent excitation times was also excited at 350 nm. UCL spectra of Zn-
MOF@UCNPs were measured with a fluorescence spectrometer
(Edinburgh, LFS-920) using an external CW 980 nm laser (Xi’an
Saipulin Laser Technology Institute, China) with a tunable power of
0–3 W acting as the excitation source. UV–vis absorption and the
fluorescence spectra were recorded with a Shimadzu UV-3150 double-
beam spectrophotometer and a Horiba Fluoro-Max4 Spectro-fluo-
rometer, respectively. The irradiation experiments were performed by
using a CW 980 nm NIR laser (SD980- 5000G3, Xi’an Saipulin Laser
Technology Institute, China) with a laser power density of 1.5 W/cm2.
4.3. Preparation of ultra-thin two-dimensional nanosheets
20 mg of bulk precursor [Zn(bpydc)(H2O)·H2O]n was dissolved in
100 ml of ethanol solution. Dispersion was carried out in an ultrasonic
bath (Branson, CPX2800H-E, 110 W, 40 kHz) for 1 h. After the end of
the ultrasonic peeling, stirring was continued for one night. The ob-
tained suspension was allowed to stand for one week, and the sediment
which settled and settled was removed by centrifugal separation. The
ultra-thin two-dimensional nanosheet colloidal suspension was ob-
tained.
4.4. Preparation of Zn-MOF@UCNPs hybrid system
3 mg of NaYF4: 20 mol% Yb3+, 1 mol% Er3+ were uniformly dis-
persed in 9 ml of ethanol solvent in a 25 ml beaker. Then, 9 ml of
colloidal suspension the ultra-thin 2D nanosheets [Zn(bpydc)
(H2O)·H2O]n was added dropwise, stirred at room temperature for 11 h,
then allowed to stand for 12 h, and the sediment was removed by
centrifugation at 1000 rpm to obtain a well-dispersed Tyndall solution.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Acknowledgments
This research was supported by the Natural Science Foundation of
China (Grant No. 21701023), Natural Science Foundation of Jiangsu
Province (Grant No. BK20170660), Zhishan Youth Scholar Program of
SEU and PAPD of Jiangsu Higher Education Institutions.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://
FlatChem 24 (2020) 100193
doi.org/10.1016/j.flatc.2020.100193.
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