Journal of Alloys and Compounds 853 (2021) 157375

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Low ligand field strength ion (I
) mediated 1D inorganic material

MoI3: Synthesis and application to photo-detectors
Kyung Hwan Choi a, 1, Seungbae Oh b, 1, Sudong Chae b, Byung Joo Jeong b, Bum Jun Kim a,
Jiho Jeon a, Sang Hoon Lee b, Sang Ok Yoon b, Chaeheon Woo b, Xue Dong a,
Asghar Ghulam a, Changmo Lim b, Zhixiang Liu a, Cong Wang b, Ali Junaid a,
Jae-Hyun Lee c, Hak Ki Yu c, *, Jae-Young Choi a, b, **
a
SKKU Advanced Institute of Nanotechnology (SAINT), Sungkyunkwan University, Suwon, 16419, Republic of Korea
b
School of Advanced Materials Science & Engineering, Sungkyunkwan University, Suwon, 16419, Republic of Korea
c
Department of Materials Science and Engineering & Department of Energy Systems Research, Ajou University, Suwon, 16499, Republic of Korea

a r t i c l e i n f o a b s t r a c t

Article history: A new type of 1D inorganic material, MoI3, which can be separated into individual 1D chains, was
Received 10 August 2020 synthesized through a vapor transport reaction between molybdenum and iodine. High-purity and
Received in revised form centimeter-scale large MoI3 crystals were obtained by controlling the growth temperature and the
25 September 2020
stoichiometric ratio between molybdenum and iodine. Their semiconductor characteristics were
Accepted 27 September 2020
Available online 28 September 2020
confirmed by measuring the electrical conductivity as a function of temperature (conductivity increased
with increased temperature across the range
70 to 30  C). Furthermore, it was confirmed that MoI3
with a 1.27 eV band gap can be separated to a few nanometer scale through mechanical and chemical
Keywords:
1D inorganic materials
exfoliation methods and can be used as a photodetector in the near IR (less than 1000 nm)-to-visible
MoI3 light region. This novel 1D material is expected to play an important role in the development of addi-
Photodetectors tional low-dimensional materials and in advanced nano-optoelectronic devices.
Mechanical exfoliation © 2020 Elsevier B.V. All rights reserved.

1. Introduction
Low-dimensional (2D and 1D) materials, which have been
extensively studied in recent years, mainly form a unit crystal
structure through ionic bonds between transition metals (such as
Mo, Nb, W, Ta, and V) and group 16 chalcogenide elements (Se and
S). Such materials form a 3D bulk structure through weak van der
Waals (vdW) bonds between unit crystals [1e8]. These low-
dimensional materials can have band gaps of ~1 eV, which is suit-
able for using as a semiconductor electronic device. They also have
limitations, including atmospheric instability and low charge mo-
bilities [9e12]. Therefore, it is necessary to devise a method to find
new types of low-dimensional materials to enhance material di-
versity of low-dimensional material-based devices.
* Corresponding author.
** Corresponding author. SKKU Advanced Institute of Nanotechnology (SAINT),
Sungkyunkwan University, Suwon, 16419, Republic of Korea.
E-mail addresses: hakkiyu@ajou.ac.kr (H.K. Yu), jy.choi@skku.edu (J.-Y. Choi).
1
K.H. Choi and S. Oh contributed equally to this work.
Halogen ions (F
, Cl
, Br
, and I
), which have four paired
electrons, can form various chemical compounds through ligand
field-induced bonding with several transition elements [13e15].
The intensity of the ligand field varies depending on the ligand
polarizability. The smaller the ion, the stronger the attraction be-
tween its nucleus and outermost electrons, thereby resulting in
decreased polarizability and in increased intensity of the ligand
field accordingly. In contrast, if the ion is large, such as I
, the effect
of ligand field on the d orbitals of the transition metal decreases so
that M-X-M angle in octahedral configuration also decreases,
leading to short distances between the central cations. Therefore,
the binding force between the ligand compounds is weakened such
as vdW forces because the strong interactions are limited only
along the direction of central cations [16e23]. That is, these ma-
terials are likely to be used as new, low-dimensional materials, by
exfoliating between unit materials, such as the vdW-based mate-
rials [24e27].
In this study, we designed experiments by selecting molybde-
num (Mo) among the elements having a 4d orbital, to be coordi-
nated by I
ions, because the Mo forms 2D chalcogenides easily

https://doi.org/10.1016/j.jallcom.2020.157375
0925-8388/© 2020 Elsevier B.V. All rights reserved.
K.H. Choi, S. Oh, S. Chae et al.
(such as MoS2 and MoSe2) [1,4]. By examining the stability of the
phase, based on the crystal structure, it was confirmed that the
MoI3 phase, which is assigned to the orthorhombic space group
Pmmn and composed of bonds between Mo-centered ions and I
in
a face-sharing octahedral configuration, forms a basic chain and can
form a 3D structure through weak vdW bonding between chains
(Fig. 1a) [28,29]. MoI3 was placed in a vacuum ampule in accor-
dance with stoichiometry to induce the reaction, and the structure
of the synthesized material, bandgap measurement, and the pos-
sibility of single chain exfoliation were evaluated to investigate the
possibility of a new type of 1D material. Furthermore, experiments
were conducted to demonstrate that it can be used as a photode-
tector by utilizing the band gap of the synthesized material.
2. Materials and methods
2.1. Synthesis
Single crystals of MoI3 were grown via a chemical vapor trans-
port (CVT) method. Elemental powders of Mo (99.9%, 1e5 mm,
Sigma-Aldrich) and iodine (crystalline, 99.99þ%, Alfa Aesar) were
thoroughly mixed with a molar ratio of 1:4 and sealed into a 15 cm-
long quartz tube (inner diameter ¼ 1.2 cm) under vacuum. The
quartz tube was placed in a horizontal tube furnace, heated to
400  C for 120 h, with a temperature gradient to 350  C at one end,
and then gradually cooled to room temperature. After the reaction,
long needle-like MoI3 crystals were formed at the cold end, and
these were collected mechanically. Excess iodine on the surface of
crystals was removed by sublimation in a tube furnace at 100  C
under Ar flow.
2.2. Exfoliation
The MoI3 was placed on wafer dicing tape (BT150E-KL, Nitto),
and the materials were stuck several times to yield thinner-than-
bulk materials. A substrate of SiO2/Si was cleaned by ultra-
sonication in acetone, ethanol, and deionized water for 15 min,
followed by heating at 100  C to remove moisture from the SiO2/Si
Fig. 1. (a) Crystal structure of MoI3. (b) Growth mechanism of MoI3 through chemical vapor transport method. (c) SEM image of bulk MoI3 crystal. Inset is an optical image of bulk
MoI3 crystal (scale bar: 0.5 cm).
2
Journal of Alloys and Compounds 853 (2021) 157375
surface. The polymer tape was strongly adhered to, and pressed
against, the SiO2/Si substrate. After adhesion, the polymer tape was
removed from the SiO2/Si substrate; this process was repeated for
exfoliation.
2.3. Characterization
XRD (D8 Advance, Bruker) was performed using Cu Ka radiation
(l ¼ 0.154 nm). Field-emission scanning electron microscopy (FE-
SEM, Hitachi, S-4300SE) and an energy dispersive spectrometer
(EDS) attached to the FE-SEM were used for morphological and
compositional analysis. Atomic force microscopy (AFM, Park sys-
tems, NX 10) was performed in non-contact mode for topographic
analysis of the mechanically exfoliated MoI3 on SiO2/Si substrates.
An aberration-corrected scanning transmission electron micro-
scopy (Cs-STEM, JEOL, JEM-ARM200F) was operated at an acceler-
ation voltage of 80 kV. Diffuse-reflectance UVeViseNIR
spectrophotometer (Shimadzu, SolidSpec-3700) was performed at
room temperature in the 200e2500 nm range. A current-voltage
curve (Vacuum chamber probe-station, MSTECH, M6VC) was ob-
tained in the temperature range
70 to 30  C for exfoliated MoI3.
Electrical contact, Cr/Au, was deposited using TEM grid as a shadow
mask. Photo-reactive response properties using four-probe tech-
nique were characterized using a laser at wavelengths of 635 and
1342 nm. Laser power was calibrated using a laser power meter.
Photo switching was examined by turning the laser on and off.
3. Results and discussion
In general, the crystal growth in CVT method occurs when the
reactants volatilized in the reaction zone is transferred to and
deposited in a growth zone with an appropriate temperature
gradient [30]. To determine the optimal conditions for synthesis of
MoI3, experiments were conducted using different composition
ratios of Mo/I and reaction temperatures. The higher the reaction
temperature and the higher the amount of Mo, the more stable is
the thermodynamically stable phase, MoI2 (Fig. S1). Therefore, in
this experiment, a temperature of reaction zone was maintained at
K.H. Choi, S. Oh, S. Chae et al.
400  C, but the amount of iodine was increased (the amount of Mo
was relatively small). As the growth proceeds, the crystals gradually
grow into long (centimeter-scale) needle-like single crystals due to
the intrinsic 1D structure characteristics of MoI3 (Fig. S2). Although
the actual reaction zone temperature was 400  C, the temperature
of the transport zone was 350  C, and it was confirmed that the
MoI3 phase can be stabilized (Fig. 1b). In the optical and electron
micrographs of the synthesized crystals, a long shape can be
observed in one direction, and the thickness was tens of micro-
meters (Fig. 1c).
X-ray diffraction results demonstrated that a pure single phase
MoI3 was synthesized (Fig. 2a). The reason for the (200) preferred
orientation is that the alignment occurred in the process of trans-
ferring the centimeters-long wires, obtained in the transport zone,
to the substrate for XRD measurement. In addition, the Mo 3d core
level XPS spectrum shows that the Mo3þ was evidently seen in the
Mo 3d core level XPS spectrum (Fig. 2b), demonstrating that MoI3
was successfully synthesized in accordance with stoichiometry (see
the supporting information about survey scan and I 3d spectrum,
Fig. S3). The presence of Mo4þ and Mo6þ in the spectrum are
attributed to oxides formed on the surface when the crystals are
exposed to air after synthesis [31]. To perform TEM analysis, the
MoI3 single crystal was dispersed in isopropyl alcohol (IPA; Fig. S4),
and it was confirmed that a thread-shape appeared easily (Fig, 2c).
This is considered because there is only a weak vdW bond between
the unit chains. The HR-TEM image and Fourier transformation
analysis confirmed that the synthesized material is a MoI3 material
having 0.712 nm between unit chains, corresponding to (001) plane
(Fig. 2d and e).
To evaluate the electrical and optical properties of the synthe-
sized material, changes in electrical resistance as a function of
Fig. 2. (a) XRD pattern of the as-synthesized crystalline MoI3. Black lines at the bottom represent the calculated powder pattern of MoI3 in space group Pmmn. (b) XPS spectrum of
Mo 3d peak of the as-synthesized MoI3. (c)e(e) TEM images and fast Fourier transform pattern (inset) of dispersed MoI3 chains.
3
Journal of Alloys and Compounds 853 (2021) 157375
temperature and light absorption were measured. In the electrical
conductivity measurement according to the temperature change,
the Electrical conductivity increased as temperature increased
from
70 to 30  C (Fig. 3a). This phenomenon occurs in typical
semiconductor materials, and thus it was confirmed that the syn-
thesized MoI3 has semiconductor properties. To measure the band
gap of MoI3, UVevis diffuse reflectance spectroscopy (DRS) was
measured (Fig. 3b). A Tauc plot (inset) confirmed that the band gap
was approximately 1.27 eV. As 1.27 eV corresponds to a wavelength
in the 1000 nm region, it can be used as a photodetector that ab-
sorbs light from the near IR (less than 1000 nm)-to-visible light
region [32e35]. In order to verify the measured band gap and
possibility to a photodetector, measurements of photoelectric
reactivity to a light source of 635 nm, corresponding to visible light,
and 1342 nm, corresponding to IR, was performed. (Fig. 3c). There
was almost no reaction at 1342 nm because MoI3 has a band cor-
responding to 1000 nm and the energy of incident light is insuffi-
cient to make excitation of free electron-hole pairs. On the other
hand, at 635 nm which is an energy larger than the band gap of
MoI3, there was steep rising and falling in current with respect to
light on and off, which is attributed to photoelectric effect [36]. The
gradual increase in current after rapid current rising is mainly
caused by the thermal effect. In addition, the photocurrent
increased proportionally to increased light intensity at 635 nm
(Fig. 3d), which suggests that it can be used as an excellent
photodetector in the near IR (less than 1000 nm)-to-visible light
region.”
To utilize the semiconductor characteristics MoI3, with a band
gap of 1.2 eV, to low-dimensional devices, the possibility of unit
chain exfoliation must also be verified. The MoI3 chain that was
primarily exfoliated through mechanical exfoliation (Fig. 4a, c) had
K.H. Choi, S. Oh, S. Chae et al. Journal of Alloys and Compounds 853 (2021) 157375

Fig. 3. (a) Electrical conductivity of MoI3, with T ranging from 200 to 300 K. (b) UVevis DRS spectrum of MoI3. Inset shows a Tauc plot of the absorption spectrum. (c) Time function
of the on-off photocurrent response at different light sources; visible (635 nm) and IR (1342 nm) lasers. (d) Current change with respect to visible light intensity.

Fig. 4. (a) AFM image of the mechanical exfoliated MoI3 on a 300 nm SiO2/Si substrate. Inset shows an optical microscope image of exfoliated MoI3. (b) AFM image of the exfoliated
MoI3 after additional peeling process. (c) and (d) Line profile of the MoI3 before and after a second exfoliation.

4
K.H. Choi, S. Oh, S. Chae et al.
a thickness of approximately 70 nm. When the AFM was applied in
the same region by performing an additional exfoliation, it was
confirmed that mechanical exfoliation proceeded to 5e7 nm
(Fig. 4b, d). A better optimized peeling process and chemical
exfoliation (using solutions and dispersants) may demonstrate that
the ultimate unit chain exfoliation and device application will be
possible.
4. Conclusions
In this study, a new 1D material (MoI3) was successfully syn-
thesized through a chemical vapor transport reaction. The MoI3
crystal contained bonds between Mo-centered ions and I
in an
octahedral configuration, forming a basic chain and a 3D structure
through weak vdW bonding between chains. These chains can be
separated to a few nanometers through mechanical and chemical
exfoliation methods because of their weak interactions between
chains. MoI3, which exhibited semiconductor characteristics, has a
band gap of 1.27 eV and can be used as a photodetector in the near
IR (less than 1000 nm)-to-visible light region. This new type of 1D
material is expected to play an important role in the development
of other low-dimensional materials and in modern nano-
optoelectronic devices.
CRediT authorship contribution statement
Kyung Hwan Choi: Methodology, Data curation, Writing -
original draft, Writing - review & editing, Writing. Seungbae Oh:
Methodology, Data curation. Sudong Chae: Data curation, Formal
analysis. Byung Joo Jeong: Data curation, Formal analysis. Bum Jun
Kim: Formal analysis. Jiho Jeon: Data curation. Sang Hoon Lee:
Formal analysis. Sang Ok Yoon: Data curation. Chaeheon Woo:
Data curation. Xue Dong: Formal analysis. Asghar Ghulam: Formal
analysis. Changmo Lim: Data curation. Zhixiang Liu: Data cura-
tion. Cong Wang: Data curation. Ali Junaid: Data curation. Jae-
Hyun Lee: Writing - original draft, Writing - review & editing,
Writing. Hak Ki Yu: Writing - original draft, Writing - review &
editing, Writing, Supervision, Funding acquisition. Jae-Young Choi:
Supervision, Funding acquisition.
Declaration of competing interest
The authors declare that they have no known competing
financial interests or personal relationships that could have
appeared to influence the work reported in this paper.
Appendix A. Supplementary data
Supplementary data to this article can be found online at
https://doi.org/10.1016/j.jallcom.2020.157375.
Acknowledgment
Funding
This research was supported by the Basic Science Research
Program through the National Research Foundation of Korea (NRF),
funded by the Ministry of Science, ICT & Future Planning (NRF-
2019R1A2C1006972, NRF-2020R1A2C2010984).
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