PROPOSAL

RESEARCH INTERNSHIP IN
TAIWAN EXPERIENCE EDUCATION PROGRAM (TEEP)
NATIONAL TAIWAN UNIVERSITY

ELYSA UMIATI
21/476555/PA/20580

Supervisor:
Prof. Indriana Kartini, S.Si., M.Si., Ph.D.
1 9690421 199803 2 002

DEPARTMENT OF CHEMISTRY
FACULTY OF MATHEMATICS AND NATURAL SCIENCES
UNIVERSITAS GADJAH MADA
YOGYAKARTA
2024
 RESEARCH INTERNSHIP PROPOSAL
TAIWAN EXPERIENCE EDUCATION PROGRAM (TEEP)
NATIONAL TAIWAN UNIVERSITY

GROWTH AND ATOM-RESOLVED STUDIES OF 2D TRANSITION

METAL DICHALCOGENIDES: FOCUSING ON TIS2 THIN FILMS AND
TIS2/TISE2 HETEROSTRUCTURES

ELYSA UMIATI
21/476555/PA/20580

Supervisor:
Prof. Indriana Kartini, S.Si., M.Si., Ph.D.
1 9690421 199803 2 002

DEPARTMENT OF CHEMISTRY
FACULTY OF MATHEMATICS AND NATURAL SCIENCES
UNIVERSITAS GADJAH MADA
YOGYAKARTA
2024
 RATIFICATION PAGE

Internship Location : National Taiwan University

Department : Center for Condensed Matter Sciences
Internship Addressed : #1, Sec. 4, Roosevelt Rd., Taipei 106 Taiwan
Name Participant : Elysa Umiati
NIM : 21/476555/PA/20580
Home Addressed : National Taiwan University of Dormitory
Phone : +62 82335164344
E-mail : elysa.umiati@mail.ugm.ac.id
Internship Duration : 4th months (March 1st to July 1st, 2024)

Yogyakarta, January 25th, 2024

Supervisor, Student,

Prof. Indriana Kartini, S.Si., M.Si., Ph.D. Elysa Umiati

NIP 1 9690421 199803 2 002 NIM 21/476555/PA/20580

Head of the Chemistry Study Program

Faculty of Mathematics and Natural Sciences
Universitas Gadjah Mada

Prof. Indriana Kartini, S.Si., M.Si., Ph.D.

NIP 1 9690421 199803 2 002

iii
 PREFACE

In this preface, I humbly extend my profound gratitude and praises to Allah

SWT, whose ceaseless mercy and guidance have been the cornerstone of my
journey through the challenging yet enriching process of completing the MBKM
Research Internship Proposal. This undertaking, pivotal in my academic and
professional growth, was conducted at the esteemed National Taiwan University,
focusing on the intricate field of “The Growth Of 2D Transition Metal
Dichalcogenide Ultrathin Films And Characterization.” The compilation of this
proposal is not just an academic exercise but a significant component fulfilling the
stringent requirements of the MBKM Research program.
The journey of developing this research proposal was an amalgamation of
rigorous scientific inquiry and collaborative efforts. Throughout this process, I was
fortunate to be under the tutelage and supervision of distinguished academicians
and researchers whose contributions have been invaluable. Their guidance was not
only instrumental in shaping the research but also in enriching my understanding
and appreciation of the complex nuances of chemistry and material science. I would
like to express my sincere appreciation and gratitude to:
1. Prof. Indriana Kartini, S.Si., M.Si., Ph.D., whose leadership as the Head of
the Chemistry Study Program and who has been an exemplary supervising
lecturer throughout my research journey. Provided me with the academic
rigor and intellectual freedom necessary for exploring new frontiers in
chemistry.
2. Dr.rer.nat. Nurul Hidayat Aprilita, M.Si., the Head of the Chemistry
Department, whose profound insights and administrative support were
crucial in navigating the intricate aspects of the research process.
3. Prof. Dr. Endang Tri Wahyuni, M.S., who played a pivotal role as the Head
or Person-in-Charge of the MBKM Research Program.
4. Dr. Woei Wu Pai, a distinguished Joint Professor of Physics and research
fellow at the Center for Condensed Matter at National Taiwan University.
His collaborative spirit and profound expertise in condensed matter physics
significantly enhanced the scope and depth of my research.
5. The entire faculty of Chemistry Lecturers at Gadjah Mada University,
whose collective wisdom, extensive guidance, and insightful advice
provided in my research capabilities.
I am deeply grateful to everyone who has been a part of this journey,
especially to Allah SWT, for the endless blessings and guidance. This preface is a
small token of my immense appreciation for the collective wisdom, encouragement,
and support extended to me by my esteemed mentors and the academic community.
Their impact on my life and career will be a source of inspiration and motivation as
I continue my path of learning and discovery.

iv
 TABLE OF CONTENTS

Ratification Page ........................................................................................ iii

Preface ......................................................................................................... iv
Table of Contents ........................................................................................ v
Figure Captions .......................................................................................... vi
Abstract ..................................................................................................... vii
Chapter 1 Introduction ................................................................................ 1
1.1 Background ................................................................................... 1
1.2 Purpose of the Research ................................................................ 3
1.3 Time and Place the Research ........................................................ 3
1.4 Center for Condensed Matter Sciences (CCMS) .......................... 3
Chapter 2 Literature Review and Hypothesis ............................................. 5
2.1 Literature Review .......................................................................... 5
2.1.1 Synthesis and Properties of VI-based TMDs ....................... 5
2.1.2 Synthesis, Properties, and Applications of Heterostructures 5
2.1.3 TiS2 Atomic Thin Films ....................................................... 6
2.1.4 TiS2/TiSe2 Heterostructure ................................................... 7
2.1.5 Molecular Beam Epitaxy ..................................................... 7
2.1.6 Scanning Tunneling Microscopy ......................................... 8
2.2 Hypothesis Formulation ................................................................ 9
Chapter 3 Research Methods ..................................................................... 11
3.1 Materials ...................................................................................... 11
3.2 Equipment ..................................................................................... 11
3.3 Procedures .................................................................................... 11
3.3.1 Preparation of STM Tip Etching ........................................ 11
3.3.2 Mounting the HOPG Sample into Sample Plate ................ 12
3.3.3 Growth Process using Molecular Beam Epitaxy ............... 12
3.3.4 Scanning Tunneling Microscopy Imaging and Analysis .... 13
Chapter 4 Result and Discussion............................................................... 17
Chapter 5 Obstacles and Future Works ..................................................... 27
References ................................................................................................. 29

v
 FIGURE CAPTIONS

Figure 1. Schematic showing the synthesis methods of TMDs, to-down and

bottom-up approaches ......................................................................................... 5
Figure 2. 2D transition metal dichalcogenides based heterostructures for electrical,
opto-electronic, sensors, and energy devices ...................................................... 6
Figure 3. (a) cracked polished tungsten wire (b) normal polished tungsten .... 12
Figure 4. Ideal STM Tip before Tip Etching Process ....................................... 12
Figure 5. Tip Etching Set.................................................................................. 12
Figure 6. (a) good tip ; (b) bad tip, not sharp ; (c) bad tip, too long ................ 13
Figure 7. Bell Jar and Vacuum Pump ............................................................... 13
Figure 8. (a) uncleaved sample plate (b) cleaved sample ................................ 14
Figure 9. a) wielding process b) The welding % energy required.................... 14
Figure 10. Cleaved HOPG under Microscope ................................................. 15
Figure 11. Area Scan Panel in LT STM ........................................................... 16
Figure 12. dI/dV Reference .............................................................................. 17
Figure 13. TiS2 Thin Films analyzed through LT STM ................................... 18
Figure 14. TiS2/TiSe2 Heterostructure analyzed through LT STM ................. 18
Figure 15. TiS2 Thin Film analyzed form Fourier Transform ......................... 19
Figure 16. TiS2/TiSe2 Heterostructure analyzed form Fourier Transform ...... 19
Figure 17. Hexagonal Structure of (a) TiS2 thin film and (b) Heterostructure 20
Figure 18. Defect Analysis for (a) 2D and (b) 3D Visualization of the TiS₂/TiSe₂
Heterostructure .................................................................................................. 21
Figure 19. Defect Analysis for (a) 2D and (b) 3D Visualization of the TiS₂ Thin
Film ................................................................................................................... 22
Figure 20. (a) Log. Scales and (b) Linear scales of PSD Curve ...................... 23
Figure 21. TiS2/TiSe2 Heterostructure analyzed form Fourier Transform ...... 23
Figure 22. TiS2 Thin Film analyzed form Fourier Transform ......................... 25
Figure 23. (a) Log. Scales and (b) Linear scales of PSD Curve ...................... 25

vi
 GROWTH AND ATOM-RESOLVED STUDIES OF 2D TRANSITION
METAL DICHALCOGENIDES: FOCUSING ON TIS2 THIN FILMS AND
TIS2/TISE2 HETEROSTRUCTURES

Elysa Umiati
21/476555/PA/20580

ABSTRACT

This research focuses on the growth and atom-resolved studies of two-

dimensional (2D) transition metal dichalcogenides (TMDCs), specifically TiS2 thin
films and TiS2/ TiSe2 heterostructures, using Molecular Beam Epitaxy (MBE) and
Scanning Tunneling Microscopy (STM). The study aims to synthesize high-quality
TiS2 thin films through MBE, analyzing the impact of various growth parameters
on the crystal quality and electronic properties. By leveraging STM, the research
seeks to achieve atomic-level characterization, providing detailed insights into the
charge density wave (CDW) phenomena and electronic structure of TiS2.
Additionally, the research explores the formation and properties of TiS2/ TiSe2
heterostructures, examining the interfacial effects on CDW stability and electronic
behaviour.
The process involves meticulous preparation and annealing of Highly
Oriented Pyrolytic Graphite (HOPG) substrates, precise control of growth
parameters, and the deposition of TiS2 and TiSe2 layers. The growth conditions are
carefully monitored and adjusted to maintain optimal conditions for high-quality
deposition. The samples are then characterized using STM to visualize atomic
surface morphology and electronic density of states. This detailed analysis aims to
establish a comprehensive understanding of the relationships between synthesis
conditions, structural characteristics, and electronic properties in these 2D
materials.
The research also investigates the potential catalytic applications of TiS2 and
TiS2/ TiSe2 heterostructures by linking their electronic properties and CDW
behaviour to catalytic performance. The ultimate goal is to develop advanced
materials with tailored properties for use in nanoelectronics, optoelectronics, and
energy conversion technologies. By overcoming challenges such as precise growth
control and achieving atomic resolution, this study aims to contribute significantly
to the field of 2D materials and their practical applications.

Keywords: 2D transition metal dichalcogenides, Molecular Beam Epitaxy,

Scanning Tunneling Microscopy, TiS2 thin films, TiS2/ TiSe2 heterostructures.

vii
 CHAPTER 1
INTRODUCTION

1.1 Background
Recently, there have been many research break throughs in two-dimensional (2D)
materials including graphene, boron nitride (h-BN), black phosphors (BPs), and transition-
metal dichalcogenides (TMDCs). The unique electrical, optical, and thermal properties in
2D materials are associated with their strictly defined low dimensionalities. These materials
provide a wide range of basic building blocks for next-generation electronics (Choi et al.,
2022). Graphene has been unambiguously produced and identified, soon causing a boom in
global research on 2D materials. Graphene shows great potential in electronics, composites,
and catalyst due to its great conductivity, high electron mobility, and high surface area.
According to quantum mechanics, finite-size effects have been theoretically predicted and
experimentally confirmed. Many studies have utilized a new type of graphene nanostructure,
graphene quantum dots (GQDs), whose sizes are smaller than 100 nm (Wang and Lu, 2015).
Transition metal dichalcogenides (TMDCs) is 2D layered semiconductor materials
with a chemical bond within an in-plane structure and an attraction by Van der Waals force
between layers, have attracted much attention in recent years. For example are the
molybdenum disulfide (MoS2), tungsten disulfide (WS2), molybdenum diselenide (MoSe2),
and tungsten diselenide (WSe2) are noted for their low cost, abundance, and easy processing.
Two-dimensional (2D) transition metal dichalcogenides (TMDs) have emerged as a class of
materials with unique electronic, optical, and catalytic properties, making them promising
candidates for various applications in nanoelectronics, optoelectronics, and energy
conversion. Among these materials, titanium disulfide (TiS2) and its heterostructures, such
as TiS2/TiSe2, have garnered significant interest due to their intriguing charge density wave
(CDW) phenomena, electronic properties, and potential for catalytic applications.
Meanwhile, 2D materials with a high surface area and high conductivity have also attracted
much attention in recent years. There is a transformation from indirect bandgap to direct
bandgap when 2D materials are stripped from bulk ones to monolayers. Studies have shown
that 2D materials show promise in catalyst and energy storage because of their unique
1
properties and structure. Similar for graphene, in bulk transition metal dichalcogenides
(TMDs) adjacent layers are bonded through Van der Waals interactions. This bonding
characteristic facilitates the separation of TMDs into monolayer and few-layer crystals using
various methods. These methods include mechanical exfoliation with Scotch tape, Molecular
Beam Epitaxy (MBE), and chemical vapor deposition (CVD). The synthesis of atomically
thin, large-scale TMDs is crucial for unlocking their novel properties and advancing their
application in various fields (Regan et al.,2022). Electronic band gaps are crucial in
determining a materials conductivity and optical properties influencing the performance of
semiconductor devices in fields like electronics and optoelectronics. Wide bandgap materials
facilitate the development of smaller, faster, and more efficient electronic components. Two-
dimensional TMDCs have become key in various applications, ranging from nanoelectronics
to sensing, due to their unique bandgap properties and structural versatility (Chaves et al.,
2020).
The upcoming proposed research internship at National Taiwan University, focused
on “Growth and Atom-resolved Studies of 2D Transition Metal Dichalcogenides,” will
further explore these TMDCs involve synthesizing and analysing ultrathin films of these
TMDCs. This project will utilize techniques such as atomic force microscopy, Raman
spectroscopy, X-ray Diffraction, and Scanning Tunneling Microscopy. This research
internship conducted by the Taiwan Experience Education Program (TEEP). This program
is a prestigious and comprehensive initiative by the Taiwan government, aimed at fostering
global talent and promoting international educational and cultural exchange. This program
offers a unique opportunity for international students and professionals to engage in
internships and educational experiences across various sectors in Taiwan. TEEP also allows
international students to gain an in-depth educational experience in Taiwan while also
preparing themselves for the Asian job market.

1.2 Purpose of the Research

This research that will be conducted about the following objectives.
2
 1. Explore how to doping the TiS2 and TiS2/TiSe2 heterostructure with various
elements during the MBE growth impacts the stability and properties of CDW.
2. Compare the CDW phenomena in TiS2 thin films and TiS2 on TiSe2
heterostructure, and understand the interfacial effects on CDW stability and
electronic properties.
3. Perform atom-resolved STM studies to visualize the atomic surface morphology
and electronic density of states in both pure TiS2 and TiS2/TiSe2 heterostructures.
4. Assess the potential of TiS2 and TiS2/TiSe2 heterostructures for catalytic
applications by linking their electronic properties and CDW behaviour to
catalytic performance.

1.3 Time and Place the Research

The research internship will be take place in the Surface Nanoscience Laboratory at
the Center for Condensed Matter Science (CCMS) department in the National Taiwan
University. This research internship will be held from March 1st, 2024 to June 21st, 2024.

1.4 Center for Condensed Matter Sciences (CCMS)

The Center for Condensed Matter Sciences (CCMS) at National Taiwan University
is known to be a prominent interdisciplinary research institute. Established in October 1992,
CCMS primarily focuses on conducting cutting-edge research in the field of condensed
matter sciences. This involves exploring the physical properties of solid and liquid matter
through experimental, theoretical, and applied research approaches.
The Center has objectives typically include advancing basic and applied research in
condensed matter sciences, fostering an environment conducive to innovative research, and
developing interdisciplinary curricula. This is aimed at cultivating new generations of
researchers who are adept in the complexities and advancements in condensed matter
sciences.
CCMS is known to collaborate with various departments and research institutions,
both nationally and internationally, pooling expertise from fields like physics, chemistry,

3
materials science, and engineering. This collaborative approach enables the Center to stay at
the forefront of research and technological development in condensed matter sciences.
Currently, the CCMS have 12 regular research faculty members, 7 additional faculty
members through joint appointments, 2 NSC research scholars, more than 20 postdoctoral
associates, and over 100 graduate students and assistants. The research work at CCMS has
been focused in the following two areas which is emergent materials and advances devices
and spectro-microscopy.

4
 CHAPTER 2
LITERATURE REVIEW AND HYPOTHESIS

2.1 Literature Review

2.1.1 Synthesis and Properties of VI-based TMDs
The transition metal dichalcogenides (TMDSs) monolayer (MX2) have three
atom layers with a transition metal atom such as Mo or W sandwiched by two layers
of chalcogen atom layer (S, Se, or Te). In order to produce the monolayer of these
TMDCs, the methods including the top-down and bottom up have been used. The
top-down methods such as the mechanical exfoliation, electrochemical, and chemical
exfoliation or direct sonication in solvents, only can produce few-layer crystals with
small size and low quality. The bottom-up methods including the chemical vapor
deposition (CVD) and physical vapor deposition PVD method have been used to
synthesis of large-size 2D TMDs monolayer substrate (Joseph et al., 2023).

Figure 1. Schematic showing the synthesis methods of TMDs, to-down and

bottom-up approaches (Joseph et al., 2023)

2.1.2 Synthesis, Properties, and Applications of Heterostructures

TMDs based heterostructures have garnered significant attention due to their
exceptional physical and chemical characteristics, which are crucial for both
fundamental studies and a range of applications such as electronics, sensing,
photonics, and energy-related devices. The unique attributes of these layered

5
materials, including adjustable electronic structures, optical transparency, peak
electrostatic efficiency, and heightened sensor sensitivity, render them highly suitable
for diverse technological uses. The weak Van der Waals interactions between layers
in these materials facilitate the creation of high-quality, atomically precise
heterostructures. This section aims to highlight the key applications of TMD-based
heterostructures, particularly in fields like optoelectronics, sensors, photovoltaic
systems, and energy devices (Joseph et al., 2023).

Figure 2. 2D transition metal dichalcogenides based heterostructures for electrical,

opto-electronic, sensors, and energy devices (Joseph et al., 2023)
Traditional 2D TMDs heterostructures are often obtained via combining the
TMDs with different chemical composition and properties by sequential mechanical
methods which has been used to fabricate the heterostructures such as MoS2/MoSe2,
MoS2/WS2. However, these heterostructure show a small overlap in sample size and
their interface contamination is difficult to avoid (Novoselov et al., 2016).

2.1.3 TiS2 Atomic Thin Films

Among various transition metal dichalcogenides TiS2 owing to its layered
structure, variable energy bandgaps, and optoelectronic properties has been
extensively studied recently. The layered structure of TiS2 takes the form of S-Ti-S
units bonded through weak Van der Waals forces where the Ti atoms are stacked
between the two hexagonal planes comprising S atoms. TiS2 is an inorganic low-cost
stable earth abundant material with high carrier mobility which would be useful as

6
an alternative to organic HTLs. The electrochemical deposition of TiS2 thin films
holds significant promises owing to its facile, versatile, scalable, and low-cost
potential. The electrodeposition of thin films of semiconductors has mostly been
conducted in either aqueous or organic electrolyte medium that often has concerns
such as corrosion, oxidation, toxicity, and high cost. The as-deposited films exhibited
highly crystalline structure formed with preferred crystallographic orientation
confirming film growth predominantly in the hexagonal (2H) TiS2 phase (Asif et al.,
2020).

2.1.4 TiS2/TiSe2 Heterostructure

The idea that an ordered stacking of two-dimensional (2D) materials leads to
exotic electronic properties has been around since the discovery of graphene. Stacked
heterostructures with different transition metal dichalcogenides (TMDs) have long-
lived inter-layer excitons, resulting in spatially separated electrons and holes an ideal
feature for photovoltaic applications. The resulting band gap energies for all
semiconducting heterostructures are smaller than the average and the individual band
gaps of their bulk counter parts, whereas the TiS2/TiSe2 heterostructure becomes
semiconducting. The trigonal heterostructure phonon modes are more strongly
hybridized than the hexagonal ones (including some optical modes as well), visible
in the more numerous mixed magenta bands. Bulk TiS2 and TiSe2 are challenging to
simulate because they present a charge-density wave (CDW), leading to a phonon
instability that is very sensitive to unit-cell volume, pseudopotential, and strain. For
TiS2/TiSe2, find that stacking dynamically stabilizes the system of the heterostructure
stays metallic, but here are no unstable phonon modes (Pike et al., 2020).

2.1.5 Molecular Beam Epitaxy

In recent years, the fabrication of large-area, high-quality epilayers of various
TMDCs using molecular beam epitaxy (MBE) has gained considerable attention in
scientific research. The ultra-high vacuum environment of MBE is pivotal for
achieving precise control over the composition, thickness, and structural phases of
7
 TMDCs. This precise control facilitates exploration in new physics, technological
applications, and fundamental sciences. MBE application in creating epitaxial
TMDC films dates back two decades with pioneering work in this field involving the
growth of epitaxial NbSe2 and MoSe2 thin films on cleaved 2H MoS2 surfaces.
Additionally, recent advancements in the synthesis and processing of TMDC thin-
film monolayers have shown significant improvement, offering enhanced
controllability and reliability. Despite, the fact that MBE typically produces small
grain sizes (<200 nm) for TMDCs (Lin et al., 2021).

2.1.6 Scanning Tunneling Microscopy

Scanning Tunneling Microscopy (STM) with a functionalized tip apex
reveals the geometric and electronic structures of a sample within the same
experiment. As the basis of SPM methods, scanning tunneling microscopy (STM)
have been widely utilized in the characterization of various systems, such as
biological samples, hybrid inorganic−organic interfaces, and individual steps of on-
surface reactions. STM have good resolution is considered to be 0.1 nm lateral
resolution and 0.01 nm depth resolution through which individual atoms within
materials can be routinely imaged and manipulated. STM provides a probe for the
morphology and electrical properties at atomic resolution in all three dimensions The
process of scanning tunneling microscopy is based on the concept of quantum
tunneling. In this technique a fine probe tip is scanned over the conducting surface
of the material to be examined with the help of a piezoelectric crystal at a distance of
0.5–1 nm and the resulting current or the position of the tip required to maintain a
constant tunneling current is monitored (Kurki et al., 2024).

2.2 Hypothesis Formulation

One of the most nascent and universally accepted categories among the 2D materials
is the transition metal dichalcogenides (TMDCs). The absence of bandgap in graphene
8
fomented the researchers to quest for an alternative semiconducting 2D materials. The
aberrant optical and electronic properties helped 2D TMDCs to excel in fundamental
research and novel device applications. Graphene has gained global interest over the years
owing to its two-dimensional (2D) layered structure and exceptional properties like high
transparency (97.7% transmittance in the visible spectrum), thermal conductivity at room
temperature (3 ×103 W/mK), elevated electrical conductivity (~ 104 W-1 cm-1), large Young’s
modulus (1.1 TPa), and a high specific surface area (2630 m2/g). These properties ensure
excellent applications in energy storage (mainly batteries and ultracapacitors), solar cells,
transparent electrodes, aerospace, composites, biomedical, catalysis, and hydrogen evolution
reaction (Choudhury et al., 2020).
The hypothesize that high-quality TiS2 thin films synthesized using Molecular Beam
Epitaxy (MBE) will exhibit well-defined Charge Density Wave (CDW) phenomena and
unique electronic properties, which can be characterized at the atomic level using Scanning
Tunneling Microscopy (STM). This hypothesis is based on the premise that MBE allows for
precise control over the growth parameters, resulting in highly crystalline thin films with
minimal defects, thereby facilitating the observation of intrinsic CDW characteristics.
Furthermore, we hypothesize that the formation of TiS2/TiSe2 heterostructures via MBE will
result in modified interfacial properties that significantly influence the stability and
characteristics of CDW, as well as the overall electronic behaviour of the material. The
heterostructures are expected to exhibit unique interlayer interactions that can enhance or
suppress CDW phenomena depending on the specific stacking order and interface quality.
Additionally, we hypothesize that doping TiS2 with various elements and varying the
layer stacking in TiS2/TiSe2 heterostructures will lead to significant changes in their
electronic properties and CDW behaviour. The introduction of dopants is expected to alter
the electronic density of states and create new active sites, potentially enhancing the
material’s catalytic activity. Similarly, varying the layer stacking is anticipated to affect the
interlayer coupling and, consequently, the CDW stability and electronic properties. These
changes can be systematically analyzed using STM, which provides atomic-level resolution
of surface morphology, and electronic structure. Through this detailed investigation, we aim
to establish a comprehensive understanding of the relationships between synthesis
9
conditions, structural characteristics, and electronic properties in these 2D transition metal
dichalcogenides.

10
 CHAPTER 3
RESEARCH METHODS

3.1 Materials
The material that using in this research methods were sulfur guns, titanium powder,
selenium powder, HOPG sample, aluminium foil, IPA, and acetone. Liquid nitrogen was
used for Low Temperature Scanning Tunneling Microscopy (LTSTM). And Nitrogen air was
used for the suitcase.

3.2 Equipment
The equipment that using in this research methods were sample plate, tantalum foil,
spot welding gun, plastic point tweezers, ultrasonicator were used for preparation of the
MBE sample. K-type thermocouple, microprocessor thermometer, Sulfur gun with filament,
Titanium gun with filament, regulated power supply, and MBE instrument were used for
MBE process. Stainless Tube, Tungsten wire, beakers, tip holder, suitcase, gasket, and a
multimeter were used for STM preparation. Softwares of XPMPro2 SPM was used for
LTSTM imaging.

3.3 Procedures
3.3.1 Preparation of STM Tip Etching
The process for preparing and etching STM tips begins with wearing gloves
and regularly cleaning them with IPA or methanol. All beakers and tweezers must be
thoroughly cleaned. The Tungsten wire is straightened using sandpaper, and a fresh
piece is cut, with the polished side made flat to prevent cracks from spreading. The
Tungsten wire is then crimped into a steel tube, ensuring that the exposed part is
symmetrical and untouched on both sides. The tip holder is attached to the etching
holder, and the tip-SS tube is positioned correctly for spot welding in three to four
areas, with the energy set to 7.0. It is crucial to ensure that the tip and the ground of
the tip holder do not touch, verified using a multi-meter. The length for surface and
the tip max for the 5 mm.
11
 a) b)
Figure 3. (a) cracked polished tungsten wire (b) normal polished tungsten
wire

Figure 4. Ideal STM Tip before Tip Etching Process

Next, the tip holder is mounted on the etching holder, being careful not to damage
the tip, and the W wire is dipped into the etching solution with the Platinum wire
half-immersed. The power supply connected with the Pt wire negatively biased and
the W wire positively biased, adjusting the DC voltage to 7.5 mV and 1.2 mA.

Figure 5. Tip Etching Set

The power supply is turned on and off immediately when the current starts
reducing. When there is a sudden drop in current, the W wire is removed, cleaned in
Distilled water, and the tip is inspected under a microscope to ensure it is properly
shaped. Throughout the process, the preparation and etching of three tips were
conducted, with one done collaboratively and two independently.

12
a) b) c)
Figure 6. (a) good tip ; (b) bad tip, not sharp ; (c) bad tip, too long

The good tip should be store for some time. The tip was inserted into a
plastic tube, which was then placed inside a bell jar connected to a vacuum pump.
After activating the pressure panel to display the pressure inside both the bell
jar and the pump pipe, the valve was briefly opened and closed to introduce a
controlled amount of air. This process was repeated, and the O-ring seal was
carefully detached and then reattached to ensure that the introduction of air into the
system was gradual. Once the O-ring valve was securely reattached, the bell jar
was ready to get opened. The plastic tube containing the tip was placed inside the
bell jar, which was then sealed by adjusting and pressing the rubber seal under the
jar’s glass to ensure a tight fit. Subsequently, the vacuum pump was activated, and
the bell jar was gently tapped and adjusted to help achieve a complete seal. The
pressure was monitored until it reached zero. Upon completion of the process, the
valve was closed, and the pump was turned off.

Figure 7. Bell Jar and Vacuum Pump

13
3.3.2 Mounting the HOPG Sample into Sample Plate
The preparation and mounting of Highly Oriented Pyrolytic
Graphite (HOPG) onto a sample plate involve several meticulous steps to
ensure a clean and stable sample for analysis. First, the sample plate must
be thoroughly cleaned with isopropanol or acetone, rinsed with deionized
water, and dried with nitrogen to remove contaminants.

a) b)
Figure 8. (a) uncleaved sample plate (b) cleaved sample
The HOPG sample is then prepared by cleaving it with adhesive tape
to expose a fresh surface, handling it with clean tweezers to avoid
contamination. The HOPG is mounted using a small piece of tantalum foil
and conductive adhesive, ensuring the cleaved surface faces up and is
properly aligned. The adhesive is allowed to dry or cure according to the
manufacturer’s instructions to ensure stability.

a) b)
Figure 9. a) wielding process b) The welding % energy required
A final inspection using an optical microscope is conducted to
confirm the surface is clean and free from debris. If necessary, additional
cleaving and cleaning are performed until a smooth, defect-free surface is
achieved, ready for high-quality analysis.

14
 Figure 10. Cleaved HOPG under Microscope

3.3.3 Growth Process using Molecular Beam Epitaxy

The growth processes of TiS2 thin films and TiS2/TiSe2
heterostructures were meticulously carried out using Molecular Beam
Epitaxy (MBE). The initial setup involved annealing the Highly Oriented
Pyrolytic Graphite (HOPG) substrate to ensure cleanliness and readiness for
growth. For the TiS2 (0.6 ML) on TiSe2 (0.8 ML) heterostructure, annealing
was performed at a current of 1.15 A and 7.0 V, under high voltage settings
of 750 V at 6 mA, achieving a vacuum pressure of 1 x 10⁻⁹ Torr. Selenium
source preparation involved heating to 150°C, stabilized at 2.20 V and 2.18
A. The growth phase maintained the substrate at 300°C, with the sulfur
filament heated to 195°C and operating under specific voltage and current
settings to ensure stable sulfur vapor pressure. The layer growth sequence
began with a 10-minute deposition of TiSe2 (0.8 ML), followed by a 12-
minute deposition of TiS2 (0.6 ML), carefully monitored and adjusted to
maintain optimal conditions with a vacuum pressure of 6 x 10⁻¹⁰ Torr.
For the growth of TiS2 (1.3 ML), the process also began with
annealing the HOPG substrate, using a current of 1.15 A at 7.05 V, under
high voltage settings of 800 V at 6 mA, achieving a vacuum pressure of 7 x
10⁻⁹ Torr. Post-annealing, the pressure improved to 1.7 x 10⁻⁹ Torr,
indicating high cleanliness. The growth phase involved setting the substrate
temperature to 280°C, with current and voltage settings of 0.90 A and 5.02
V. The sulfur filament was heated to 195°C, operating under specific

15
conditions to ensure a consistent sulfur supply. Titanium deposition was
carefully controlled with the source set at 0.5 mA, under voltage settings
below 6 A and 2 kV. Sulfur source management maintained a vapor pressure
of 1.2 x 10⁻⁸ Torr, ensuring proper stoichiometry and layer quality. The TiS2
(1.3 ML) growth was completed over 26 minutes, with continuous
monitoring and adjustments to maintain optimal conditions, ensuring
uniform and high-quality deposition.

3.3.4 Scanning Tunneling Microscopy Imaging and Analysis

Scanning Tunneling Microscopy (STM) imaging and analysis is a
vital technique for characterizing samples grown using Molecular Beam
Epitaxy (MBE). This method provides atomic-scale resolution, crucial for
understanding the surface structures of thin films and heterostructures. For
samples grown in MBE, STM imaging starts with careful sample
preparation, including cleaving and annealing to ensure a clean surface. The
sample is then placed in the STM chamber under ultra-high vacuum
conditions. STM works by scanning a sharp metal tip close to the sample
surface, with a bias voltage applied between the tip and the sample. This
causes electrons to tunnel through the vacuum gap, with the tunneling
current providing topographical information.

Figure 11. Area Scan Panel in LT STM

During STM imaging, the tip height is adjusted to maintain a
constant current, generating detailed images of the surface. This reveals

16
atomic steps, defects, and atom arrangements, essential for assessing layer
quality and identifying structural imperfections. Additionally, by varying
the bias voltage and recording the tunneling current, STM can measure the
local density of states, providing insights into the electronic properties of
the material. Analysis of STM data involves interpreting topographical
images and electronic measurements to understand the material’s properties.
For TiS2 and TiSe2 heterostructures grown in MBE, STM can reveal
stacking order, interface quality, and electronic interactions. This detailed
analysis is crucial for optimizing growth parameters and improving material
quality. The Scanning Tunneling Microscopy (STM) analysis of the sample
provided by your collaborators in France that from my analysis.

Figure 12. dI/dV Reference

17
 CHAPTER 4
RESULT AND DISCUSSION

4.1 Result
4.1.1 TiS2 Thin Film Imaging through LT STM
TiS2 thin film was produced with Molecular Beam Epitaxy (MBE)
with the Ti flux was set at 1nA. The obtained TiS2 was produced at 1.3
monolayer. The TiS2 Thin Film was analyzed using LT STM that operated
with a Tungsten tip at 78K.

Figure 13. TiS2 Thin Films analyzed through LT STM

4.1.2 TiS2/TiSe2 Heterostructure Imaging through LT STM

TiS2/TiSe2 heterostructure was produced with Molecular Beam
Epitaxy (MBE) with the Ti flux was set at 1nA. The obtained TiS2 (0.6
monolayer) on TiSe2 (0.8 monolayer) was produced after this process. The
heterostructure was obtained when the Selenium source preparation
involved heating to 150°C and the Sulfur source preparation involved
heating to 195°C.

Figure 14. TiS2/TiSe2 Heterostructure analyzed through LT STM

18
 4.1.3 Charge Density Wave of TiS2 from the Fourier Transform
TiS2 1.3 monolayer using Scanning Tunneling Microscopy (STM)
and Fourier Transform (FT) techniques to identify and characterize the
Charge Density Wave (CDW) phenomena within the material. CDWs are
periodic modulations of the electronic charge density that occur due to
strong electron-phonon interactions, and they play a crucial role in
determining the electronic properties of materials.

Figure 15. TiS2 Thin Film analyzed form Fourier Transform

4.1.4 Charge Density Wave of TiS2/TiSe2 Heterostructure from the

Fourier Transform
TiS2 (0.6 monolayer) on TiSe2 (0.8 monolayer) using Scanning
Tunneling Microscopy (STM) and Fourier Transform (FT) techniques to
identify and characterize the Charge Density Wave (CDW) phenomena
within the material. CDWs are periodic modulations of the electronic charge
density that occur due to strong electron-phonon interactions.

Figure 16. TiS2/TiSe2 Heterostructure analyzed form Fourier Transform

19
4.2 Discussion
4.2.1 Analysis of TiS2 Thin Film and TiS2/TiSe2 Heterostructure
The STM image analysis of TiS₂ thin films reveals a well-ordered
lattice structure with a lattice constant of approximately 4.8 Å. This value is
slightly larger than the lattice constant reported for bulk TiS₂, which could
be due to strain effects or the thin film synthesis process. The high-
resolution imaging confirms the crystalline quality of the thin films, with
minimal defects and uniform atomic distribution. The comparison with the
findings of Fang et al., (1997) supports the reliability of our measurements
and the structural integrity of the TiS₂ thin films. The slight increase in
lattice constant might be attributed to the thin film's unique environment,
where strain and surface effects can play a significant role. These findings
are crucial for understanding the material’s properties and potential
applications in nanoelectronics and optoelectronic devices.

a) b)
Figure 17. Hexagonal Structure of (a) TiS2 thin film and (b)
Heterostructure
The STM image from our research reveals a well-ordered atomic
arrangement with a lattice constant of approximately 4.2 Å for the
TiS₂/TiSe₂ heterostructure. This finding aligns with the minimal lattice
mismatch reported by Duong et al., (2017), which is essential for forming
stable heterostructures. The close match in lattice constants between TiS₂
(approximately 3.40 Å) and TiSe₂ (approximately 3.54 Å) supports the
observed stability and periodicity in our STM image. The consistency
between our experimental results and the literature underscores the
reliability of our methods and the structural integrity of the TiS₂/TiSe₂
heterostructure. The minimal lattice mismatch facilitates the seamless

20
stacking of layers, preserving the unique properties of each constituent
material. This structural integrity is crucial for potential applications in
nanoelectronics and optoelectronic devices, where maintaining the distinct
electronic characteristics of each layer is necessary for device performance.

4.2.2 Defect Analysis in TiS2 Thin Film and TiS2/TiSe2 Heterostructure

The surface morphology and defects are highlighted in the STM
images provided. In image (a), a top-view STM, the 2D image offers a
detailed view of the surface morphology at the atomic level, revealing a
regular lattice structure indicative of a well-ordered crystalline surface.
However, several darker spots and irregularities are visible, likely
corresponding to vacancies, which are missing atoms, or adsorbed
impurities on the surface. These imperfections can significantly influence
the electronic properties of the material. Image (b), the 3D STM
visualization, provides a clearer depiction of the surface topography,
showcasing an undulating pattern that suggests the presence of step edges
and terraces, common features in layered materials such as TiS₂/TiSe₂
heterostructure. The protrusions and depressions observed in this 3D
visualization correspond to atomic-scale defects, including vacancies and
interstitials. These defects can alter the material’s electronic and structural
properties by introducing localized states and scattering centers, thereby
affecting its overall performance in electronic and optoelectronic
applications.

a) b)
Figure 18. Defect Analysis for (a) 2D and (b) 3D Visualization of
the TiS₂/TiSe₂ Heterostructure

21
 Meanwhile this 2D of the TiS₂ thin film at the atomic level, revealing
a well-ordered crystalline surface characterized by a regular lattice
structure. However, several darker spots and irregularities are visible, likely
corresponding to vacancies where Ti or S atoms are missing, or to adsorbed
impurities on the surface. Such defects disrupt electronic uniformity and
create localized states within the bandgap, affecting the film’s overall
electronic properties. The 3D STM visualization offers a comprehensive
view of the surface topography of the TiS₂ thin film. The undulating pattern
indicates the presence of step edges and terraces, typical features in layered
materials like TiS₂. The observed protrusions and depressions correspond to
atomic-scale defects such as vacancies or interstitials. These defects
significantly impact the film's structural integrity and electronic behavior,
as step edges and terraces scatter charge carriers, while vacancies and
interstitials introduce trap states, influencing the film's conductivity and
carrier mobility.

a) b)
Figure 19. Defect Analysis for (a) 2D and (b) 3D Visualization of
the TiS₂ Thin Film

4.2.3 CDW Phenomena between TiS2 Thin Film and TiS2/TiSe2

Heterostructure from the FT Technique
4.2.3.1 TiS2/TiSe2 Heterostructure
The PSD vs. frequency plot shows a significant peak at low spatial
frequencies (around 0.1 Å⁻¹), indicating strong periodic modulations in the
charge density characteristic of the CDW in the TiS₂/TiSe₂ heterostructure.
This prominent peak, along with the sharp decline in PSD values beyond it,
suggests that the CDW is defined by long-wavelength modulations with

22
minimal high-frequency disturbances. Additionally, the log-log PSD plot
reveals a linear decay, indicative of scale-invariant features and fractal-like
behavior in the CDW, implying self-similar patterns across different length
scales.

a) b)
Figure 20. (a) Log. Scales and (b) Linear scales of PSD Curve
The low-frequency peak in the PSD plot indicates a stable CDW
with well-defined periodicity, essential for understanding the electronic
structure of the heterostructure. The amplitude of this peak reflects the
strength of charge density modulations; a higher amplitude signifies a more
pronounced CDW, which can influence the electronic band structure and
potentially open gaps at the Fermi surface. The sharp decline in PSD values
at higher frequencies suggests a stable CDW, free from high-frequency
disturbances, which is crucial for maintaining consistent electronic
properties and reducing scattering events. The linear decay in the log-log
PSD plot further suggests the CDW’s fractal nature, enhancing its stability
and resilience against external perturbations.

Figure 21. TiS2/TiSe2 Heterostructure analyzed form Fourier Transform

23
The significant peaks near -2 to 0 1/nm in the PSD plot indicate strong
periodic modulations in the charge density, characteristic of a well-formed
Charge Density Wave (CDW). These high amplitude peaks highlight the
robustness and stability of the CDW within the TiS₂/TiSe₂ heterostructure.
Additionally, the relatively low amplitude in the region from -16 to -3 1/nm
suggests minimal background noise, reinforcing the presence of a well-
defined CDW signal. This low noise level indicates that the observed CDW
is not significantly disrupted by extraneous factors, ensuring a clear and
distinct modulation pattern.
The PSD analysis from the FT results highlights the stability and
properties of the CDW in the TiS₂/TiSe₂ heterostructure. The prominent
low-frequency peak and the linear decay in the log-log plot indicate a stable,
well-defined CDW with fractal-like behavior. These characteristics suggest
that the CDW in this heterostructure is robust and significantly influences
the electronic properties, enhancing the material’s potential for advanced
electronic applications. Understanding these correlations is essential for
optimizing the heterostructure’s performance and tailoring its properties for
specific uses.
4.2.3.2 TiS2 Thin Film
The FT plot of TiS₂ thin films reveals significant peaks at low
frequencies (0 to 2 1/nm), indicating strong periodic modulations in the
charge density characteristic of a well-formed Charge Density Wave
(CDW). The highest amplitude peak near 1 1/nm suggests a dominant
periodicity in the CDW, corresponding to the real-space wavelength of the
charge density modulation. Additionally, the relatively low amplitude
beyond 2 1/nm indicates minimal background noise, reinforcing the
presence of a well-defined CDW signal with smooth FT amplitude decline
at higher frequencies, suggesting a CDW characterized mainly by low-
frequency components with minimal high-frequency disturbances.

24
 Figure 22. TiS2 Thin Film analyzed form Fourier Transform
The PSD vs. frequency plot further confirms these findings with a
prominent peak at low frequencies (around 0.1 Å⁻¹), reflecting strong
periodic modulations in the charge density. The rapid decline in PSD values
beyond this peak suggests that the CDW is characterized by long-
wavelength modulations, with minimal high-frequency noise. The log-log
PSD plot shows a linear decay, indicating scale-invariant features and
fractal-like behavior in the CDW, with self-similar patterns across different
length scales.

a) b)
Figure 23. (a) Log. Scales and (b) Linear scales of PSD Curve
These analyses highlight that the CDW in TiS₂ thin films is stable
and well-defined, with significant low-frequency peaks and minimal high-
frequency noise. The high amplitude of the low-frequency peaks suggests
strong charge density modulations, which stabilize the CDW and enhance
electron mobility and overall material conductivity by reducing electronic
scattering. The fractal nature of the CDW, as indicated by the linear decay
in the log-log PSD plot, suggests robustness and resilience against external

25
perturbations, making TiS₂ thin films promising for advanced electronic
applications.

4.2.4 Doping Effect of CDW between TiS2 Thin Film and TiS2/TiSe2
Heterostructure
Doping significantly impacts the Charge Density Wave (CDW)
stability and properties in TiS₂ thin films and TiS₂/TiSe₂ heterostructures. In
TiS₂ thin films, doping can introduce localized impurity states that either
stabilize the CDW by pinning it or disrupt it, depending on the type and
concentration of dopants. In TiS₂/TiSe₂ heterostructures, doping can modify
interlayer interactions, enhancing or destabilizing the CDW. By altering
carrier concentration and introducing lattice strain, doping affects electronic
properties, potentially shifting the Fermi level and modifying the CDW gap.
Overall, controlled doping can optimize the material’s electronic and
structural characteristics for advanced applications.

4.2.5 Catalytic Potential of TiS2 Thin Film and TiS2/TiSe2

Heterostructure
The TiS₂ thin film and TiS₂/TiSe₂ heterostructure exhibit significant
catalytic potential due to their unique electronic and structural properties.
TiS₂ thin films offer high surface area and active sites, enhancing catalytic
reactions such as hydrogen evolution. The heterostructure of TiS₂/TiSe₂ can
further improve catalytic efficiency by providing synergistic effects between
the layers, optimizing charge transfer, and reducing energy barriers. These
materials tunable properties through doping and structural
modifications make them promising candidates for various catalytic
applications, including energy conversion and environmental remediation.

26
 CHAPTER 5
OBSTACLES AND FUTURE WORK

5.1 Obstacles
Conducting research on the growth and atom-resolved studies of TiS2 thin
films and TiS2/TiSe2 heterostructures using MBE and STM involves several
obstacles. Precise control over MBE growth parameters and ensuring high-quality
interfaces in heterostructures are challenging, as small variations can significantly
impact crystal quality and electronic properties. Achieving atomic resolution with
STM requires ultra-clean surfaces and stable conditions, necessitating meticulous
sample preparation. Consistently reproducing doped samples and accurately
characterizing CDW phenomena under varying conditions further complicate the
research. While advanced tools like RHEED, XPS, SIMS, and ARPES can help,
they require specialized knowledge, high costs, and complex setups, highlighting
the balance between technological capabilities and practical constraints.

5.2 Future Work

The exploration of ultrathin TMD films holds significant promise for future
advancements in nanoscience, particularly in the realm of high-specific-power solar
cell applications. These films are characterized by their high optical absorption
capabilities, optimal band gaps, and self-passivated surfaces. Such features not only
enhance the efficiency of solar cells but also align with the goals of sustainable
material usage and cost-effectiveness. Additionally, the inherent chemical and
mechanical stability of TMDs ensures reliability and longevity comparable to
traditional silicon solar panels. This stability coupled with their biocompatibility
opens new avenues for their use in wearable and implantable electronics. The
ongoing advancements in nanoelectronics, especially in TMD growth and device
fabrication are paving the way for cost-effective mass production. These
developments echo the early stages of silicon solar cell production, where
microelectronics advancements played a crucial role. The ongoing research
suggests that with further optimization, TMD solar cells could revolutionize solar

27
cell technology particularly for high-specific-power applications in emerging
technologies (Dallaev et al., 2023)

28
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