Advanced Materials - 2023 - Li - Substrate Engineering For Chemical Vapor Deposition Growth of Large Scale 2D Transition

REVIEW
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Substrate Engineering for Chemical Vapor Deposition

Growth of Large-Scale 2D Transition Metal Dichalcogenides
Shaohua Li, Decai Ouyang, Na Zhang, Yi Zhang, Akshay Murthy, Yuan Li,* Shiyuan Liu,*
and Tianyou Zhai*
1. Introduction
The large-scale production of 2D transition metal dichalcogenides (TMDs) is
essential to realize their industrial applications. Chemical vapor deposition In the past few years, 2D TMDs have
been widely studied for electronics and
(CVD) has been considered as a promising method for the controlled growth
optoelectronics owing to their attractive
of high-quality and large-scale 2D TMDs. During a CVD process, the substrate intrinsic optical properties, superior me-
plays a crucial role in anchoring the source materials, promoting the chanical flexibility, relative ease of stacking
nucleation and stimulating the epitaxial growth. It thus significantly affects for creating various heterostructures, and
the thickness, microstructure, and crystal quality of the products, which are high compatibility with current nanofabri-
particularly important for obtaining 2D TMDs with expected morphology and cation platforms.[1–5] The mature growth of
large-scale and high-quality 2D TMDs has
size. Here, an insightful review is provided by focusing on the recent
been realized to be of great significance for
development associated with the substrate engineering strategies for CVD their future practical device integration.[6–8]
preparation of large-scale 2D TMDs. First, the interaction between 2D TMDs Currently, CVD is considered to be a
and substrates, a key factor for the growth of high-quality materials, is promising approach for the production
systematically discussed by combining the latest theoretical calculations. of industrial-level TMDs.[9–11] In a typical
CVD synthesis process, the substrate plays
Based on this, the effect of various substrate engineering approaches on the
a crucial role in anchoring the source
growth of large-area 2D TMDs is summarized in detail. Finally, the materials, promoting the nucleation, and
opportunities and challenges of substrate engineering for the future stimulating the epitaxial growth,[12–14] and
development of 2D TMDs are discussed. This review might provide deep thus building a close relationship between
insight into the controllable growth of high-quality 2D TMDs toward their the substrate and the final morphology of
industrial-scale practical applications. products such as nucleation density, nucle-
ation sizes, and epitaxial orientation.[15,16]
As a result, substrate engineering
has been widely used as an essential
strategy for the controlled growth of ideal 2D TMDs with various
S. Li, D. Ouyang, N. Zhang, Y. Zhang, Y. Li, T. Zhai
microstructures.
State Key Laboratory of Materials Processing and Die & Mould
Technology Toward the preparation of large-scale 2D TMDs, considerable
School of Materials Science and Engineering efforts have been made on different substrates to achieve con-
Huazhong University of Science and Technology trollable thickness, microstructure, and high crystal quality of the
Wuhan 430074, P. R. China products,[17–21] the key technological nodes of which are displayed
E-mail: yuanli1@hust.edu.cn; zhaity@hust.edu.cn
in Figure 1 to illustrate the evolution of substrate engineering in
A. Murthy
Superconducting Quantum Materials and Systems Division recent years. Initially, the growth was carried out on various pris-
Fermi National Accelerator Laboratory (FNAL) tine substrates to explore the vital mechanism of epitaxial growth
Batavia, IL 60510, USA and meet the demand of possible industrial applications.[22–26]
Y. Li, T. Zhai For example, the dangling-bond-free and atomically flat surface
Shenzhen Huazhong University of Science and Technology Research of mica substrates highly promotes the lateral growth by van
Institute
der Waals epitaxy,[27] and the convenient large-scale growth on
Shenzhen 518057, P. R. China
SiO2 /Si substrates facilitates subsequent nanopatterning and in-
S. Liu
State Key Laboratory of Digital Manufacturing Equipment and Technology tegration, demonstrating high compatibility with the comple-
School of Mechanical Science and Engineering mentary metal-oxide-semiconductor (CMOS) techniques. More-
Huazhong University of Science and Technology over, the matched lattice symmetry with 2D TMDs of sapphire
Wuhan 430074, P. R. China substrates makes the domains usually exhibit two opposite ori-
E-mail: shyliu@hust.edu.cn
entations to form highly oriented large-scale films. To improve
The ORCID identification number(s) for the author(s) of this article the crystal quality (e.g., the higher degree of single crystallinity)
can be found under https://doi.org/10.1002/adma.202211855 based on large-scale preparation, the nucleation density[28] and
DOI: 10.1002/adma.202211855 domain orientations[29] constitute crucial factors that determine
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Figure 1. A historical overview of the major experimental progress for the CVD growth of 2D TMDs via substrate engineering. Reproduced with
permission.[25,45,175,176] Copyright 2012, 2017, 2018, 2019, American Chemical Society. Reproduced with permission.[27,74,129,154,186] Copyright 2015,
2022, 2021, 2017, 2022, Wiley-VCH. Reproduced with permission.[26,30,31,73] Copyright 2015, 2021, 2022, 2022, Springer Nature.
the growth process. In 2021, the stepping engineering of sap- Then based on those theories and fundamental fundings, we
phire substrates represented a huge milestone in fabricating discuss the effect of different substrate engineering approaches
large-scale single-crystal 2D TMD films as wafer-scale ones were including surface-stepped substrates, chemically-functionalized
successfully synthesized.[30] The resultant stepped surface breaks substrates, curved substrates, substrate seeding strategies and
the 6-fold symmetry of sapphire and guides the unidirectional other substrate modification methods on the CVD growth of var-
alignment of 2D TMDs, eliminating the problem of grain bound- ious large-area 2D TMDs. Finally, we put forward the challenges
aries generated by random antiparallel domains.[30] In particu- and opportunities of substrate engineering toward the mature
lar, precise layer control has been reached by adjusting the step production and practical application of 2D TMDs. This review
height of the stepped c-sapphire.[31] Overall, such substrate engi- will help guide future theoretical understanding of the growth
neering strategies reflect the great significance of lattice symme- mechanisms and experimental design for large-scale synthesis
try matching design in crystalline quality improvement of large- of various 2D TMDs.
scale 2D TMDs, which will satisfy the device consistency require-
ment of industrial integration. 2. Interaction with Substrates upon the TMD
Up to now, substrate engineering has made significant ad- Growth
vances in achieving large-scale, consistently oriented growth and
nanopatterned arrays of 2D TMDs.[32–36] This review article is fo- Understanding the interaction with substrates upon the TMD
cused explicitly on the application of substrate engineering for growth is essential for achieving high-quality epitaxial growth.
the growth of large-area 2D TMDs in the past few years. First, we Therefore, it is crucial to have a comprehensive understand-
demonstrate the interactions between 2D TMDs and substrates ing of the physicochemical properties of the substrates that di-
with theoretical computational simulations. Second, we summa- rectly influence the growth of 2D TMDs. Figure 2 shows the
rize the typical researches of large-scale TMDs growth on pristine growth model of TMDs on several regularly used substrates
substrates such as SiO2 /Si, Mica, Au, and sapphire substrates. (e.g., SiO2 /Si, mica, metal, and sapphire). Due to the amorphous
Figure 2. The interactions of 2D TMDs with commonly used substrates. a) SiO2 /Si; b) Mica; c) Nobel metal (Au); d) Sapphire.
surface of the SiO2 /Si substrates, the domains of TMD on this will develop into a large-scale single crystal over growth time.
substrate usually show random orientation and then form un- However, getting a single nucleation in a CVD process can be
controllable grain boundaries[37–39] (Figure 2a). Thanks to the challenging.[28,56,57] Currently, most methods of preparing large-
absence of dangling bonds (Figure 2b), mica substrates can scale 2D TMD thin films are composed of nucleation and crys-
promote the transverse diffusion of atoms[40] and benefit the tal domain stitching with growth. There are usually many nu-
growth of unstable materials. The Au and c-plane sapphire sub- cleation sites on the substrates.[58] If the nucleation sites have
strates have well-matched lattice symmetry with TMDs, making the same orientation, millions of unidirectional domains of 2D
them more suitable for the growth of wafer-scale single-crystal TMDs grown on the substrate can be seamlessly stitched together
TMDs.[30,41] The chemical interaction between the edge TMD into a single crystal (Figure 3b).[59,60] On the contrary, the do-
atoms and the Au substrates is much stronger than the intralayer mains with different orientations stitch together to form large-
van der Waals interaction,[42,43] and thus the orientation of the nu- scale polycrystalline films (Figure 3c). The uncontrollable grain
cleation is determined by the edge interaction (Figure 2c). The top boundary formation and limited grain size can significantly re-
layer atoms of sapphire have a 6-fold symmetry, which is prefer- duce their performance and uniformity, and seriously hinder
ential for the generation of antiparallel domains[44,45] and benefi- their practical applications in high-performance devices.[61] The
cial for preparing highly-oriented TMDs (Figure 2d). Accordingly, oriented domains require a single crystal substrate and align-
selecting suitable substrates may be an effective way to achieve ment registry between 2D TMDs and the substrate, which can
the growth of wafer-scale single-crystal 2D TMDs and even ex- effectively avoid the formation of grain boundaries during the
tendable for other 2D materials. growth.[62]
In a typical CVD process, the nucleation density, size and do- As we know, the low nucleation barrier of 2D materials leads
main orientation of the obtained 2D TMDs are closely related to random nucleation on substrates, and thus the preparation
to the microstructure and pretreatment of the substrates.[46–48] of uniform patterned 2D TMDs arrays is still in challenge.[63]
It is known that the growth of large-scale single-crystal TMDs It is necessary to control the location and density of the
is necessary for the construction of high-performance optoelec- nucleation sites on the substrate for the large-scale periodic
tronic devices.[49–55] As schematically shown in Figure 3a–d, there arrays.[64,65] Through substrate engineering, the defects as seed-
are four methods for the growth of 2D TMDs with various mi- ings are placed in specific positions on substrates, and the
crostructures such as single crystal films, polycrystalline films nucleation of 2D TMDs in the CVD growth prefers to take
and nanopatterned arrays. The growth process of 2D TMDs on place on the high-energy defect surface.[66] By substrate seed-
substrates mainly includes nucleation and growth. For this, it is ing strategies, the nucleation of 2D TMDs is restricted to spe-
highly essential to control the nucleation orientation and density. cific sites, and then large-scale periodic arrays can be prepared
If there is only a single nucleation on substrates (Figure 3a), it (Figure 3d).
Figure 3. The strategies for the growth of large-scale 2D TMDs on various substrates. a) A single domain on the substrate and growing into a large area
single-crystal film; b) Millions of unidirectional domains and seamlessly stitching into a large-scale single-crystal film; c) Random domains on substrate
and stitching into a large area polycrystalline film; d) Site-specific growth of nanopatterned arrays.
In order to relate the effect of substrates and the interaction be- the bilayer MoS2 is more favorable to nucleate than the trilayer at
tween substrates and TMDs, many theoretical studies have been this step height. Further calculation indicates that the step with
conducted.[67–71] Dong et al.[71] indicate that the alignment of 2D a height of 2.20 nm is conducive to nucleation and growth of tri-
materials on the substrate depends on their symmetry and the layer MoS2 (Figure 4h). By controlling the step height, MoS2 films
symmetry of the substrate. And they present the various ways in with different thicknesses can be obtained, and the optimum step
which 2D materials with 3-fold and 6-fold symmetries are aligned height for the nucleation and growth of bilayer, trilayer and four-
on three low-index surfaces of an FCC crystal (Figure 4a). The layer 2D MoS2 is 1.30, 1.75, and 2.20 nm, respectively. Overall,
authors then conclude that the number of equivalent but dif- the layer-controlled epitaxial growth of 2D TMDs can be realized
ferent orientations of 2D materials on substrates can be calcu- by introducing proper step-edge interfacial interactions.[74] These
|G |
lated by N1 = |G sub | , where Gsub and G2D@sub are the number theoretical predictions have been widely used in TMDs growth to
2D@sub
of nonequivalent symmetry operations of the substrate and that understand their growth mechanism.[30,31,73]
of the system of the 2D material on the substrate. The Density
Functional Theory (DFT) calculation of binding energies of the 3. Growth on the Pristine Substrates
WS2 on the h-BN substrate indicates that the 0° and 60° domains
have the same formation energy, and the WS2 domains have two 3.1. SiO2 /Si Substrates
equivalent orientations on the h-BN surface (Figure 4b,c).[71] Ji
et al.[72] prepare large-area MoS2 by using a salt-assisted CVD As known, silicon substrates with wet-oxidized SiO2 surface lay-
method. The calculation of the formation energy shows that halo- ers are the most common substrate for various electronic and op-
gen atoms acting as passivation reduce the energy of formation of toelectronic devices including transistors, photodetectors, inte-
the reaction, but there are still two equivalent growth directions grated circuits, and so on. As a result, the SiO2 /Si substrates have
(Figure 4d). Figure 4e presents the distribution of charge differ- been preferentially used for the growth of many TMDs.[75–77] The
ence within MoS2 grown on vicinal a-sapphire, and the calcula- conventional CVD growth of TMDs on such SiO2 /Si substrates is
tion results show that the binding energy between the step edge usually conducted in a horizontal tube furnace as shown in Fig-
and WS2 depends on its alignment and the surface step breaks ure 5a.[78–80] However, the growth process can be affected by the
the C2 symmetry of the WS2 /a-plane sapphire system.[73] Those substrate position,[81] which can cause the random distribution of
facts suggest that obtaining unidirectional domains of 2D mate- materials on the substrate (Figure 5b). In addition, the solid pre-
rials on a low symmetry surface is more accessible. cursors have faster sublimation that may lead to excessive nucle-
Theoretically, 2D TMDs with controllable layer numbers can ation sites, so that the gaseous precursor can be controlled more
be obtained by the substrate engineering of creating steps with precisely and uniformly in the vapor deposition reaction. There-
different heights on c-plane sapphire.[74] And the (1010) ̄ oriented fore, Tang et al.[82] designed a vertical chemical vapor deposition
step on the sapphire c-plane is thought to guide the unidirec- (VCVD) system for the growth of monolayer TMDs to guarantee
tional nucleation of the MoS2 domains. Figures 4f,g show the a uniform and steady supply of gaseous H2 S precursors over the
model of bilayer and trilayer MoS2 near the step with a height of whole substrate (Figure 5c). By using this design, the H2 S can be
1.75 nm, and then the calculation of formation energy shows that controlled more precisely and uniformly on the same substrate.
Figure 4. The theoretical interactions between 2D materials and substrates. a) The schematic of the alignment of 2D materials with different symmetries
on various high-symmetry substrates. b) Cluster model of a WS2 domain on the h-BN surface. c) The binding energies of the WS2 on the h-BN surface
as a function of the alignment angle (𝜃). Reproduced with permission.[71] Copyright 2021, Springer Nature. d) Energy landscapes and intermediate
edge structures of MoS2 growth with (top) and without (bottom) halide. Reproduced with permission.[72] Copyright 2021, American Association for the
Advancement of Science (AAAS). e) Optimized structures of antiparallel WS2 ribbons crossing an atomic step of a-plane sapphire for 𝜃 = 0° (left) and 𝜃
= 60° (right). Reproduced with permission.[73] Copyright 2022, Springer Nature. f) Bilayer and g) Trilayer MoS2 near the step with a height of 1.75 nm.
h) Trilayer MoS2 near the step with a height of 2.20 nm. Reproduced with permission.[74] Copyright 2022, Wiley-VCH.
They realized the complete growth of WS2 films with good crys- using the Knudsen-type effusion cells. The size of the prepared
talline quality on the centimeter-scale SiO2 /Si substrates (Fig- TMDs can be adjusted between 10 and 200 μm. The prepared
ure 5d). Seol et al.[83] developed a pulsed metal-organic chemical TMDs possess high optical quality compatible with the mechan-
vapor deposition (MOCVD) for the high-throughput growth of ically exfoliated samples,[88] enabling their implementation in
WS2 on a 6-inch wafer-level SiO2 /Si substrate. The growth strat- electronic, photonic and optoelectronic devices. Chen et al.[76]
egy and process are schematically illustrated in Figure 5e,f. The reported that wafer-scale monolayer WS2 film can be grown di-
periodical injection of the precursor Mo(CO)6 drives vertical Ost- rectly on SiO2 /Si substrates by CVD and thermal evaporation ap-
wald ripening and inhibits the secondary nucleation (Figure 5e). proach. The wafer-scale WS2 film is used to make FET arrays, and
The specifically designed cold-wall MOCVD system (Figure 5f) its maximum mobility is nearly one order of magnitude higher
selectively heats the substrates and effectively reduces the chem- than currently reported devices based on CVD-grown TMDs. Li
ical side reactions in the gas phase under a high temperature. et al.[89] prepared ultrathin 2D VTe2 nanoplates with a thickness
By using this method, the contamination of the products is sig- of 3 nm through a CVD process. Then they fabricated a FET de-
nificantly inhibited, enabling the production of large-scale field- vice on the SiO2 /Si substrates to investigate the electronic prop-
effect transistor (FET) arrays that exhibit consistent electrical per- erties of VTe2 nanoplates and found that VTe2 nanoplates exhibit
formance and a high on/off ratio of 107 .[83] ferromagnetism properties. However, the amorphous structure
Since the SiO2 /Si substrates are promising for device fabrica- of SiO2 /Si substrates is mismatched with crystalline 2D TMDs,
tion, many studies have been conducted to control the growth which can’t serve as a catalyst for the nucleation and growth pro-
of TMDs on this conventional substrate specifically for practi- cesses. And thus, most TMD films grown on such amorphous
cal applications.[84–86] Recently, George et al.[87] prepared single- SiO2 surfaces are found to be polycrystalline with randomly
crystal TMD monolayers by controlling the S precursor flow rates oriented grains, which primarily influence the uniformity and
Figure 5. The growth of TMDs on SiO2 /Si and mica substrates. a, c) Schematics of typical HCVD and VCVD. b, d) Growth profiles of the two different
CVD systems. Reproduced with permission.[82] Copyright 2020, American Chemical Society. e) Schematic of the growth mechanism by pulsed MOCVD.
f) Schematic illustration of the reactor geometry (left) and injection sequence of precursors (right) for growing wafer-scale monolayer TMDs. Reproduced
with permission.[83] Copyright 2020, Wiley-VCH. g) Crystal structure of H-phase VS2 . h) Schematic illustration of the CVD synthesis process. i) Optical
image (OM) of H-phase VS2 with hexagonal morphology. j) Optical image of monolayer H-phase VS2 transferred from mica to SiO2 . Reproduced with
permission.[95] Copyright 2020, Wiley-VCH. k) The atomic model of CuSe crystal. l) AFM image with the thickness profile of a typical ultrathin CuSe
nanosheet. m) High-resolution TEM image and TEM-EDS mapping image of CuSe nanosheet. n) Current–Voltage (I–V) switching curves of a CuSe
memristor during 100 cycles. The inset is the structure schematic of the 2D CuSe memristor. Reproduced with permission.[96] Copyright 2022, Wiley-
VCH.
reproducibility of various devices and limit the further applica- SiO2 /Si substrates. The weak van der Waals interaction between
tion of the products.[85] precursor atoms and mica substrates promotes their lateral mi-
gration. As a result, the mica substrates are also preferentially
employed for the growth of 2D TMDs with poor chemical stabil-
3.2. Mica Substrates ity in ambient conditions.[94] For instance, H-phase VS2 is ther-
modynamically unstable (Figure 5g) and has been thought dif-
Mica substrates confer numerous advantages, such as a smooth ficult to be synthesized on the conventional SiO2 /Si substrates.
surface without dangling bonds, chemical inertness, superior Su et al.[95] reported the growth of 2D H-phase VS2 nanostruc-
transparency, and good thermal stability.[27,90] According to re- tures on mica substrates by applying a salt-assisted CVD method
ports, the grain size is significantly impacted by the different sub- (Figure 5h). The obtained VS2 reaches a lateral size as large as
strate types,[91–93] and Huang et al.[92] found that the grain sizes 250 μm (Figure 5i), because of the catalytic effect of the alkali
of SnSe2 on mica substrates are 6 times larger than those on metal that reduces the growth energy barrier significantly. Since
the van der Waals interaction between VS2 and mica substrate is scale monolayer SeMoS on Au (111) substrates through one-pot
weak, it is easy to transfer the as-synthesized material to any sub- CVD. Figure 6d shows the schematic illustration of the process
strate, such as SiO2 /Si substrate (Figure 5j). More recently, Yin for synthesizing ML Janus SeMoS. The Au surface can absorb
et al.[96] successfully synthesized layered CuSe nanoflakes using and catalytically dissociate the S clusters under 700 °C, and the
van der Waals epitaxy technique on mica substrates (Figure 5k) S atoms can move on the Au surface and exchange the Se atoms
and transferred the products onto SiO2 /Si substrates for the re- in the bottom layer of MoSe2 . The triangular crystal with a high
search of non-volatile memory behavior. The AFM image of CuSe density and uniform distribution can be found in the optical im-
(Figure 5l) shows that its thickness can be as thin as 2.4 nm. age (Figure 6e). The transferred SeMoS monolayers on SiO2 /Si
The TEM image along the [001] zone axis and TEM-EDS element substrates have an average thickness of 0.8±0.2 nm (Figure 6f).
mapping image (Figure 5m) indicate the perfect hexagonal lattice More importantly, the prepared monolayer SeMoS on Au (111)
fringes and high-quality single-crystal phases. On this basis, the substrates has a good optical quality with strong exciton-phonon
resultant memristor has a low switching voltage (≈0.4 V), supe- coupling and enables an exciton g-factor of -3.3.[107]
rior switching speed, high switching uniformity and stable per- In addition to this strategy, 2D TMDs can be obtained directly
formance (Figure 5n) due to the high activity of Cu ions, low mi- by vulcanizing the noble metal substrate. Yu et al.[113] developed
gration barrier, and good cycling performance.[96] a method to synthesize high-quality PtTe2 thin films, which can
Highly flexible insulating mica substrates allow the mass pro- be used for spin-orbit torque (SOT) devices. The thin Pt films are
duction of flexible devices without transferring processes.[97–99] first prepared on SiO2 /Si wafers by a magnetron sputtering sys-
For instance, Wang et al.[100] pasted PbI2 flakes synthesized on tem. Then the thin PtTe2 films are transformed from the Pt sub-
mica directly onto PET substrates, and found that the flexible strate by annealing the sources in tellurium vapor in a CVD fur-
PbI2 photodetector has good mechanical stability and excellent nace. A typical AFM image of the as-grown PtTe2 thin film reveals
optoelectronic response to 470 nm light. Tang et al.[101] designed that the root-means-square roughness is 0.4 nm. The overlaid Pt-
a confined micro-reactor to grow high-quality 2D In2 Se3 on mica Te atomic model in the HRTEM image displays a well matching
substrates with large domain sizes exceeding 200 μm. The flexi- between the ideal PtTe2 (001) pattern with the real atoms, show-
ble broadband photodetectors based on the In2 Se3 show consid- ing the high-quality crystal structure of the PtTe2 thin films.[113]
erable flexibility, good stability and excellent photoelectric perfor- The Au substrate exhibits a good chemical inertness toward
mance, such as efficient response with 5.6 A W−1 and good detec- precursors containing VI A group elements and is suitable for
tivity with 7×1010 Jones. However, most of TMDs grown on mica preparing large-area 2D TMDs.[26,114] Gao et al.[26] successfully
substrates need to be transferred to SiO2 /Si substrates for device synthesized millimeter-scale monolayer single crystal WS2 thin
fabrication, which may damage the materials to a certain extent films on Au substrates through a CVD process. Then they accord-
and affect the behavior of 2D TMDs. Moreover, it isn’t easy to di- ingly realized the large-area roll-to-roll/bubbling productions of
rectly obtain highly oriented wafer-scale 2D TMDs on the mica WS2 and WS2 /graphene heterostructures, as well as the batch
substrates.[102,103] production of large-area flexible monolayer WS2 film FET arrays.
Shi et al.[114] directly synthesized the uniform wafer-scale mono-
layer 2H-TaSe2 films with a tunable thickness on Au substrates
3.3. Noble Metal Substrates by a facile CVD. Au substrates can be used to prepare wafer-
scale TMDs, but we need to transfer films from Au or metal
The noble metal substrates have highly matched lattice symmetry substrates to other substrates for device applications. This pro-
with TMDs, as a result, various noble metal substrates with good cess can damage the material and fails to maintain the original
chemical inertness have been chosen to grow 2D TMDs.[104–106] properties.[26,115] Besides, the films grown on Au substrates can
For example, Li et al.[104] prepared Au (111) single crystal thin be directly used for STM/STS characterization or electrocatalytic
film substrate by sputtering Au (111) onto the c-plane sapphire hydrogen evolution, which is conducive to studying the intrin-
wafer. Figure 6a shows the flow chart of MoS2 growth on the Au sic properties and properties of TMDs.[116] And meanwhile, the
(111) substrate. The seamless stitching of MoS2 domains results 6-fold symmetry of Au substrates is incompatible with the 3-fold
in highly oriented wafer-level MoS2 films. The authors indicate symmetry of TMDs. This incompatibility inevitably results in an-
that high growth temperature can make the MoS2 seeds rotate tiparallel domains and twin boundaries, making it challenging to
in an optimal growth direction, eventually reaching more than prepare a single crystal.[117]
99% rotational alignment and the average size is ≈4.1 μm of the
products (Figure 6b). The atomic steps with a cross angle of 60°
in three directions were also observed on the MoS2 film surface 3.4. Sapphire Substrates
(Figure 6e), which reflects the characteristics of the Au (111) sub-
strate. Both macroscopic and microscopic studies confirm that The bulk c-plane sapphire substrates have a 3-fold symmetry,
unidirectional MoS2 domains on Au (111) film can be seamlessly which matches well with TMDs. However, the top atomic layer
spliced into highly oriented MoS2 films.[104] in close contact with the TMDs has a 6-fold symmetry, which is
The Au substrate also plays an essential role in the growth of preferential for the generation of antiparallel domains during the
2D Janus TMDs.[107] In recent years, the 2D Janus TMDs with growth of 2D TMDs.[71,118] For example, Zhang et al.[119] reported
new structures have been prepared,[108–110] and the different elec- the epitaxial growth of highly oriented large-scale MoS2 films by
tronegativity of the top and bottom chalcogen layers break the using a multi-source CVD method. In this setup (Figure 6g),
out-of-plane mirror symmetry with a manifold of novel physical seven miniature quartz tubes in the growth chamber served as
phenomena.[111,112] Gan et al.[107] successfully synthesized large- pockets for reaction sources. This multi-source design provides
Figure 6. The growth of TMDs on metal and sapphire substrates. a) Schematic diagram of single crystal MoS2 growth. b) SEM image and c) AFM
morphology image of MoS2 domains growth on the Au(111) substrates. Reproduced with permission.[104] Copyright 2021, Wiley-VCH. d) Schematic
illustration of the one-pot CVD for the growth of Janus SeMoS. e) Typical optical image and f) AFM image of transferred monolayer Janus SeMoS.
Reproduced with permission.[107] Copyright 2022, Wiley-VCH. g) Schematic diagram of the multisource CVD setup. h) Optical image of the beginning
of growth MoS2 . i) Typical STEM image of the MoS2 domain boundary. Reproduced with permission.[119] Copyright 2020, American Chemical Society. j)
Optical image of rectangle MoS2 grains grown on the a-plane sapphire substrate. k) Optical image of MoS2 grown at 750 °C. l) PL spectra of as-grown
MoS2 grain at different temperatures. m) Adsorption energy as a function of orientation angle between the MoS2 seed on sapphire. Reproduced with
permission.[120] Copyright 2020, Wiley-VCH.
a uniform cross section of the precursors, which is key for the Recently, the growth of 2D TMDs on 2-fold symmetry a-plane
uniform growth on substrates. Figure 6h shows that the MoS2 sapphire substrates was also reported. Xu et al.[120] synthesized
domains have two consistent orientations at the beginning of highly aligned single crystal MoS2 on a 2-fold symmetry a-plane
growth. The STEM image (Figure 6i) of a representative MoS2 do- sapphire substrate. The MoS2 grains grown on a-plane sapphire
main boundary shows an atomic structure of 60° domain bound- present a novel rectangular shape with almost one orientation
aries in the obtained MoS2 . The authors realized a 4-inch wafer- as shown in Figure 6j. They also found that high temperature
scale highly oriented monolayer MoS2 with large domain sizes by is favorable for the rotation of initial MoS2 seeds to the ori-
this method. And the monolayer MoS2 shows remarkable unifor- entation configurations. The triangular MoS2 grains with ran-
mity across the entire sapphire substrates.[119] dom orientation were obtained at 750 °C, which is similar to the
products grown on c-plane sapphire substrates (Figure 6k). The tooth-gullet step edges. In the annular dark-field STEM (ADF-
photoluminescence (PL) intensity of MoS2 on sapphire substrate STEM) image, the atomic sawtooth Au (533) surface and the top-
decreases gradually with the increase of growth temperature (Fig- most WS2 monolayer is clearly distinguishable (Figure 7g). And
ure 6l), indicating a strong MoS2 -substrate interaction which in- then the absence of grain boundaries in WS2 films was verified
duces the anisotropic growth of MoS2 and thus enabling the for- by HRTEM (Figure 7h). Figure 7i shows the model of the WS2 do-
mation of rectangular grains. The DFT calculation (Figure 6m) mains on the Au (221) substrate. And the B edge is considered as
confirms that the 0° orientation is the most energetically stable a nucleation site, where a topmost Au atom is placed between the
configuration. The authors first synthesized highly aligned MoS2 second top Au layers along the step edge. The DFT calculations
grains on 2-fold symmetry a-plane sapphire, and discovered that indicated that the sulfur atoms energetically favor 0° at the step
the size, orientation and shape of MoS2 domains significantly de- edge over other angles independent of Miller indices, and Fig-
pend on the growth temperature.[120] ure 7j shows the structural model of the single crystal WS2 across
Besides, a number of other studies have also proved that the the Au (221) step edges. The atomic sawtooth Au (221) substrate
sapphire substrate is one of the most ideal substrates for the can also be used to synthesize the MoSe2 /WSe2 heterostructure
growth of large-scale TMDs.[45,121,122] Aljarb et al.[123] systemati- (Figure 7k), and the domains with an oriented arrangement could
cally studied the growth of MoS2 monolayer on c-plane sapphire be observed clearly.[129]
through the CVD method. And DFT simulations confirmed that
there exist two preferred orientations (0° or 60°) on sapphire.
Claro et al.[124] also obtained ultrathin films of wafer-scale 2D 𝛽- 4.1.2. Stepped Sapphire Substrates
In2 Se3 on a c-sapphire substrate with excellent structural quality.
Furthermore, hundreds of photodetector devices are fabricated The unidirectional alignment of TMD islands has been achieved
using wafer-scale films, which show a fast response time of 7 ms. on Au substrates by taking advantage of the strong coupling be-
Although highly oriented TMD films can be obtained, few grain tween the TMDs edge and step edge on the Au surface. When
boundaries can also deteriorate the carrier transport, and optical growing TMDs on an insulating substrate like sapphire, strong
and even chemical stability.[125,126] edge-step edge coupling may not be appropriate due to the
self-passivation of the TMD edge and the inert surface of the
4. Growth on Modified Substrates insulator.[130,131] For example, Chubarov et al. prepared WS2 do-
mains with high nucleation density and small unidirectional ori-
4.1. Surface-Stepped Substrates ̄ steps. However, the ex-
entation on c-plane sapphire with <1120>
istence of translational boundaries was observed.[132] Therefore,
4.1.1. Stepped Metal Substrates it needs more careful control of the growth kinetics to achieve
perfect domains stitching on sapphire substrates.
Recently wafer-scale single crystal h-BN was successfully pre- To get wafer-scale single crystal TMDs, recently, Li et al.[30]
pared on Cu substrates with step edges.[127] The coupling of h-BN custom-designed c-plane sapphire wafers with a major miscut an-
zigzag edges with Cu <211> step edges results in the unidirec- gle towards the A axis (C/A), and successfully synthesized wafer-
tional alignment of h-BN domains. On this basis, Yang et al.[128] scale single crystal MoS2 films in a low-pressure CVD system un-
realized the epitaxial growth of wafer-scale uniform single crys- der a sulfur-rich condition. The Mo foil and O2 precursors are
tal MoS2 monolayers on vicinal Au (111) through a CVD method. also crucial for the controlled growth of MoS2 . The in situ oxi-
Figure 7a shows the schematic illustration of the Au (111) forma- dation of Mo foil to MoO3 with the supply of O2 accurately ad-
tion and the single crystal MoS2 growth process, in which the justs the “on/off” of MoO3 vapor, thus achieving precise control
formation of 60° oriented domains is inhibited. The SEM image over the “start/stop” of the deposition process. Figure 8a shows
(Figure 7b) indicates the MoS2 domains with trapezoid shapes the corresponding epitaxial MoS2 domain alignment along the
and consistent orientation. Figure 7c shows one edge of the MoS2 sapphire steps, showing a consistent orientation. The optical
domain docks with the step of Au (111). To explain the unidi- microscopy image (Figure 8b) of a representative as-grown tri-
rectional growth behavior of MoS2 domains on vicinal Au (111), angular MoS2 domain shows a 100% unidirectional alignment.
DFT calculations are carried out. Figure 7d shows three typical Through the polarization SHG mapping (Figure 8c) of the com-
contacting directions of MoS2 docking to the steps of the Au sub- bined unidirectional domains, no significant decrease of inten-
strate. The calculation (Figure 7e) demonstrates the surface and sity is observed across the boundary, proving that there is no
step contact energies with various edges, and the coupling be- grain boundary at the splice. Under the S-rich condition, the first-
tween the Mo zigzag edge and B-step is energetically more favor- principles calculation (Figure 8d,e) indicates that the ZZ-Mo-S2
able. In addition to the effect of the steps, highly oriented MoS2 with a 100% S coverage bonding with <1010> ̄ steps are the most
domains can also be obtained by precisely controlling the S/Mo stable configuration, whose formation energy is lower than that
ratio. of the antiparallel domain orientation (ZZ-S2 ). Meanwhile, the
While single crystal TMDs have been produced on the Au domains with these two orientations bonding with <1120> ̄ step
(111) vicinal surface,[128] the effect of the substrate surface with edge have the same formation energies. The nucleation along the
other Miller indices still requires investigation. Choi et al.[129] step edges also is found in the AFM image (inset in Figure 8e).
successfully synthesized single crystal TMDs using the atomic This method can also be used to grow MoSe2 single crystals with
sawtooth Au substrate, which is regardless of Miller indices. Fig- a size of up to 8 inches.[30]
ure 7f shows the seamless stitching of unidirectional WS2 do- The same substrate treatment method applies to a-plane sap-
mains on the atomic sawtooth Au surface composed of periodic phires. Wang et al.[73] reported the successful epitaxial growth of
Figure 7. The growth of large-scale TMDs on the stepped metal Au substrates. a) Schematic of the Au(111) formation and MoS2 growth process. b)
SEM image of isolated MoS2 domains c) STM image of one edge of the MoS2 domains docking with the step. d) Schematic view of the three typical
directions of the contacting edges for MoS2 docking to the steps. e) Surface and step contact energies per MoS2 unit of MoS2 nanoribbons with various
edges. Reproduced with permission.[128] Copyright 2020, American Chemical Society. f) Schematic illustration of WS2 film grown on an atomic sawtooth
Au surface. g) Cross-sectional ADF-STEM image and the corresponding ball-and-stick model of as-grown WS2 on an atomic sawtooth Au (533) surface.
h) ADF-STEM image of WS2 . i) Side and top views of WS2 cluster on Au (221) surface. j) The corresponding structural model of the WS2 across the
Au step edges. k) SEM image and schematic illustration of as-grown MoSe2 /WSe2 heterostructure. Reproduced with permission.[129] Copyright 2021,
Wiley-VCH.
a 2-inch single-crystal WS2 monolayer on the vicinal a-plane sap- monolayer single-crystal film. The optical image clearly shows all
phire surface at the same time. Figure 8f shows the schematic of the unidirectional islands with the same trapezoidal shape. The
the growth process of a WS2 monolayer on vicinal a-plane sap- AFM image (Figure 8g) shows that the longest edge of the WS2
phire. The WS2 domains on this substrate have a uniform ori- ̄
island is a zig-zag edge along the <1100> direction of substrates.
entation and seamlessly interconnect with one another, forming Based on the DFT calculations (Figure 8h), the relative energy
single-crystal WS2 films. Further characterization and theoreti- difference between two antiparallel WS2 islands across the step
cal calculations provide insight into the growth mechanism of edge on the substrate is attributed to symmetry breaking. It is
Figure 8. The growth of wafer-scale 2D TMDs on the stepped sapphire substrates. a) Step orientations on C/A c-plane sapphire. b) Optical microscopy
image of MoS2 domains grown on miscut sapphire. c) Polarized SHG mapping of two merging MoS2 domains on the C/A substrate. d) The formation
̄ steps with different S coverage. e) Four possible edge configurations on the miscut sapphire.
energy of ZZ MoS2 edges attached to the sapphire <1010>
Reproduced with permission.[30] Copyright 2021, Springer Nature. f) Schematic of the growth process of a WS2 monolayer on vicinal a-plane sapphire.
g) AFM image of a WS2 domain. h) Top: DFT calculations of the binding energies of a WS2 triangular island with different rotation angles. Bottom:
relative energy difference between two antiparallel WS2 domains due to symmetry breaking. Reproduced with permission.[73] Copyright 2022, Springer
Nature. i) The DFT calculation and analytical model free energy at the different top and bottom layer sizes. j) The formation energy of bilayer MoS2 at
various step heights. k) Cross-sectional HAADF-STEM image of bilayer MoS2 at the sapphire step edge. l) AFM image of the bilayer MoS2 domains.
Reproduced with permission.[31] Copyright 2022, Springer Nature.
thought that a dual-coupling-guided mechanism governs the epi- The carrier mobility of monolayer MoS2 is comparatively low
taxial alignment of WS2 domains and the step edge reduces the and can be severely affected by optical phonons, defects, and
symmetry of the sapphire from C2 to C1 . The low symmetry of impurities.[133] The controllable epitaxial growth of multilayers
the substrate step edge allows us to distinguish the two antipar- is very important in optoelectronic devices.[134,135] More recently,
allel alignments of the WS2 islands and finally, only WS2 islands Liu et al.[31] successfully synthesized bilayer MoS2 using c-plane
with one type of alignment exist.[73] sapphire with a miscut angle of ≈1° as an epitaxial substrate.
Figure 9. The growth of TMDs on stepped 𝛽-Ga2 O3 substrates. a) Schematic illustration of the growth of the monolayer MoS2 nanoribbons along the
aligned ledges on the 𝛽-Ga2 O3 (100) substrate. b) Cross-sectional HAADF HR-STEM image of the 𝛽-Ga2 O3 (100) substrate. c,d) Computer-generated
atomic models suggest two possible nucleation events on (−201) ledges with orientations towards 0° c) and 180° d). Reproduced with permission.[140]
Copyright 2020, Springer Nature.
Figure 8i shows that the monolayer is the most thermodynam- steps may also be an effective way to achieve large-scale single-
ically stable, and the bilayer is metastable, making it challenging crystal 2D TMDs.[138,139] For example, Aljarb et al.[140] successfully
to prepare bilayer MoS2 in a controllable way. The DFT calcula- demonstrated the edge-directed epitaxial growth of continuous,
tions for the formation energy of MoS2 bilayers indicate that the self-aligned, and monolayer single-crystal MoS2 nanoribbons on
interfacial formation energy markedly decreased with step height stepped 𝛽-Ga2 O3 substrates (Figure 9a). The growth is guided by
(Figure 8j). The cross-sectional HAADF-STEM image (Figure 8k) the combination of the steps and the surface-diffusion-limited
proves that bilayer MoS2 is obtained on the stepped sapphire sub- pathway, which is intrinsic to the Ga2 O3 substrates. The nucle-
strate with a step height of 1.48 nm. Moreover, the image also ation of MoS2 domains takes place at the steps of substrates. The
presents that the nucleation and growth of the bilayer are simul- cross-sectionalw HAADF HR-STEM is performed to understand
taneous instead of layer by layer. The AFM image (Figure 8l) the preferred nucleation and the controlled growth along the step
shows that the transferred MoS2 is still bilayer. Therefore, by in- of the substrates. Additionally, Ga vacancies are observed on the
troducing step-edge interfacial interactions, the bilayer MoS2 is ̄
top of (201) ledges (Figure 9b). Due to natural presence of Ga va-
synthesized.[31] In summary, steps on sapphire substrates can cancies, computer-generated atomic models suggested two pos-
lift the energy degeneracy of antiparallel orientations and guide ̄
sible nucleation events on (201) ledges (Figure 9c,d). The pres-
the unidirectional alignment of nucleation and growth of the 2D ence of the ledge provides an energetically favorable docking site
TMD domains. Generally, the step edges on the substrate ca be that breaks the energetic degeneracy by ≈2 eV, thus unidirection-
used as the preferred nucleation sites, making 2D TMDs more ally orienting the seeding flakes. This epitaxial growth mode[140]
likely to nucleate at step edges and form the energy stable chem- also shows universal generalization for the growth of p-type WSe2
ical bonds with edge atoms.[136,137] nanoribbons and lateral heterostructures of p-type WSe2 and n-
type MoS2 .
The direct growth of TMDs on h-BN by CVD methods would
4.1.3. Other Stepped Substrates be a significant advancement in fabricating high-quality TMD
electronic devices in a scalable and controllable way.[141–143] The
In addition to the substrate treatment used to get steps on the high dielectric constant and chemically inert surface of h-BN in-
surface, choosing substrates with suitable symmetry of intrinsic hibit the scattering of charged impurities and substrate phonons,
resulting in higher mobility and higher exciton density in the ad- served directional growth of MoS2 crystals. The 2D MoS2 crys-
jacent TMDs monolayer.[144–146] In addition, with a band gap of tal serves as a seed during the early growth stage of the MoS2
5.9 eV, the h-BN can be used as an electrical insulation layer to nanoribbons can be observed in the HRSEM image (Figure 10k).
construct FETs. Fu et al.[147] obtained highly oriented monolayer The Monte Carlo simulations (Figure 10l) reveal that P preferen-
MoS2 domains on low symmetry h-BN substrates under an envi- tially separates at the surface, resulting in a stepped structure that
ronment with a high temperature and ultralow precursor. Zhang primarily terminates by the Si-P and P-P dimers. And the DFT
et al.[148] found a defect-controlled approach for the nucleation calculation (Figure 10m,n) proves that the Si-P has a stronger in-
and epitaxial growth of WSe2 on h-BN. The single atom vacancy teraction with an incipient MoS2 crystal, which can explain the
on the h-BN surface can capture W atoms, breaking the surface proliferation of stabilized nanoscale 2D seed crystals. Moreover,
symmetry and resulting in a decrease in the formation energy the width of these MoS2 nanoribbons is systematically controlled
of WSe2 in one direction.[148] In summary, it is a promising ap- between 50 and 430 nm by varying the total dose of PH3 during
proach for the growth of wafer-scale single-crystal 2D TMDs on the surface treatment.[153]
surface-stepped substrates. On the one hand, the edge on the sur- The surface modification of inert substrates (e.g., SiO2 /Si) to
face has the lowest formation energy, and the nucleation is more attach functional groups on the surface is beneficial for the prepa-
likely to occur at the step edge during the growth.[149] On the ration and transfer of large-area TMDs.[154,155] Chen et al.[154] syn-
other hand, the steps break the limit of the intrinsic symmetry thesized large-area, uniform WS2 films on SiO2 /Si substrates
of substrates, which may lead to oriented nucleation.[71] These decorated with 3-aminopropyltriethoxysilane (APS). The pres-
might enable the fabrication of wafer-scale single-crystal TMDs ence of APS functional groups on the treated substrate provides
by guiding the unidirectional growth of 2D domains and seam- a higher degree of freedom to the precursors, which is helpful
lessly stitching on design substrates with surface-step edges. for preparing centimeter-scale WS2 films. This strategy can also
be used for the growth of large-area MoS2 .[154] Briefly, the surface
functionalization treatment on an inert substrate can reduce the
4.2. Chemically-Functionalized Substrates formation energy of 2D TMDs, and is beneficial to the growth
of larger-size TMDs. However, it is still challenging to prepare
Surface functionalization of the substrate with proper chem- wafer-scale single-crystal 2D TMDs on such substrates.
ical reagents may provide a high degree of freedom to the
precursor[29] and decrease the formation energy during CVD
growth,[150] enabling better control of the size and shape of 4.3. Curved Substrates
2D products.[151] Recently, Baek et al.[93] successfully obtained
micrometer-scale SnS grains on SiO2 /Si substrates at a low tem- In addition to the substrate modification methods mentioned
perature by modifying the surface with hexamethyldisilazane above, the growth of TMDs on curved substrates is also an
(HMDS). Figure 10a shows the schematic diagram for the growth essential method for integrating 2D TMDs directly with 3D
of SnS grains, and an inert surface is created on the substrate af- substrates.[156,157] For instance, the growth of 2D TMDs on optical
ter the HMDS treatment. The SEM image (Figure 10b) shows fibers is highly promising for the integrated optoelectronic and
that the SnS grains grown at 270 °C are rectangular. The cross- photonic systems.[157–159] However, the growth of large-scale and
sectional HRTEM image (Figure 10c) confirms the layered struc- high-quality monolayer TMDs on optical fiber is still challenging.
ture and sharp interface of large SnS grain. The HDMS can re- Ngo et al.[158] directly synthesized the monolayer MoS2 on the
act with the hydroxyl groups on the SiO2 surface (Figure 10d). fiber’s core and demonstrated the enhanced second-harmonic
And the XPS results (Figure 10e) also prove the replacement of generation in the functionalized fibers (Figure 11a). The precur-
the functional group by the -OSi(CH3 )3 . The optical image (Fig- sors are carried onto the exposed-core SiO2 fibers (ECFs) by the
ure 10f) indicates that the contact angle for the HMDS-primed gas, and then the MoS2 crystals directly grow on the ECF’s core
surface is increasing and that the treatment reduces the surface during the CVD process (Figure 11b). The densely coated MoS2
energy of the substrate. Further calculation also shows that the monolayer on the SiO2 fiber substrate is prepared (Figure 11c) by
reaction barrier decreases after treatment (Figure 10g). The large adjusting the precursor flow rate and the position of the ECF in
grain under a low temperature is attributed to the increase in the reaction zone. The height of the synthesized MoS2 is 0.9 nm,
the surface diffusivity of the absorbate through substrate surface which is overall equivalent to the thickness of a MoS2 monolayer.
modification, which can effectively decrease the migration bar- Moreover, the MoS2 -functionalized fiber exhibits a second-order
rier of substrates.[93] susceptibility value of 44 pm V−1 and a second-harmonic gener-
The chemical treatment of substrate surfaces can also control ation conversion efficiency of 0.2 × 10−3 m−2 W−1 .[158]
the morphology and dimensions of TMDs.[152,153] For instance. Similarly, Zou et al.[159] prepared the highly nonlinear 2D
Chowdhury et al.[153] developed a method to control the structure MoS2 , which is directly grown onto an optical fiber’s internal
and dimension of 2D TMD crystals by treating Si(001) substrate walls by a two-step CVD process (Figure 11d). The key aspect
surfaces with PH3 . Figure 10h shows the typical growth mode of the growth is the pre-deposition of Mo source into the fiber
for forming triangular 2D MoS2 crystals on SiO2 substrates. The holes. The coverage and thickness of MoS2 can be facilely tuned
PH3 -treated substrates enable the directional growth of MoS2 , re- by the concentration (c) of Na2 MoO4 . When the concentration
sulting in crystal MoS2 nanoribbons with adjustable width (Fig- of Na2 MoO4 increased from 6 to 8 mg ml−1 , the size of MoS2
ure 10i). The HR-SEM image (Figure 10j) shows that the single increased gradually from 250 μm triangles to a continuous film
nanoribbon has a uniform width along its length. Further calcu- (Figure 11e). No apparent defects are observed from the STEM
lation and characterization identify the mechanism for the ob- image, confirming the formation of high-quality MoS2 domains
Figure 10. The growth of 2D TMDs on the chemically-functionalized substrates. a) Schematic illustration of the growth of SnS on HMDS pretreated
substrate. b) SEM and c) cross-sectional HRTEM image of SnS grown on HMDS-primed SiO2 . d) The surface change of SiO2 after HMDS treatment. e)
XPS spectra of the Si 2p core level in pristine and HMDS-primed SiO2 . f) Optical images of a water droplet on SiO2 before and after HDMS processing.
g) Schematic of the reaction barrier for surface diffusivity of SnS. Reproduced with permission.[93] Copyright 2020, American Chemical Society. h, i)
Scheme illustration synthesis of MoS2 crystals on SiO2 (h) and PH3 -treated Si(001) substrates (i). j) High-resolution SEM image of a single MoS2
crystal on PH3 -treated Si substrate. k) High-resolution SEM image of the early stage of MoS2 crystal on PH3 -treated Si substrate. l) Side and top views
of a representative Monte Carlo snapshot of the PH3 -treated Si surface. m) DFT-calculated adsorption energy between an incipient MoS2 crystal and a
P-P dimer-covered surface, a Si-P dimer-covered surface, and a SiO2 . n) Cluster model of a MoS2 domain on SiO2 , Si-P, and P-P surfaces. Reproduced
with permission.[153] Copyright 2020, Springer Nature.
through this method. Furthermore, the marginal variations in electric characteristics. For instance, Wang et al.[164] synthesized
the frequency difference between A1g and E2g as well as the nar- the monolayer WS2 on the curved substrate with various curva-
row distribution of the full-width at half-maximum values of the tures. As shown in Figure 11j, large monolayer WS2 crystals with
E2g peak along the entire fiber (Figure 11f) indicates that the 5 to 120 mm edge lengths can conformally coat on the “donut” ar-
as-prepared monolayer MoS2 film is highly uniform. More im- rays and accommodate the induced strain, while retaining their
portantly, both second- and third-harmonic generation of mono- equilateral-triangle shape. The height (20 nm) of the donuts fur-
layer MoS2 /fiber can be enhanced by ≈300 times compared with ther confirms the conformal growth (Figure 11k). The curvature-
monolayer MoS2 on silica.[159] The integration of TMDs with op- induced strain is observed evidently in the PL mapping (Fig-
tical fibers can inspire versatile nonlinear applications in optical ure 11l). An SHG mapping (Figure 11m) of the monolayer MoS2
fibers, such as terahertz sources, high-harmonic generation, and is provided and indicates that the entire crystal in the flat regions
nonlinear parametric amplification.[160–163] of the substrate appears to have the same crystalline orientation.
Various 2D TMDs have been grown on curved substrates to They also discover that the strain between substrates and TMDs
explore the effect of strain on their growth direction and photo- can accelerate the crystal growth in specific directions.[164] The
Figure 11. The growth of large-scale 2D TMDs on curved substrates. a) Illustration of the concept to demonstrate SHG with embedded 2D materials on
an ECF. b) Cross-sectional SEM image of the core region of the ECF during the CVD process. c) The optical image of MoS2 on optical fiber. Reproduced
with permission.[158] Copyright 2022, Springer Nature. d) Schematic of the designed two-step growth method. e) Dependence of MoS2 coverage on the
Na2 MoO4 aqueous solution concentrations. f) Statistical (A1g - E2g ) and FWHM values of the E2g peak plotted as a function of the numbered sites along
the whole MoS2 -embedded fiber. Reproduced with permission.[159] Copyright 2020, Springer Nature. g) AFM phase image of a monolayer WS2 crystal
grown on a hexagonal array of 1.7 mm-diameter, 20 nm-height donuts on 4 mm centers. h) AFM image is taken from an individual “donut” with the
corresponding AFM height profile (blue inset curve). i) PL peak position and j) SHG intensity correspond to the highlighted region in (g). Reproduced
with permission.[164] Copyright 2019, AAAS. k) Illustration of synthesizing large-scale MoS2 on polymer substrates. l) AFM image for the MoS2 film
on PI substrate after being annealed at 350 °C. m) HRTEM image of the synthesized MoS2 . Inset: SAED pattern of the MoS2 film. Reproduced with
permission.[169] Copyright 2022, Wiley- VCH.
growth of 2D TMDs on curved substrates presents an important turing of flexible devices provides new ideas for the application
strain engineering strategy for the growth and optoelectronic de- of 2D TMDs.[166–168] Gong et al.[166] directly synthesized mono-
vice application of 2D crystals. layer MoS2 on curved flexible substrates under 450 °C by using
In addition, the direct growth of 2D TMDs on the curved flex- (NH4 )2 MoO4 as precursors. Then they built a flexible photode-
ible substrate can be directly used to prepare flexible electronic tector with strong photoresponse directly on the MoS2 /PI.[166]
devices such as flexible gas sensors,[165] and the direct manufac- Li et al.[169] also directly prepared large-scale MoS2 on flexible
substrates by combining inkjet printing and annealing under a the controlled synthesis of periodic 2D van der Waals arrays (Fig-
low temperature. In the process, the precursors have been de- ure 12e). The large-area 2D semiconducting TMDs (for example,
posited onto the flexible substrate through inkjet printing. Then WSe2 , MoS2 , WS2 ) are chosen as the van der Waals epitaxial sub-
the substrate is placed into a hot zone for annealing under 350 °C, strates. Then periodic defect arrays are formed on the substrate
and the MoS2 is synthesized directly on flexible substrates (Fig- via focused laser (488 nm) irradiation combined with a raster
ure 11k). The obtained MoS2 has a thickness of 15 nm (Fig- scan in a confocal laser system. These defect arrays serve as the
ure 11l), and few-layer MoS2 can also be achieved by lowering only nucleation site for metallic TMDs growth at a specific loca-
the ink concentration or decreasing the printing passes. The tion on substrates, resulting in patterned van der Waals arrays.
low-magnified TEM image confirms that the synthesized MoS2 Additionally, enlightened by self-seeding fullerene nuclei,[178]
film is large and continuous without cracks (Figure 11m). The seeds such as Pt/Ti and Au have also been used to serve as the
MoS2 on flexible substrates exhibits superior mechanical flexi- nucleus point for the growth of TMD arrays.[179,180] For example,
bility and durability (2% variation resistance over 10000 bend- Li et al.[175] employed Au nanoparticle arrays obtained by pho-
ing cycles).[169] The direct growth on polymer substrates without tolithography technique as seeds for the growth of MoS2 arrays
transfer is essential for integrating 2D TMDs and flexible sub- (Figure 12f). First, the Au nanoparticles serve as the specific nu-
strates, which is an important step towards the scalable fabrica- cleation sites for MoS2 growth, then MoS2 fully covers the Au
tion of 2D flexible electronics. seeds and subsequently grows along the substrate. The match-
ing of the Au (111) surface with the lattice outside MoS2 leads to
a reduction of MoS2 formation energy. Thus, Mohapatra et al.[180]
4.4. Substrate Seeding Strategies also successfully synthesized a large-area MoS2 membrane with
controllable microstructure by combining Au seeds growth with
In a typical CVD process, the low nucleation barrier of 2D TMDs a confined area strategy. Such seeds as growth promoters can-
leads to random nucleation on the substrate, which seriously hin- not be removed and can degrade the device’s properties. More
ders the growth of a high-quality and large-area arrays of prod- recently, Gan et al.[181] prepared the large-scale fabrication of pat-
ucts, making it less beneficial for industrial applications.[170,171] terned TMDs monolayer arrays for applications in electronics
Therefore, substrate seeding strategies may be an effective way and optoelectronic devices by using the liquid Na2 MoO4 seeds
for the growth of uniform 2D TMD heterojunctions. It is usu- that can be removed without influence on the device properties.
ally realized by the creation of defects or pre-patterning of nanos- First, the liquid Na2 MoO4 precursors are patterned on SiO2 /Si
tructures that can decrease the formation energy of TMDs on the wafers via the soft lithography-based micro-molding in capillaries
substrate. As a result, it is an effective method for controlling the technique, and then the liquid precursors are converted to TMDs
growth of large-scale single-crystal 2D TMDs by precisely control- by a CVD process. This surface treatment method selectively in-
ling the number and position of the nucleus on a macroscopically troduces defects, allowing for accurate control of TMD nucleation
sized substrate.[172–177] position. It has the advantages of convenient processing, good
More recently, Zhang et al.[173] created periodic triangular stability and high universality,[182,183] but it is tough to precisely
WS2 -WSe2 arrays with precisely controlled dimensions and control the orientation for the growth of 2D TMDs, which is not
atomically clean edges using laser irradiation and thermal etch- conducive to the consistency of 2D TMD-based devices.[81]
ing to fabricate defects as seedings. Figure 12a schematically
shows the process for producing the WS2 -WSe2 mosaic het-
erostructures in monolayer WS2 films. Briefly, laser irradiation 4.5. Other Substrate Modification Methods
is used to create a periodic defect array in monolayer WS2 crys-
tals, then anisotropic thermal etching is used to produce a ho- Additionally, there are many other substrate modification meth-
ley WS2 with a periodic array of triangular holes and atomically ods for the growth of large-scale 2D TMDs, such as placing the
clean edges. Finally, the WS2 -WSe2 heterostructure arrays are precursor on the substrate surface,[184,185] and then directly trans-
produced by endoepitaxial growth in a CVD process. The Ra- forming the precursor to large-area 2D TMDs. Wang et al.[186]
man spectra (Figure 12b) of different points in the heterostruc- successfully prepared WS2 by placing the precursor W foil on
tures show that the WSe2 region has a blue shift at the interfaces, the undersurface of the Au substrate to form an alloy substrate
and the phenomena may be attributed to compressive strain and accurately controlled the internal defects. The internal de-
generated at the interface. The Raman mapping (Figure 12c) at fects are ubiquitous in 2D TMDs, and they can affect the struc-
251 cm−1 also proves the existence of compressive strain at the ture and properties of the materials and also introduce new
interface, and the inhomogeneity of strength may be attributed functionalities.[187–189] Figure 13a shows the schematic illustra-
to the inhomogeneity of strain in the endoepitaxial process. Then tion of the growth process of monolayer WS2 exhibiting a high
the schematic growth is observed, and the endoepitaxial growth density of antisite defects, where Au is used as the growth sub-
process initiates at the three edges of the triangular pore and strate and W foil is chosen as the W precursor. In this anneal-
gradually grows inward (Figure 12d). The same method is used ing process, the Au substrate allows the diffusion of W atoms
to prepare WS2 -MoS2 heterostructures. This designable material to form an alloy substrate. The SEM image (Figure 13b) shows
platform establishes a foundation for basic research and devel- the well-defined triangular WS2 domains with sharp edges. The
opment of complex devices and integrated circuits based on 2D antisite defect structure is determined by the HAADF-STEM,
heterostructures.[173] and Figure 13c demonstrates the defect distribution in the
Direct laser etching is also an effective method to fabricate WS2 monolayers, revealing a defect density of about 5.0%. The
defects as seedings on the substrates. Li et al.[174] first reported STM images (Figure 13d,e) verify that the atomic structures of
Figure 12. Substrate seeding strategies for the growth of large-scale 2D TMDs. a) Schematic illustration of the lateral endoepitaxial growth of WS2 -WSe2
monolayer mosaic heterostructures. b) The Raman spectra were collected from locations 1–3 as marked in the inset. c) Raman mapping images of the
WS2 -WSe2 monolayer mosaic heterostructures at 251 cm−1 frequencies. d) Schematic growth of WS2 -WSe2 mosaic heterostructure: The pits of arrayed
WS2 (left) Incompletely filled mosaic heterojunction (right). Reproduced with permission.[173] Copyright 2022, Springer Nature. e) Schematic illustrating
the defect-induced growth of TMD heterostructures. Reproduced with permission.[174] Copyright 2020, Springer Nature. f) Au seeds-induced MoS2 array
on SiO2 /Si substrate. Reproduced with permission.[175] Copyright 2018, American Chemical Society.
predominant antisite defects are SW and S2W , which is in good posited Mo-W layers on the substrates via ion bombardment.
agreement with the previous STEM analysis. The calculation of Then the uniform wafer-scale MoS2 -WS2 vertical heterostruc-
the density of states of monolayer WS2 with SW or S2W defect (Fig- tures are directly obtained. Similarly, Kim et al.[194] successfully
ure 13f) shows that the S2W defect will cause a defect state in the synthesized uniform wafer-scale WS2 films at a low tempera-
bandgap, which is 0.4 eV below the Fermi level. The metal anti- ture on the plasma-treated substrates. The substrates pretreat-
site defects on the S sites possess a theoretically predicted local ment process promotes nucleation and growth across the en-
magnetic moment and paramagnetic triplet ground states with tire substrate. Different from the above strategies, Xu et al.[195]
various spin splitting levels for spin qubits.[190–192] also successfully prepared high-quality and wafer-scale MoS2
Using a different strategy, Seok et al.[193] synthesized wafer- films by directly sulfurizing MoO2 film substrates which are
scale MoS2 -WS2 vertical heterostructures on the plasma pretreated by a capping layer annealing process (Figure 13i). The
treated substrate at 300 °C (Figure 13g). The synthesis mecha- crystalline quality of the substrate is significantly improved,
nism of the heterostructures is identified using HRTEM char- and its defects are minimized, enabling high-quality films
acterization (Figure 13h). With the aid of Ar plasma, the H2 S+ to be acquired on these substrates. And the as-grown MoS2
permeates through the bottom layers and reacts with the de- films exhibit field-effect mobility of 6.3 cm2 V−1 s−1 , which
Figure 13. Other substrate modification methods for the growth of 2D TMDs. a) A schematic illustrating the growth process of monolayer WS2 on Au/W
substrate. b) An SEM image of monolayer WS2 grown on Au/W substrate. c) HAADF Z-contrast STEM image of monolayer WS2 . d) and e) Simulated
STM images at a bias of −1.0 V for the structures of SW and S2W antisite defects in WS2 . f) The DFT calculation of states with and without antisite
defects. Reproduced with permission.[186] Copyright 2022, Wiley-VCH. g) The schematic of MoS2 -WS2 vertical heterostructures by plasma-enhanced
CVD. h) Illustration of the mechanism using time-dependent Ar + H2 S plasma and cross-sectional HRTEM images. Reproduced with permission.[193]
Copyright 2021, American Chemical Society. i) Flow diagram showing the synthesis of single-crystal MoS2 films converted from MoO2 films treated by
capping layer annealing process. Reproduced with permission.[194] Copyright 2020, Wiley-VCH.
is further suggestive of the high-quality nature of the MoS2 be used as a growth substrate for the high-quality MoS2 layers.
films.[195] Hoang et al.[197] also directly prepared wafer-scale MoS2 films on
In addition to the substrates mentioned above, a strategy the graphene template and the high-quality MoS2 /graphene het-
for the growth of large-scale TMDs by using 2D materials as erojunction exhibits ultrahigh photoresponsivity (4.3×104 A W−1 )
the template has been developed.[196–199] The atomically smooth upon exposure to visible light of a wide range of wavelengths.
and insert surface of 2D templates ensures the minimum dif-
fusion barrier of precursors, making it easier to prepare ultra- 5. Conclusions and Outlooks
thin and clean TMDs/2D materials heterojunctions.[200–202] The
unique photoelectric properties and novel physical phenomena In this review, we have summarized the recent applications of
of heterojunctions will broaden the application of optoelectronic substrate engineering strategies for the preparation of large-
devices.[174,203] Shi et al. [196] synthesized high-quality MoS2 by scale 2D TMDs. Substrates are considered to have a signifi-
using graphene as a template at a low temperature and found cant influence on the size, composition, thickness, and crys-
that other hexagonal structured substrates, such as h-BN, can tal quality of 2D TMDs. Accordingly, the substrate engineering
Figure 14. Outlooks on the future development of substrate engineering for the mature growth of 2D TMDs. a) The growth of large-scale single-crystal
heterojunctions. b) The direct large-scale growth on flexible substrates. c) The evolution of growth mechanism via substrate engineering.
strategies such as surface-stepping, chemical-functionalization, promote the basic physics research and device application of 2D
seeding approaches, and some other substrate modification semiconductors in the field of nanoelectronics and optoelectron-
methods have been developed significantly, paving the way for ics.
the mature production of 2D TMDs. For instance, by using Wafer-scale 2D TMD films are usually synthesized on rigid
such substrate engineering strategies, wafer-scale single-crystal substrates. They can be transferred with a large area to flexi-
2D MoS2 has been successfully synthesized on the stepped sap- ble substrates by a roll-to-roll process,[26,210] which is fast and
phire substrate, where the stepped sapphire has a miscut orien- avoids chemical contamination.[211–215] But it also remains a chal-
tation toward the C-axis or A-axis of the pristine sapphire sub- lenge for the growth of large-area 2D TMDs on flexible polymer
strate, and the step breaks the limit of intrinsic symmetry of the substrates during a CVD process that requires a high tempera-
substrate.[30,73] Similarly, the controlled epitaxial growth of bilayer ture to convert the precursors to TMD films,[216] because of the
MoS2 on the stepped sapphire has also been realized.[31,74] Al- low operating temperature of polymer substrates. Reducing the
though significant progress has been made in the past few years, reaction temperature is a universal way for the direct growth
the growth of wafer-scale 2D TMDs by substrate engineering still of large-scale 2D TMDs on various flexible polymer substrates.
faces several major challenges, and special attention should be With this regard, due to the rich functional groups of the sub-
given to the following aspects. strate surface, surface modification engineering can be used to
Stacking of 2D TMDs into heterostructures can be tailored for modify the surface with functional groups, which can be com-
specific applications, opening the door to the fabrication of var- bined with MOCVD by using the organic precursor solution, and
ious promising photoelectric devices.[204–206] While high-quality then the large-scale 2D TMD films can be directly converted in
wafer-scale TMDs have been successfully prepared on stepped a low-temperature annealing process on the flexible substrates
substrates through substrate engineering, the synthesis of het- (Figure 14b).[93,217] The direct preparation without destroying 2D
erojunctions of 2D TMDs continues to present many problems, TMD films on flexible polymer substrates under a low tempera-
and universal growth of large-scale heterojunctions with a high- ture can promote the development of flexible electronic devices.
quality interface is required. The as-prepared wafer-scale films The growth model of 2D TMDs on substrates remains a
may be used for the growth of large area high crystal quality het- work in progress, particularly with regard to comprehending
erojunctions. By precisely fabricating defects on the first layer the growth behaviors associated with nucleation on various sub-
TMD films as nucleation sites, highly controllable in-plane het- strates to form large-scale 2D TMDs. In a CVD system, extremely
erostructures arrays can be obtained.[207,208] For the preparation complex chemical processes in terms of thermodynamics and
of vertical heterojunction, the high metal/chalcogenide compo- kinetics affect the quality of the 2D TMDs.[218–220] It is essen-
sition radio in the precursor materials are conducive to the for- tial to directly observe the growth progress. In-situ growth and
mation of clusters with high activity barrier, which nucleate at characterization techniques can help elucidate the growth mech-
the top of the as-prepared large-scale single crystal TMDs to re- anism of 2D TMDs (Figure 14c).[221] MBE and MOCVD can
alize vertical heterostructures (Figure 14a).[209] The controllable help in this respect and also generally possess in-situ charac-
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Shaohua Li received his B.S. degree from the School of Materials Science and Engineering, Northeast-
ern University. He is currently a graduate student in the School of Materials Science and Engineering,
Huazhong University of Science and Technology (HUST). His research interests focus on the growth
of large-scale 2D materials for integrated optoelectronic devices.
Yuan Li received his B.S. degree and M.S. degree from Central South University in 2009 and 2011, re-
spectively. He then received his Ph.D. degree in materials science from the University of Alabama in
2015. Afterward he joined Northwestern University as a NUANCE postdoctoral research associate.
He is currently a professor in the School of Materials Science and Engineering in Huazhong University
of Science and Technology. His research interests mainly focus on 2D nanofabrication and integrated
optoelectronic devices.
Tianyou Zhai received his B.S. degree in chemistry from Zhengzhou University in 2003, and then re-
ceived his Ph.D. degree from the Institute of Chemistry, Chinese Academy of Sciences in 2008. After-
ward he joined in National Institute for Materials Science as a JSPS postdoctoral fellow and then as an
ICYS-MANA researcher within NIMS. Currently, he is a chief professor at the School of Materials Sci-
ence and Engineering, Huazhong University of Science and Technology. His research interests include
the controlled synthesis and exploration of fundamental physical properties of inorganic functional
nanomaterials, as well as their promising applications in electronics and optoelectronics.

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