- Open Access
Synthesis of 2D transition metal dichalcogenides by chemical vapor deposition with controlled layer number and morphology
© The Author(s) 2018
- Received: 2 August 2018
- Accepted: 10 September 2018
- Published: 28 September 2018
Two-dimensional (2D) transition metal dichalcogenides (TMDs) have stimulated the modern technology due to their unique and tunable electronic, optical, and chemical properties. Therefore, it is very important to study the control parameters for material preparation to achieve high quality thin films for modern electronics, as the performance of TMDs-based device largely depends on their layer number, grain size, orientation, and morphology. Among the synthesis methods, chemical vapor deposition (CVD) is an excellent technique, vastly used to grow controlled layer of 2D materials in recent years. In this review, we discuss the different growth routes and mechanisms to synthesize high quality large size TMDs using CVD method. We highlight the recent advances in the controlled growth of mono- and few-layer TMDs materials by varying different growth parameters. Finally, different strategies to control the grain size, boundaries, orientation, morphology and their application for various field of are also thoroughly discussed.
- Transition metal dichalcogenides (TMDs)
- 2D materials
- Growth mechanisms
- Chemical vapor deposition
In the last decade, after tremendous success of the first two-dimensional (2D) material, i.e. graphene, transition metal dichalcogenides (TMDs) have attracted significant research attention due to their extraordinary properties. The TMDs represent a large family of layered materials with a generalize single layer formula as MX2, where M represents a transition metal from group IVB to group VIII (layered structures are usually found in group IVB to VII B, like Ti, V, Nb, Mo, W, Re), and X represents the chalcogen (S, Se, and Te) . Compared with graphene, bulk TMDs show much wide range of physical properties, starting from insulators (e.g., HfS2) , semiconductors (e.g., MoS2, WS2) [3, 4], and semi metallics (e.g., WTe2 and TiSe2) [5, 6] to metallics (e.g., NbS2, VSe2) [7, 8]. Apart from this, a few of them (e.g., NbSe2, TaS2) shows unusual interesting properties like superconductivity, charge density wave (CDW, periodic crystal lattice distortion) and Mott transition (transition from metal to non-metal) [9–11]. However, mono- or few-layer TMDs exhibits other additional exciting electronics characteristics alone with abovementioned properties. As for example, monolayer MoS2 shows strong photoluminescence (PL) over bulk due to quantum confinements, confirmed by the change of bandgap from indirect to direct for bulk to monolayer MoS2 . Further research also indicates that the CDW transition temperature of NbSe2 increases on reducing the layer number due to the enhanced electron–phonon interactions in 2D materials . Due to numerous unique properties of thin layer TMDs materials, it has been used to fabricate new generation electronic [14–16] and optoelectronic devices [17–20] such as transistors, photodetector, photodiode, photovoltaic devices, etc. Therefore, researchers have devoted considerable efforts to synthesis high-quality and large-size TMDs thin layers, which plays a significant role in fundamental research and application exploration. Several techniques have been already introduced to synthesize atomically thin layer of high quality TMDs material such as mechanical exfoliation method [21, 22], liquid exfoliation method [23–25], chemical vapor deposition (CVD) method [26–29], wet chemical method [30, 31], etc. Among all synthesis techniques, the chemical vapor deposition (CVD) is promising for synthesis of high-quality TMDs layers with controllable layer number and domain size, as well as excellent properties, due to their simplicity and compatibility with industry standards.
In this review, we summarized some of the key and control factors affecting the growth of TMDs via CVD method. Here, CVD is used as a general term which covers the vapor transport and deposition methods. The growth mechanisms and synthesis approaches of mono- or few-layer TMDs are also be introduced. Moreover, we will thoroughly discuss the controllable growth of TMDs based on grain size/boundary, orientation, and morphology.
Different strategies have been applied in the synthesis technique to obtain high quality large scale mono- and few-layer TMDs to explore their promising properties in various field of applications. Typically, all the synthesis methods have been classified into either “top-down” or “bottom-up” approaches . Generally, exfoliation methods are followed “top-down” technique while CVD is based on “bottom-up” methods [33–35]. In a typical CVD process, precursors are reacted/or decomposed and deposited as mono- or few-layer film on the exposed substrate at relative high temperature. Many fundamental researches have been done to produce ultrathin TMDs materials with high crystal quality, scalable size, tunable thickness, and excellent electronic properties [26, 36, 37]. Compared with chemical vapor transport (CVT) method, which is commonly used to synthesize bulk single crystal materials, the typical CVD method we discussed in this review is for synthesizing mono- or few-layer TMDs. The reaction process is much quicker than CVT, and no subsequent mechanical exfoliation is required to obtain few layer structure for following study and application.
2.1 Synthesis routes for TMDs layers
On the other hand, due to the lower melting point of metal halides over metal sources, it is more efficient to control the ratio of metal and chalcogen. High quality single crystalline 3R-MoTe2 flakes were synthesized by CVD method by using MoCl5 as Mo precursor . Very recently, molten-salt-assisted CVD method has reported for synthesizing a series of (2D) transition-metal chalcogenides (TMCs), especially for some high melting points, low vapor pressure metal and metal oxides precursors. The addition of molten salts reacted with metal precursors, and form intermediate oxychlorides which has lower melting points, thus the mass flux and reaction rate successfully is increased. This method has demonstrated to be able to synthesize 47 kinds of transition-metal chalcogenides (TMCs), including 32 binary compounds, 13 alloys, and 2 hetero-structures . Similarly, some graphene-like molecules, such as reduced graphene oxide (rGO), perylene-3,4,9,10 tetracarboxylic acid tetra-potassium salt (PTAS) and perylene-3,4,9,10-tetracarboxylic dianhydride (PTCDA) can be used as growth seeds and promoted the MoS2 layer growth . Further research have also investigated how the seeding promoters and seed concentration influence the growth of MoS2 monolayer . It is believed that different kinds of aromatic molecules acted as a seeding promoters, deposited on various substrates and increased the surface adhesive force of MoS2 to improve the layer growth of MoS2.
2.2 Thermodynamics and Kinetics for TMDs Growth
Three growth modes have been identified for different kinds TMDs materials including island growth (Volmer-Weber growth mechanism), layer-by-layer growth (Frank-vander Merwe growth mechanism), and mixed growth (Stranski–Krastanov growth mechanism). It is well recognized that the integration of thermodynamics and kinetics with nucleation growth provided important guidance to understand the growth mechanism as well as TMDs layers control. Hence, in this review, we mainly discuss thermodynamics and kinetics for the growth of 2D TMDs, and several mechanistic models have been introduced based on those thermodynamic and kinetic mechanisms.
On the other hand, the growth rate of subsequent layer depends on the sizes of initial layer and subsequent layer. Recently, a multiscale model has been developed and found that a maximum size of layer-1, while minimum size of layer-2 ensured vertical growth according to thermodynamic criterion. The increasing size of layer-1 decreased the growth rate of layer-2, while the size of layer-1 reaching the maximum size, the growth of layer-2 ceased to grow. A successful vertical growth happens when the size of layer-2 exceeds the critical size before layer-1 reaching maximum size. By changing the kinetic parameters (growth temperature and flux), it was demonstrated that the monolayer was obtained at relatively low temperature but high gas flow rate conditions (Fig. 2c, d), consistent with the trend of growth of bilayer graphene at decreased supply of adatoms [57, 58]. In order to investigate and predict vdW epitaxy growth process to guide experimental study, a Kinetic Monte Carlo (KMC) simulation method was used to investigate the complex competitions in growth rate, morphology, homogeneous nucleation and layer number. Extrinsic parameters (including temperature, adsorption rate, chalcogen to metal ratio of the precursors), intrinsic parameters, site energy, adsorption energy and transition energy barriers, as well as substrate effects were introduced to provide a fundamental understanding about the growth mechanisms at atomic scale . Although this model was set for molecular beam epitaxy (MBE) growth of TMDs, after further refinements it applied to predict CVD growth qualitatively and quantitatively.
The potential applications in electronic and optoelectronic devices has demanded the scalable synthesis of uniform, high-quality TMDs layers. Generally, high-quality refers to high crystallinity, large domain size, defect-free, and limited grain boundaries. The quality of large scale uniform MoS2 layers largely depends on property factors such as grain size and boundaries, orientation and their morphology, as discussed below.
3.1 Domain size and grain boundaries
Depending on various mass flux and growth rate, the growth of 2D TMCs is divided into four routes (Fig. 3c). The formation of nucleus and the growth of domains depends on mass flux, especially metal precursor, while the grain size is determined by growth rate. High mass flux of metal precursor but low growth rate tends to form polycrystalline film with small grains and lots of grain boundaries (Route I), while high growth rate can produce smoother monolayer film with large grain size and limited grain boundaries (Route II). However, at low mass flux, it prefers to form single-crystalline with small domains at low growth rate (Route III), large monolayer single-crystal at high growth rate (Route IV) . In order to decrease the nucleation density, without changing the amounts of precursors or growth parameters, some additional attempts have been successfully made. For example, NiO foam was used to grow centimeter scale continuous monolayer MoS2 by trapping chemical precursors . Metal precursors (MoO3) reacted with NiO and form a Ni–Mo complex, thus the precursor concentration as well as nucleation density decreased. Recently, “liquid-state” substrates show a new possibility to grow large grain size TMDs materials. Because of the low nucleation density together with low migration coefficient, large MoSe2 and MoS2 monolayer single-crystals up to ~ 2.5 mm successfully deposited on the low-defect and homogeneous molten glass surface . Similarly, another report has further demonstrated that the uniform distribution of Na in soda-lime glass will promote the growth rate of monolayer MoS2. A face-to-face metal precursor supply route was designed to synthesize 6-inch uniform monolayer MoS2 with grain edge length larger than 400 μm. The DFT calculations proved that during the MoS2 growth, the energy barrier was reduced with Na adsorption . On the other way, due to the different facet-dependent binding energy between Au and MoS2, it is found that at relative high growth temperatures, large single-crystal domains prefer to grow on Au (100) and Au (110) than on Au (111) facets .
The grain boundary is another important factor that significantly affects the quality of layered TMDs, and therefore it is essential to understand the grain boundary formation mechanism, as well as the electric and optical performance at boundary. Two possible modes are observed for MoS2 boundary formation during vapor phase growth process. The traditional grain boundaries growth involves formation of chemical bonds between two single layer grains, where in-plane growth is stopped but the boundary site contributes to the nucleation of second layer. While the other mode of boundary formation involves no chemical bonds, with two grains overlap and continue to grow on top of each other . At the same time, the optical and electronic properties of faceted tilt and mirror twin grain boundaries in poly-crystalline MoS2 has been investigated, observing strong enhancement of PL and slight decrease of electrical conductivity at faceted tilt boundaries, with the opposite at the mirror twin boundaries . This has been further demonstrated that the PL mapping can be used to identify grain boundaries in MoS2 quickly due to the thermal mismatch induced non-uniform tensile strain . Meanwhile, it is also found that 60° grain boundaries, either point sharing or edge sharing, both consists of distinct fourfold ring chains and exhibit metallic behavior. Further work has provided insight into various small-angle (18.5°, 17.5°) grain boundaries possessing distinct kinds of dislocation core structures. The interaction of grain boundaries with point defects showed the possibility to control the precise grain boundary .
As mentioned above, the grain boundary formed from different misorientation of adjacent grains, which leads to distinct electronic structures across the boundary . In most cases, the distorted grain boundaries with high misorientation angles and defects lowered the quality of TMDs as electronic devices. Therefore, like grain-size controlled strategy, control the grains orientation as well as highly aligned growth of 2D TMDs are also important to promote the formation of large-size uniform layers. Two mechanisms have been developed to explain the dominant 60° misorientation. In the first scenario, the small 2D islands were pre-aligned at 60°; while at the second scenario, the random orientations of islands were drawn by capillary forces into 60° .
Recently, the evolution of novel structures of TMCs, like polygonal twins, screw dislocations, etc. is also widely studied because the possibility of new functions. The merging of single-crystal or changes of layer stacking not only form different morphologies, but also affect the optical, electronic, and magnetic properties of TMCs. Recent report has shown that the preparation of a spirals of layered MoS2 with AA lattice stacking morphology (contrast to centrosymmetric AB stacking in intrinsic MoS2), this non-centrosymmetric spiral leads to second-harmonic generation (SHG) signal . It is further confirmed that the triangular spiral WSe2 plates with strong SHG and enhanced PL signal, and the plates contain both triangular and hexagonal dislocations with diverse mixed properties . Wulff constructions is used for bowtie- and star-shape MoS2 twin-islands (high-symmetry poly-crystals with 60° lattice misorientation angles) under thermodynamic and or kinetic control conditions. Based on the comparison of the length of grain boundary and base edge, it is possible to distinguish the thermodynamic and kinetic control by measuring the aspect ratio of bowtie shape. The phase field model was also employed to simulate the growth of MoS2 and symmetric shape evolution . Successfully growth of dendrites MoS2 is demonstrated by pretreating substrates with adhesive tapes and controlling S:Mo vapor ratio. The successive nucleation of twin crystals at the side edges contributed to the sub-branch growth, and the accumulated sulfur vacancies in cyclic twin regions lead to strong and localized enhancement of PL emission, determined the shape dependency of optical property .
Recent progress of 2D TMDs materials brings lots of advances and opportunities in the scientific community with numerous concepts and technologies. There have been many breakthroughs in the synthesis of TMDs layers by CVD techniques in the past several years. In this review, we analyze the possibility of controllable growth of 2D TMDs by CVD method based on the discussion of growth routes and mechanisms. The control of grain size, boundaries, orientation and morphology are highlighted, aiming to bring inspiration to future research in this field.
Although the latest published researches have successfully achieved the growth of high quality inch-size TMDs, it is still challenging to realize the controllable growth of wide range of TMDs with desired layer number, large domain size, target orientation and morphologies. One of the most important reason is that most of the precursors of TMDs are solid-state in common CVD growth system, except MOCVD. Unlike gas sources for graphene, it is difficult to control and maintain the concentrations of precursors precisely over whole growth process. Additionally, by using inductively coupled plasma enhanced CVD, graphene can be synthesized at temperature as low as 300 °C, but it is still challenging to grow TMDs at such low temperature. These show the importance of development of new CVD system, such as using external heating equipment, or introducing additives to lower melting points and reaction barriers. Meanwhile, suitable analytical model combined with simulations and calculations should be further developed to reveal the growth mechanism and set reliable theoretical predictions to control the growth experimentally.
On the other hand, 2D TMDs layers are promising materials for different kinds of electronics and optoelectronics devices. Although most of the TMDs based on VIB group metal, like MoS2, WS2, MoSe2 and WSe2 have widely been synthesized by CVD method, the growth of other novel layered materials may open up the possibility to explore the applications of 2D materials. Furthermore, the defects engineering, grain boundaries and phase transitions of TMDs display tremendous opportunity for specific area of applications. Additionally, we mainly focused on the synthesis of binary compounds in this review, but it is worth noting that the alloying of semiconductors and construction of heterostructures are ideal ways to tailoring the band structure of TMDs. Hence, the design and preparation of novel TMDs heterostructures as well as alloys is also important aspects to create new practical applications. Some other issues, such as the direct growth on flexible substrates or a successful method to transfer the TMDs on the target substrate after growth is necessary for the fabrication of most electronic devices. Therefore, considering the growth and application of 2D TMDs layers are still at the exploration stage, there are still numerous possibilities and strong demand to further understanding and developing the synthesis of 2D TMDs materials.
JWY, MDH and ZTL contributed to the preparation of the manuscript. All authors read and approved the final manuscript.
Miss Jiawen You received her B.S. degree in Applied Chemistry from Donghua University in 2016. Now she is pursuing her MPhil. degree under the supervision of Prof. Zhengtang Luo at Department of Chemical and Biological Engineering (CBE), Hong Kong University of Science and Technology (HKUST). Her current research interests mainly focus on the CVD growth of 2D materials and their heterostructures for optoelectronics.
Mr. Md Delowar Hossain received his B.Sc. and M.Sc. degree in Applied Chemistry and Chemical Engineering from University of Rajshahi, Bangladesh. Now he is pursuing his Ph.D. degree under the supervision of Prof. Tom Luo at CBE, HKUST. His research interests are the theoritical and experimental investigation to find the origin of catalysts activity in case of 2D material applied for different energy applications.
Prof. Zhengtang Luo is an Associate Professor in Hong Kong University of Science and Technology (HKUST). He earned his B.S. (1998) and M.S. (2001) degrees from South China University of Technology (SCUT), and a Ph.D. degree from University of Connecticut (2007). After working as a postdoctoral researcher at University of Pennsylvania (UPenn), he joined CBE, HKUST at 2012. His research mainly focuses on materials chemistry, materials physics and the nanofabrication of semiconductor nano-bioelectronics.
Technical assistance from the Materials Characterization and Preparation Facilities is greatly appreciated.
The authors declare that they have no competing interests.
Availability of data and materials
This project was supported by the Innovation and Technology Commission (ITC-CNERC14SC01), the Research Grant Council of Hong Kong SAR (Project Number 16204815), NSFC-RGC Joint Research Scheme (N_HKUST607/17).
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