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Chemical Vapour Deposition PRIMER Chemical vapour deposition Luzhao Sun 1,2, Guowen Yuan3, Libo Gao3 ✉ , Jieun Yang4, Manish Chhowalla4 ✉ , Meysam Heydari Gharahcheshmeh 5, Karen K. Gleason5 ✉ , Yong Seok Choi6,7,8, Byung Hee Hong6,7,8 ✉ and Zhongfan Liu 1,2 ✉ Abstract | Chemical vapour deposition (CVD) is a powerful technology for producing high-quality solid thin films and coatings. Although widely used in modern industries, it is continuously being developed as it is adapted to new materials. Today, CVD synthesis is being pushed to new heights with the precise manufacturing of both inorganic thin films of 2D materials and high-purity polymeric thin films that can be conformally deposited on various substrates. In this Primer, an overview of the CVD technique, including instrument construction, process control, material characterization and reproducibility issues, is provided. By taking graphene, 2D transition metal dichalcogenides (TMDs) and polymeric thin films as typical examples, the best practices for experimentation involving substrate pretreatment, high-temperature growth and post-growth processes are presented. Recent advances and scaling-up challenges are also highlighted. By analysing current limitations and optimizations, we also provide insight into possible future directions for the method, including reactor design for high-throughput and low-temperature growth of thin films. Chemical vapour deposition (CVD) is a widely used reactions or diffuse directly through the boundary layer materials processing technology in which thin films to the substrate. In both cases, the reactant gases and the are formed on a heated substrate via a chemical reac- intermediate reactants adsorb onto the heated substrate tion of gas-phase precursors. In contrast to physical surface and diffuse on the surface. The subsequent heter- vapour deposition methods, such as evaporation and ogeneous reactions at the gas–solid interface lead to con- sputtering, CVD offers a clear advantage by relying on tinuous thin film formation via nucleation, growth and chemical reactions that enable tunable deposition rates coalescence as well as formation of reaction by-products. as well as high-quality products with excellent confor- Finally, any gaseous products and unreacted species desorb mality. The greater demand for semiconductor thin films from the surface and are carried away from the reaction starting after World War II was the initial driving force zone. The gas-phase reactions occur when the tempera- for rapid development of CVD technology1–5. Recently, ture is sufficiently high or additional energy is introduced, low-dimensional materials such as carbon nanotubes, for example, in the form of plasma. In addition, the het- graphene and 2D transition metal dichalcogenides erogeneous reaction is essential if the deposition reaction (TMDs) have injected new vitality into the electronics relies on the surface catalysis of the underlying substrate, industry6–8 and introduced more stringent requirements such as in the case of the catalytic growth of graphene on for successful CVD of these materials with high purity a metal surface. and fine structure. CVD allows the tuning of the struc- In this Primer, we first provide an overview of the tures and properties of the resulting products9,10, and var- CVD instrumentation set-up before describing best ious advanced CVD systems and their variants have been practices for material preparation and characterization. developed, such as plasma-enhanced CVD2 and metal– The growth of graphene on metal and dielectric sub- organic CVD (MOCVD)4 (BOx 1). Usually, CVD does not strates are taken as representative examples of catalytic require high-vacuum working environments, making it CVD and non-catalytic CVD processes, respectively. a popular technology for electronics, optoelectronics, We then demonstrate the flexibility of this method by surface modification and biomedical applications. discussing important applications of CVD, including ✉e-mail: [email protected]; Irrespective of the variations in CVD types, the fun- growth of binary and ternary 2D materials and poly- [email protected]; damental process is similar and consists of the follow- meric thin films. We also highlight recent progress and [email protected]; 11,12 (Fig. 1) [email protected]; ing common elementary steps . First, the reactant challenges when scaling-up this technology, an impor- [email protected] gases are transported into the reactor. These reactant gases tant aspect of CVD when applied to industry. Finally, https://doi.org/10.1038/ then either undergo gas-phase reactions to form interme- we discuss what affects experimental reproducibility, s43586-020-00005-y diate reactants and gaseous by-products via homogeneous the current limitations of the technique and future NATURE REVIEWS | METHODS PRIMERS | Article citation I­D: (2021) 1:5 1 0123456789(); PRIMER Author addresses Mass flow controllers are essential for the gas supply, where the gas flow rate is automatically set via feedback 1 Center for Nanochemistry, Beijing Science and Engineering Center for Nanocarbons, control according to the mass of flowing gas. Liquid Beijing National Laboratory for Molecular Sciences, College of Chemistry and Molecular source reactants are delivered by ‘bubbling’ a carrier gas Engineering, Peking University, Beijing, China. controlled by the mass flow controller13,14 (Fig. 2b). Solid 2Beijing Graphene Institute, Beijing, China. 3National Laboratory of Solid State Microstructures, School of Physics, Collaborative source precursors that are less volatile are introduced Innovation Center of Advanced Microstructures, Nanjing University, Nanjing, China. to the reaction chamber by dissolution in a suitable 15 16–22 4Department of Materials Science and Metallurgy, University of Cambridge, solvent or by sublimation into the gas phase . Cambridge, UK. 5Department of Chemical Engineering, Massachusetts Institute of Technology, Reaction chamber. The horizontal23,24 (Fig. 2a) and verti- Cambridge, MA, USA. cal25,26 (Fig. 2c–e) configurations are the two main config- 6Graphene Research Center, Advanced Institute of Convergence Technology, urations of the reaction chamber (BOX 1). The reaction Suwon, Korea. chamber itself is usually a quartz tube, widely employed 7 Department of Chemistry, Seoul National University, Seoul, Korea. in semiconductor manufacturing because of its tolerance 8Graphene Square Inc., Suwon, Korea. to high temperatures and to rapid heating and cooling. A gas inlet injector is connected to the chamber using a developments of CVD together with exploration of metal flange, which is fitted with cooling components. new materials. To guarantee that the gas flow is laminar, a gas distribu- tor with through-holes is usually employed23,25 (FIG. 2c–e). Experimentation The substrate is usually located on a substrate holder To obtain high-quality thin films by CVD, suitable (also known as a ‘boat’ or ‘susceptor’) composed of quartz equipment is needed, and custom-built systems pro- or graphite because of their good chemical stability and vide the flexibility of operation often desired by CVD high-temperature resistance23,27,28. In order to meet the researchers. In this section, we discuss a series of designs target deposition characteristics (thickness, composition that satisfy the requirements of materials synthesis, and so on),the configuration of the substrate holder and including the heating methods, gas-flow control, the the deposition conditions (total gas flow, gas composi- loading of substrate and so on. In addition, the growth tion, temperature, pressure and so on) must be optimized parameters, including substrate, temperature, atmos- via experimental and numerical process engineering phere, pressure and so on, are essential for controlling studies23,25,26,29,30. In manufacturing applications, a cool- the quality of as-grown materials as well as the reaction ing chamber with a loading/unloading subsystem is rate (growth rate). Here, we will introduce CVD growth necessary to improve the productivity. of graphene following the procedure of substrate pre- treatment, heating, annealing, high-temperature growth Vacuum system. Purging the deposition chamber to and cooling. start the deposition process and obtaining the neces- sary pressure for transport of the reactants relies on the CVD equipment vacuum system, where measurement and control of A CVD system must meet the following basic require- the vacuum are essential and complement one another. ments: delivery of the gas-phase reactants in a control- To measure the pressure of the vacuum system, various lable manner; provision of a sealed reaction chamber; gauges are alternated: the Bourdon gauge, piezo sensor, evacuation of the gases and control of the reaction capacitance manometer and diaphragm manometer are pressure; supply of the energy source for the chemical the main mechanical gauges, which can measure the reactions; treatment of the exhaust gases to obtain safe vacuum by detecting physical changes in the strain or and harmless levels; and automatic process control to electrical capacitance, for example. The Bourdon gauge improve the stability of the deposition process. Figure 2 is inexpensive and has a long life, but it does not have shows a typical CVD system consisting of a gas deliv- an electronic output, and so is not suitable for feed- ery system, a reaction chamber, a vacuum system, an back control (Fig. 2f). Using a capacitance manometer, a energy system, an exhaust gas treatment system and measurement range of
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