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Carbon nanomaterials such as graphene, carbon nanotube (CNT), and carbon nanofiber (CNF) have received tremendous attentions in the past two decades due to their extraordinary mechanical strength and thermal and electrical properties. Recently, it indicates that three-dimensional (3D) nanocarbon hybrids overcome the weakness of individual low-dimensional nanocarbon materials and exhibit unique properties among carbon nanomaterials. Efforts have thus been made to acquire synergistic integration of one-dimensional (1D) and two-dimensional (2D) carbon nanomaterials. Meanwhile, chemical vapor deposition (CVD) is a widespread and effective method of fabricating three-dimensional nanocarbon hybrids compared with other synthetic methods. In this case, a number of 3D nanocarbon hybrids are synthesized by using different precursors at diverse temperature, and the nanocarbon hybrids are expected to be a promising choice for various application areas in the future.

There has been continuous progress in the development of different synthesis methods to readily produce graphene at a lower cost. Compared with the other methods, chemical vapor deposition (CVD) is an effective and powerful method of producing graphene and has attracted increased attention during the last decade. In this way, we can obtain good uniformity with a multitude of domains, excellent quality, and large scale of the produced graphene. Meanwhile, it is also helping for large-area synthesis of single-crystal graphene. In the CVD method, precursors are typically absorbed on the surface followed by pyrolytic decomposition, which leads to the generation of absorption sites on the surface and promotes the growth of continuous thin films.

As a new carbon material in the twenty-first century, carbon nanotubes (CNTs) have excellent optical, electrical, magnetic, thermal, chemical, and mechanical properties. There are many synthesis methods to produce CNTs. Compared with other methods, chemical vapor deposition (CVD) is the most effective method that has broad prospects for large-scale control of CNTs in recent years due to its simple equipment, simple operation, and lower cost. In order to gain a comprehensive understanding of the controlling parameters about the formation of CNTs, this chapter reviews the latest progress in the preparation of CNTs by CVD from three of the most important influencing factors: carbon sources, catalysts, and substrates. Among them, the catalyst is the most influential factor for the morphology, structure, and properties of CNTs. It should be pointed out that many growth factors can control the particle size distribution, composition, and structure of the catalysts, such as catalyst substrate, metal transition components added, calcination temperature, etc.