Fabrication of Si/N-doped carbon nanotube composite via spray drying followed by catalytic chemical vapor deposition (2023)


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Journal of Alloys and Compounds

Available online 6 January 2023

, 168743

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Developing an effective structure for the silicon-carbon composite that promotes electric-ionic conductivity and reduces the volume change is a key issue for Si-based anode. In this study, spherical granules comprising silicon nanoparticles (Si-NPs) grafted with nitrogen-doped carbon nanotubes (Si-NCNTs) are fabricated via spray drying followed by catalytic chemical vapor deposition (CCVD). The initial discharge and charge capacities of the Si-NCNTs are 2,457 and 1,820mAh g−1, respectively. The Si-NCNTs shows a capacity retention of 57% after 200 cycles as well as improved rate capability when compared to the Si-NPs and commercial CNTs composites (Si-CNTs) fabricated via spray drying alone. The Li+ ion-diffusion-coefficient (DLi+) of the Si-NCNTs is approximately ~three times larger than that of the Si-CNTs at critical lithiation potential. The NCNTs that form the interconnections between Si-NPs play the role of electrically conductive buffers that could accommodate the volume change produced and favor Li+ ion transport.


The conventional lithium-ion batteries (LIBs) comprising lithium transition metal oxide and graphite as cathode and anode based on intercalation reactions, respectively, are reaching their limit of energy density [1], [2], [3]. Therefore, numerous efforts have been made to achieve a breakthrough in overcoming limitations with regard to energy density by combining these materials with anode materials that can form alloys [4], [5], [6], [7], [8]. Among these anode materials, silicon (Si) which has a high theoretical capacity (close to 4,000mAh g−1) is a promising candidate as an alternative to graphite used in the conventional anode of LIBs. However, Si generally suffers from intrinsic drawbacks such as low electrical conductivity and significant volume changes during alloying and dealloying with Li, which results in the pulverization and swelling-induced deformation of the electrodes [9], [10], [11], [12], [13].

The co-utilization of carbonaceous materials and Si has been considered the most suitable approach for the conventional LIBs to achieve high energy density with Si [14], [15], [16]. Much research has been conducted on the preparation of the Si/carbon composite using highly electrically conductive crystalline carbon such as graphite, graphitic carbon, graphene, and carbon nanotubes (CNTs) [16], [17], [18], [19], [20], [21]; various methods have also been used to prepare the composite [13], [15], [17], [22], [23]. The spray drying process is widely applied to produce Si/carbon composite particles because the process is simple and continuous as well as capable of producing spherical particles which could have high tap density [24], [25], [26], [27], [28]. In addition, since the graphene and CNTs are flexible, spherical Si/CNTs or Si/graphene composites can be prepared through the spray drying process [29], [30], [31], [32], [33]. However, it is difficult to effectively achieve high degrees of dispersion and contact between carbonaceous materials and silicon due to the density difference between silicon and carbonaceous materials [34].

Among the carbonaceous materials, CNTs have many advantages due to their high electrical conductivity, mechanical flexibility and chemical stability [35], [36], [37]. Low-dimensional structured materials, such as CNT, have been developed for improved electrochemical properties [38], [39]. The low dimensional structures have shown fast electron transfer and shortened lithium diffusion pathway due to their large surface area. Park et al. prepared the Si/CNT/C composite using the spray drying process. To improve contact between Si and CNTs, amorphous carbon was introduced in the Si/CNT composite [20]. However, low electrical conductivity could hinder Li+ ion and electron transport across the amorphous carbon created from sucrose. Han et al. used copper silicide as a mechanical matrix to integrate Si and CNTs using the spray drying process followed by high-temperature carbonization processes [40]. Copper silicide successfully contributed to improving cycling stability owing to its good mechanical strength. However, the undesirable capacity loss brought about by the electrochemically inactive copper silicide, and its insufficient dispersion among Si and CNTs remained unsolved. When it comes to fabricating Si/CNTs composite materials, it is important to avoid contact among Si particles which would induces local volumetric deformation during lithiation and delithiation. CNTs connecting every single Si particle could play the role of a buffer preventing volume expansion, and additionally could contribute to a better rate performance through its superior electrical conductivity. Furthermore, substitutional doping of nitrogen in the lattice of CNT is known to increase the rate capabilities by contributing free electrons to the conduction band [41].

In this study, Si aggregates with the catalyst uniformly distributed for the growth of nitrogen-doped CNTs (NCNTs) were first fabricated via the spray drying method. Next, the aggregates were post-treated by the catalytic chemical vapor deposition (CCVD) method where the NCNTs produced are dispersed in the composite as the electrical bridges, to form silicon nanoparticles grafted with nitrogen-doped carbon nanotubes (Si-NCNTs). The structure and properties of the carbonaceous materials converted from various carbon sources are very important in electrochemical fields [42], [43]. In this study, the NCNTs were grown on the internal and external surfaces of the Si aggregates using the CHx and NHx gases formed by the decomposition of dicyandiamide. The Li-ion cell applied with the Si-NCNTs showed highly improved capacity retention (57% after 200 cycles) and rate capability (48% at 3Ag−1) compared to Si-CNTs (under 50% within 31 cycles and 22.5% at 3Ag−1, respectively).

Section snippets

Sample preparation

The Si-NCNTs powders were fabricated via the spray drying process followed by CCVD (Fig. S1). The precursor solution was prepared by dissolving 0.01M nickel nitrate hexahydrate (Samchun, 98%) in 200mL of distilled water, the reduced phase of which serves as a seed for the growth of NCNTs. 1g of silicon nanoparticles (NanoAmor, ~100nm) were then dispersed in the solution with vigorous stirring by a magnetic stirrer at a rotating speed of 600rpm to assist their wetting and dispersion. The

Results and discussions

The mechanism of formation of the Si-NCNTs composite synthesized by the spray drying and post-treatment is illustrated in Scheme 1. In the first step, as the spray solution passes through the tip of the twin-fluid atomizer of the spray dryer, the compressed air induces it to split into droplets and travel through the cylindrical drying chamber; the cruising droplets which contain silicon nanoparticles and dissolved nickel nitrate undergo volume precipitation and desiccation. The drying of the


In this study, spherical granules comprising silicon nanoparticles grafted with nitrogen-doped carbon nanotubes are fabricated via spray drying followed by CCVD. The nitrogen-doped CNTs are highly dispersed in the composite and connect every single primary Si particle, providing sufficient electrical contact to the Si particle and buffer for the volumetric expansion of Si. The Li+ ion cells with Si-NCNTs showed high reversible capacity (1,820mAh g−1) as well as superior capacity retention (57%

CRediT authorship contribution statement

Hyemin Kim; Conceptualization, Data curation, Methodology, Investigation. Seongmin Shin; Methodology, Investigation. Dae Soo Jung; Data curation, writing, Jung Hyun Kim; Supervision, Writing – review & editing

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.


This work was supported by the “Policy R&D program” funded by the Korea Institute of Ceramic Engineering and Technology, Republic of Korea (KPP21008). This work was supported by the Technology Innovation Program (20009985) funded by the Ministry of Trade, Industry & Energy.

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    How carbon nanotubes are synthesized by catalytic chemical vapor deposition? ›

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    Carbon nanotubes for thin film transistors are usually synthesized by thermal CVD or plasma-enhanced chemical vapor deposition (PECVD). Floating catalyst chemical vapor deposition (FCCVD) is also an alternative for CNT growth.

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    Arc Method

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    One of the best techniques for the production of CNTs is chemical vapor deposition (CVD). There are different CVD techniques such as catalytic chemical vapor deposition either thermal [33] and water assisted [6], plasma enhanced oxygen assisted CVD [34, 35, 36] or hot filament CVD (HFCVD) [37].

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    The four most adopted methods of synthesis of single crystals are solid-state, hydrothermal, slow evaporation at room temperature, and flux methods.

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    About 1.0 g of soot was taken in 200 ml of concentrated nitric acid in 250 ml R.B. flask. The mass was sonicated for 15 min and then heated at 85°C on an oil bath with continuous stirring for 12 h. After this, the reaction mass was cooled to room temperature and diluted to its double mass by DI water.


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