In this study, carbon nanotube (CNT) purification results were compared between the conventional wet process using strong acids and the dry process using chlorine gas at high temperatures. To evaluate the effect of catalyst support in both methods, purification experiments were conducted using Tuball SWCNT from OCSiAl (without support) and CVD CNT synthesized with supported catalysts (Fe-Mo/MgO). Before and after treatment, the CNT samples were analyzed using scanning electron microscopy (SEM), Raman spectroscopy, and thermogravimetric analysis (TGA) to compare the morphology of CNT bundles, the distribution and content of impurities, and crystallinity. The results confirm that the dry process exhibited superior characteristics for both Tuball SWCNT and CVD CNT. In particular, changes in the IG/ID ratio observed in Raman spectroscopy and the reduction of residue in TGA clearly demonstrate high crystallinity and high-purity purification without damaging the CNTs. TGA reveals a reduction in ash content from 20.2 % to 3.2 % for Tuball SWCNT and from 63.1 % to 5.4 % for CVD CNT, while Raman spectroscopy confirms the preservation of the IG/ID ratio (~50) in Tuball SWCNT and its increase from 6.86 to 9.05 in CVD CNT. The purification method proposed in this study is expected to be effectively applied in fields requiring high-purity SWCNTs, such as electronics, sensors, and energy storage devices.
Carbon nanotube (CNT) fibers were synthesized in this study under a hydrogen atmosphere using the floating-catalyst chemical vapor deposition (CVD) technique. Acetone, ferrocene, and thiophene served as the sources of carbon, catalyst, and promoter, respectively. By adjusting the amount of thiophene, the sulfur molar ratio in the CVD reactor was varied to study its impact on the morphology and composition of the CNT fibers. Raman and TEM analyses showed that the structural properties of the CNTs, especially the production of single-walled CNTs (SWCNTs) with a high Raman IG/ ID ratio of approximately 23.8, can be finely tuned by altering the sulfur content, which also affects the accumulation of spherical carbonaceous particles. Moreover, it was established that the electrical conductivity of the CNT fibers is significantly influenced by their specific components—SWCNTs, multi-walled CNTs (MWCNTs), and spherical carbonaceous particles. The ratios of these components can be adjusted by modifying the molar ratios of catalyst and promoter in the precursor mixture. Remarkably, SWCNTs with enhanced crystallinity were found to substantially improve the electrical conductivity of the CNT fibers, despite the presence of numerous spherical carbon impurities.
The inclusion of conductive carbon materials into lithium-ion batteries (LIBs) is essential for constructing an electrical network of electrodes. Considering the demand for cells in electric vehicles (e.g., higher energy density and lower cell cost), the replacement of the currently used carbon black with carbon nanotubes (CNTs) seems inevitable. This review discusses how CNTs can contribute to the development of advanced LIBs for EVs. First, the reason for choosing CNTs as a conducting agent for the cathode is discussed in terms of energy density. Second, the reinforcing effect of CNTs on the anode is described with respect to the choice of silicon as the active material. Third, the development of water-based cathode fabrication as well as dry electrode fabrication with aid of CNTs is discussed. Fourth, three technical hurdles, that is, the price, dispersion issue, and entrapped metal impurities, for widespread use of CNTs in LIBs are discussed.
In this study, Fe–Mo–MgO catalysts for the synthesis of carbon nanotubes (CNTs) were prepared using the combustion method and CNTs were synthesized through catalytic chemical vapor deposition. The combustion time was controlled to 0.5, 1, 2, 3, 5, 10, and 24 h in the catalyst preparation stage. The residual carbon contents after the combustion stage and the morphologies of synthesized CNTs were also analyzed. The diameter, yield, and crystallinity of the synthesized CNTs were found to remarkably vary according to the combustion time in the catalyst preparation process. The amount of residual carbon in the catalyst considerably affects the purity, crystallinity, diameter and its distribution, and wall number of CNTs. Based on the yield and crystallinity, CNTs synthesized using the catalyst with a combustion time of 3 h were determined to be the most appropriate for application in field emitters
Free-standing hybridized electrode consisting of double-walled carbon nanotubes (DWNTs) and activated carbon have been fabricated for flexible supercapacitor applications. The xanthan-gum, used in our methodology, showed high ability in dispersing the strongly bundled DWNTs, and was then effectively converted to activated carbon with large surface area via chemical activation. The homogeneously dispersed DWNTs within xanthan-gum derived activated carbon acted as both electrical path and mechanical support of electrode material. The hybridized film from highly dispersed DWNTs and activated carbon was mechanically strong, has high electrical conductivity, and exhibited high specific capacitance of 141.5 F/g at the current density of 100 mV/s. Our hybridized film is highly promising as electrode material for flexible supercapacitors in wearable device.
Among various methods to produce graphene sheets, electrochemical exfoliation has been regarded as an effective method for the mass production of high-quality graphene sheets because of its simplicity and environmental friendliness. However, conventional electrochemical exfoliation has a disadvantage of accumulating intercalating ions at graphite interlayers owing to the use of a constant voltage. In this study, we developed a DC switching technique to achieve more efficient intercalation of ions than that in the conventional method. In the DC switching method, positive and negative voltages are successively applied to release the accumulated intercalating ions. By testing various conditions, we found the optimum switching time to produce high-quality graphene sheets with the highest yield rate and the highest electrical conductivity. As a result, the graphene sheets using this DC switching technique showed 85% higher yield rate, 193% higher electrical conductivity, 160% larger area, and 25% thinner thickness than those obtained when using a constant DC method. We believe that this DC switching technique can be used for large-scale production of high-quality graphene sheets.
In this paper, nitrogen-doped reduced graphene oxide(rGO) is obtained by thermal annealing of nitrogen-containing compounds and graphene oxide (GO) manufactured by modified Hummers' method. We use melamine as a nitrogen-containing compound and treat GO thermally with melamine at over 800 ~ 1,000℃ and 1 ~ 3 hr under Ar atmosphere. The electrical conductivity of doped rGO is measured by 4-point probe method. As a result, nitrogen contents on rGO are found to be in the range of 2.5 to 12.5 at% depending on the doping conditions after thermal annealing. The main doping site on graphene oxide is changed from pyridinic-N and pyrrolinic N to the graphitic site as the heat treatment temperature increases. The electrical conductivity of doped rGO increases as the N doping content increases. As the thermal treatment time increases, the change of both total doping contents and doping sites is slight and the surface resistance is remarkably reduced, which is caused by healing effects of doped graphene oxide at high temperature.
Poly(vinylidene chloride) (PVDC)-derived nanoporous carbons were prepared by various activation methods: heat-treatment under an inert atmosphere, steam activation, and potassium hydroxide (KOH) activation at 873, 1073, and 1273 K. The pore structures of PVDC-derived nanoporous carbons were characterized by the N2 adsorption technique at 77 K. Heat treatment in an inert atmosphere increased the specific surface area and micropore volume with elevating temperature, while the average micropore width near 0.65 nm was not significantly changed, reflecting the characteristic pore structure of ultramicroporous carbon. Steam activation for PVDC at 873 and 1073 K also yielded ultramicroporosity. On the other hand, the steam activated sample at 1273 K had a wider average micropore width of 1.48 nm, correlating with a supermicropore. The KOH activation increased the micropore volume with elevating temperature, which is accompanied by enlargement of the average micropore width from 0.67 to 1.12 nm. The average pore widths of KOH-activated samples were strongly governed by the activation temperature. We expect that these approaches can be utilized to simply control the porosity of PVDC-derived nanoporous carbons.