The electrochemical cycling was carried out between 1.5 and 3.0 V in C/10 rate for the initial three cycles and thereafter C/2 (1 C = 1,675 mA g−1 of sulfur). Results and discussion The pyrolytic decomposition of Fe-Pc and its adhesion on the spherical silica with a high surface area were described in Figure 1. The thermal decomposition of metal-phthalocyanine and other related compounds has been well studied before, especially to produce a nitrogen-doped graphitic carbon or carbon nano-tubes [18–21]. These were typically applied to fuel cells or metal air cells as an efficient oxygen reduction catalyst on the cathode [21, 22]. The decomposition of Fe-Pc occurs around
500°C to 600°C, where the ring starts to open to form an intermediate species which interacts with the adjacent silica surface, resulting in a selleck chemicals thin layer of the poorly ordered nitrogen-doped carbon on the surface at 600°C [23]. Around 900°C, the nitrogen contents of the carbon layer decrease, and the crystallinity of the graphene layers increases due to the catalytic act of metallic Fe nanoparticles. It is well known that the graphitic carbon from the decomposition of metal-phthalocyanine typically contains approximately 1% to 8% of nitrogen contents [22, 24]. Especially, Fe-Pc is known as an efficient carbon source for SCH727965 mouse producing a highly graphitic
carbon, where its Fe particles in the Metalloexopeptidase final product can be easily removed by simple acid leaching. Figure 2a,b shows the scanning electron microscope
(SEM) and transmission electron microscope (TEM) images of the mono-dispersed GHCS synthesized in this work. The diameter of these carbon spheres is around 460 to 480 nm which is just a little smaller than the size of the original silica sphere, and the wall thickness is less than 10 nm. From the N2 isotherm at 77 K (Figure 3), the BET surface area was measured to be 297 m2 g−1, and the pore size distribution deduced from the Barret-Joyner-Halenda algorithm indicates the presence of mesopores about 3.7 nm on the wall (Figure 3 inset). These pores can act as pathways for the impregnation of sulfur into the interior when sulfur/carbon nano-composite is formed [4, 12]. The graphitic nature of this wall was investigated by analyzing the XRD pattern and Raman spectra in Figure 2c,d respectively. The XRD pattern shows distinct (002) and (101) planes, and the full width at half maximum (FWHM) for (002) plane is 1.25°, which indicates the Vistusertib order formation of nano-crystallite with coherent length of 6.5 nm. The Raman spectrum shows D and G bands at 1,350 and 1,580 cm−1, respectively. They were deconvoluted using commercial software (IgorPro™, WaveMetrics, Inc., Lake Oswego) by fitting to Lorentzian functions. The ratio of the FWHM to D and G peaks is calculated to be 2.84 which is a much higher value than that for the carbon made from sucrose (2.