br Geometrical construction and intrinsic features
3.2. Geometrical construction and intrinsic features of wrinkled [email protected]–C
Morphological and topographical overview of the [email protected]–C was in-vestigated by field-emission scanning electron microscopy (FE-SEM). As shown in Fig. 1A, a high yield of spherical carbon was formed with homogenous carbon dispersion and formally aligned spheres with varied sizes. Fig. 1A clearly shows the 3D round spheres. Diﬀerent carbon sphere sizes that ranged from 1 μm to 5 μm formed and may have self-assembled without capping agents. Figs. 1B and C show low magnification of [email protected]–C. The S–C microspheres appeared and were low bright than the bump mapping spheres because of the successful decoration of S–C with Ru°. Fig. 1D shows the 3D spheres of S–C dense dressed by Ru° and exhibiting homogeneous nanoparticle distribution. The well-dispersed Ru particles at the entire S–C microsphere surfaces
Scheme 1. Formation of spherical sulfur-doped carbon after successive condensation of glucose and thiourea, then calcined at 800 °C under N2 Relebactam for complete carbonization. Reduction of Ru3+ ions at S-C microspheres upon stepwise addition of aqueous solution of 0.1 M NaBH4 as a reducing agent leads to formation of [email protected] The Ru NPs homogeneously loaded at the S-C-surface like bump mapping networks, which open the high eﬃcient catalytic activity of Ru for H2O2 detection with high sensitivity, and low detection limit.
led to produce (i) rough surfaces with a mount of protrusions, (ii) in-terfacial voids-like caves, and (iii) nano-buds/bumps, which are well-dispersed along the surface mapping network without disturbing the spherical S-C core structures. These structural surface features enabled to create high eﬃcient catalytic activity of Ru/S-C catalysts for H2O2 monitoring assay with high sensitivity, and low detection limit (Scheme 1 & Fig. 1). The confirmation of particle size was illustrated by Fig. 1E and F, where the high magnification of the FE-SEM proceeded. The particle size was around 10 nm, and the particles exhibited homo-geneous dispersion at the S–C surface skin matrices. EDX-SEM was performed for the atomic dispersion of C, O, Ru, and S (Fig. 1H [i–iv]).
The homogeneous dispersions of C, O, Ru, and S were clearly illustrated at 72.28% C, 19.87% O, 0.2% Ru, and 7.65% S. The FE-SEM and EDX-SEM results showed the successful decoration of sulfur-doped carbon microspheres through the use of ruthenium nanoparticles and forma-tion of wrinkled spheres of [email protected]–C.
Further confirmations of the decoration of well-defined RuNPs (5–15 nm) along the entire surfaces of the S-C microspheres were illu-strated by HR-TEM. Fig. 2A shows the STEM-DF image of the concentric [email protected] microspheres. The spherical [email protected] with size of 2.1–2.5 μm diameter was observed. The wrinkled RuNPs distributions at the sur-faces of S-C spheres are stabilizing selection clearly illustrated and further confirmed by the
Fig. 1. A) Low magnification of FE-SEM images for S-C obtains the spherical formation of S-doped carbon after calcination at 800 °C. B) The FE-SEM image at low magnification with obtains the brightness of the formed spheres as a result of dressing the spheres by Ru. C–G) gradual magnification of [email protected] obtains the homogeneous dispersion of Ru at the surface of sulfur-doped carbon microspheres. E&G) shows the dressing of the S-CMS surface with Ru° and the average size ranged from 5 to 15 nm. H) The EDX-SEM mapping shows the atomic distribution and percentage of C (H-a), O (H-bI), Ru (H-c), and S (H-d) for [email protected]
The distributions of surface pores were evident in N2-adsorption
isotherms. Figure S1 A shows the N2 adsorption isotherms for S–C and [email protected]–C, which both presented types I and IV isotherms with H3 hysteresis loops at relative pressure (P/P0) between 0.2 and 0.8, characteristic of the microporous and mesoporous structures [35–38]. The pore size distributions obtained through the NLDF (Fig. S1B) were 1.7 and 11 nm for S–C and [email protected]–C, respectively. The pore size dis-tribution in the S–C changed from microporous to mesoporous owing to the formation wrinkled microsphere surfaces and presence of pre-dominant mesoporous Ru [39–41]. Furthermore, the BET surface areas of S–C and [email protected]–C were 209 and 22.6 m2 g−1, respectively. The sharp decrease of the surface area of S–C may be attributed to the binding of 10 nm Ru into the pores of S–C and successful decoration to the outer spherical surface of the S–C microspheres.