In this study, relationships between preparation conditions, structure, and activity of Pt-containing TiO2 photocatalysts in photoinduced reforming of glycerol for H2 production were explored. Commercial Aerolyst® TiO2 (P25) and homemade TiO2 prepared by precipitation-aging method were used as semiconductors. Pt co-catalysts were prepared by incipient wetness impregnation from aqueous solution of Pt(NH3)4(NO3)2 and activated by calcination, high temperature hydrogen, or nitrogen treatments. The chemico-physical and structural properties were evaluated by XRD, 1H MAS NMR, ESR, XPS, TG-MS and TEM. The highest H2 evolution rate was observed over P25 based samples and the H2 treatment resulted in more active samples than the other co-catalyst formation methods. In all calcined samples, reduction of Pt occurred during the photocatalytic reaction. Platinum was more easily reducible in all of the P25 supported samples compared to those obtained from the more water-retentive homemade TiO2. This result was related to the negative effect of the adsorbed water content of the homemade TiO2 on Pt reduction and on particle growth during co-catalyst formation.
Comparison of physicochemical properties and electrocatalytic behavior of different N-doped carbonaceous materials as potential catalysts for oxygen reduction reaction (ORR) was attended. Ball-milling of graphite with melamine and solvothermal treatment of graphite oxide, graphene nanoplatelets (GNP) with ammonia were used as preparation methods. Elemental analysis and N2 physisorption measurements revealed the synthesis of N-doped materials with strongly different morphological parameters. Contact angle measurements proved that all three samples had good wettability properties. According to analysis of XRD data and Raman spectra a higher nitrogen concentration corresponded to a smaller size of crystallites of the N-doped carbonaceous material. Surface total N content determined by XPS and bulk N content assessed by elemental analysis were close, indicating homogenous inclusion of N in all samples. Rotating disc electrode tests showed that these N-doped materials weremuch less active in acidic medium than in an alkaline environment. Although the presence of in-plane N species is regarded to be advantageous for the ORR activity, no particular correlation was found in these systems with any type of N species. According to Koutecky–Levich analysis, both the N-containing carbonaceous materials and the reference Pt/C catalyst displayed a typical one-step, four-electron ORR route. Both ball-milled sample with high N-content but with low SSA and solvothermally synthesized N-GNP with high SSA but low N content showed significant ORR activity. It could be concluded that beside the total N content other parameters such as SSA, pore structure, structural defects, wettability were also essential for achieving high ORR activity.