Solid solutions of scandium in anatase as semiconductor material for DSSC photoanodes were prepared by the controlled hydrolysis of titanium(IV) isopropoxide and scandium(III) isopropoxide in hydroalcoholic medium. The final powder was constituted by mesoporous anatase beads doped with Sc. A superstructure characterizes the beads, which are spherical at the microscopic level (approximate to 650 nm) and rice-grain-shaped at the nanoscopic level (approximate to 20 nm). The BJH pore size distribution and BET surface area of the powder beads were found depending from the Sc content ranging the peak of the former between 7 and 25 nm and between 65 and 128 m(2) g (-1) the latter. Data obtained by XRD and EXAFS confirm that we are dealing with real solid solutions with Sc-Ti. substitution defects. The electronic properties of the synthesized semiconductor material as a function of Sc doping were investigated by the measure of the flat band potential, band gap, and deep levels. In the range 0.0-1.0 at. % of Sc, the flat band energy changes from -4.15 to -4.07 eV, whereas the band gap height increases by 0.03 eV. The presence of Sc modifies heavily the cathodoluminescence spectrum of anatase at the lowest concentration too. Several DSSCs with photoanodes at different Sc doping were tested both under solar simulator and in the dark. The maximum efficiency of 9.6% was found at 0.2 at. % of Sc in anatase that is 6.7% higher with respect to the DSSCs with pure anatase
The thermodynamic quantities associated to the transformation from graphite to multiwalled carbon nanotubes (MWCNTs) were determined by electromotive force (emf) and differential scanning calorimetry (DSC) measurements. From the emf versus T data of galvanic cell Mo|Cr(3)C(2), CrF2, MWCNTs|CaF2 s.c.|Cr(3)C(2), CrF2, graphite|Mo with CaF2 as solid electrolyte, Delta(r)H(T) degrees= 8.25 +/- 0.09 kJ mol(-1) and Delta(r)S(T) degrees= 11.72 +/- 0.09 JK(-1) mol(-1) were found at average temperature T = 874 K. The transformation enthalpy was also measured by DSC of the Mn(7)C(3) formation starting from graphite or MWCNTs. Thermodynamic values at 298 K were calculated to be: Delta(r)H(298) degrees = 9.0 +/- 0.8 kJ mol(-1) as averaged value from both techniques and Delta(r)S(298) degrees approximately Delta(r)S(T) degrees. At absolute zero, the residual entropy of MWCNTs was estimated 11.63 +/- 0.09 JK(-1) mol(-1), and transformation enthalpy Delta(r)H(0) degrees approximately Delta(r)H(298) degrees. The latter agrees satisfactorily with the theoretical calculations for the graphite-MWCNTs transformation. On thermodynamic basis, the transformation becomes spontaneous above 704 +/- 13 K.
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