Study on the reduction of highly porous TiO2 precursors and thin TiO2 layers by the FFC-Cambridge process

Reduction of porous titanium oxide precursors by the FFC-Cambridge process is reported in this paper. Porous TiO2 precursors were prepared by mixing the powder with different concentrations of graphite and polyethylene as fugitive agents and sintered at 1,073 K. The maximum porosity achieved before the mixture saturation was approximately 75%. After the electro-deoxidation by the FFC-Cambridge process, shrinkage of approximately 40% in volume and increase in porosity were observed, which might be due to atomic rearrangement, change of density and subsequent grain growth during reduction. The potential applied (below the decomposition potential of CaCl2) had a direct effect on the minimum level of oxygen achieved, which was approximately 3,000 ppm for 48 h at 3.00 V and the same level at half the time (24 h) when increasing potential to 3.15 V. On the other hand, thin layers (300 μm thickness) screen-printed on titanium foils showed shorter reduction time than that observed for thicker porous pellets. This led to the conclusion that cathode geometry (porosity and thickness of the pellet) might have an effect on the rate of reduction by increasing the surface area available and improving the mass diffusion of oxygen ions.