In this research we investigated the in situ formation mechanism of NbC in mechanically alloyed Fe-Nb-C mixture. Powders of iron, niobium and graphite with a composition Fe-20 %Nb was milled in a planetary mill for various milling times (i.e. 5, 10, 15 and 20 h) to investigate the influence of this variable on phase formation and properties of composite. The mixture was cold pressed and sintered at 1300°C for 1 h. Only phase of the initial raw materials was observed after milling, whilst NbC phase was detected after sintering. Increasing the milling time resulted in an increase in crystallite size and strain energy, which is beneficial for hardness and density improvement.
An anodic film with a nanoporous structure was formed by anodizing niobium at 60 V in fluorinated ethylene glycol (fluoride-EG). After 30 min of anodization, the anodic film exhibited a "pore-in-pore" structure; that is, there were smaller pores growing inside larger pores. The as-anodized film was weakly crystalline and became orthorhombic Nb2O5 after heat treatment. The energy band gap of the annealed nanoporous Nb2O5 film was 2.9 eV. A photocatalytic reduction experiment was performed on Cr(VI) under ultraviolet (UV) radiation by immersing the nanoporous Nb2O5 photocatalyst in a Cr(VI) solution at pH 2. The reduction process was observed to be very slow; hence, ethylenediaminetetraacetic acid (EDTA) was added as an organic hole scavenger, which resulted in 100% reduction after 45 min of irradiation. The photocatalytic reduction experiment was also performed under visible light, and findings showed that complete reduction achieved after 120 min of visible light exposure.
In this study, nanoporous anodic film was produced by anodization of niobium, Nb in a fluoride ethylene glycol electrolyte. The effect of anodization voltage and electrolyte temperature was studied to find an optimum condition for circular, ordered, and uniform pore formation. The diameter of the pores was found to be larger when the applied voltage was increased from 20 to 80 V. The as-anodized porous film was also observed to comprise of nanocrystallites which formed due to high field-induced crystallization. The nanocrystallites grew into orthorhombic Nb2O5 after post-annealing treatment. The Cr(VI) photoreduction property of both the as-anodized and annealed Nb2O5 samples obtained using an optimized condition (anodization voltage: 60 V, electrolyte temperature: 70 °C) was compared. Interestingly, the as-anodized Nb2O5 film was found to display better photoreduction of Cr(VI) than annealed Nb2O5. However, in terms of stability, the annealed Nb2O5 presented high photocatalytic efficiency for each cycle whereas the as-anodized Nb2O5 showed degradation in photocatalytic performance when used continually.