Photoelectrochemical Properties of Annealed Anodic TiO2 Layers Covered with CuOx.

In this work, we present a systematic study on the influence of Cu2+ ion concentration in the impregnation solution on the morphology, structure, optical, semiconducting, and photoelectrochemical properties of anodic CuOx-TiO2 materials. Studied materials were prepared by immersion in solutions with different concentrations of (CH3COO)2Cu and subjected to air-annealing at 400 °C, 500 °C, or 600 °C for 2 h. The complex characterization of all studied samples was performed using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), reflectance measurements, Mott-Schottky analyses, and photocurrent measurements. It was found that band gap engineering based on coupling CuO with TiO2 (Eg~3.3 eV) is an effective strategy to increase the absorption in visible light due to band gap narrowing (CuOx-TiO2 materials had Eg~2.4 eV). Although the photoactivity of CuO-TiO2 materials decreased in the UV range due to the deposition of CuO on the TiO2 surface, in the Vis range increased up to 600 nm at the same time.

Photoelectrochemical Performance of Nanotubular Fe2O3-TiO2 Electrodes under Solar Radiation.

Fe2O3-TiO2 materials were obtained by the cathodic electrochemical deposition of Fe on anodic TiO2 at different deposition times (5-180 s), followed by annealing at 450 °C. The effect of the hematite content on the photoelectrochemical (PEC) activity of the received materials was studied. The synthesized electrodes were characterized by field emission scanning electron microscopy (FE-SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), Raman spectroscopy, diffuse reflectance spectroscopy (DRS), Mott-Schottky analysis, and PEC measurements. It was shown that the amount of deposited iron (ca. 0.5 at.%-30 at.%) and, consequently, hematite after a final annealing increased with the extension of deposition time and directly affected the semiconducting properties of the hybrid material. It was observed that the flat band potential shifted towards more positive values, facilitating photoelectrochemical water oxidation. In addition, the optical band gap decreased from 3.18 eV to 2.77 eV, which resulted in enhanced PEC visible-light response. Moreover, the Fe2O3-TiO2 electrodes were sensitive to the addition of glucose, which indicates that such materials may be considered as potential PEC sensors for the detection of glucose.

A Photoelectrochemical Sensor Based on Anodic TiO2 for Glucose Determination.

A simple photoelectrochemical (PEC) sensor based on non-modified nanostructured anodic TiO2 was fabricated and used for a rapid and sensitive detection of glucose. The anodic TiO2 layers were synthesized in an ethylene glycol-based solution containing NH4F (0.38 wt.%) and H2O (1.79 wt.%) via a three-step procedure carried out at the constant voltage of 40 V at 20 °C. At the applied potentials of 0.2, 0.5, and 1 V vs. saturated calomel electrode (SCE), the developed sensor exhibited a photoelectochemical response toward the oxidation of glucose, and two linear ranges in calibration plots were observed. The highest sensitivity of 0.237 µA µmol-1 cm-2 was estimated for the applied bias of 1 V. The lowest limit of detection (LOD) was obtained for the potential of 0.5 V vs. SCE (7.8 mM) with the fastest response at ~3 s. Moreover, the proposed PEC sensor exhibited relatively high sensibility, good reproducibility, and due to its self-cleaning properties, a good long-term stability. Interfering tests showed the selective response of the sensor in the presence of urea and uric acid. Real-life sample analyses were performed using an intravenous glucose solution, which confirmed the possibility of determining the concentration of analyte in such types of samples.