Task 3.1 The electronic structure of the materials was evaluated, optimized, and presented an excellent photocatalytic activity by studying the optical properties and assessing the energy of the forbidden band.
Task 3.2 The following methods synthesized the TiHO powders: by the synthesis of titanium dioxide by the sol-gel method, followed by heat treatment at temperatures between 400 and 800°C, to control the crystalline phases of anatase and rutile, then chemical reduction with sodium borohydride, to obtain the black TiO2 powder which shows defects of Ti3+ and oxygen vacancies. Also, at this stage, a new method of obtaining TiHO started by oxidizing TiH2 with H2O2.
Task 3.3 - Material characterization: XRD analysis (crystallinity, structure, phase composition, crystallite size), SEM-EDX analysis (morphology, elemental analysis), insulating point (pHzpc), BET specific surface area. The impact on the environment has been achieved through nanomaterial toxicity studies on green algae Chlorella Vulgaris.
Task 3.4 - Synchrotron measurements, for which we submitted a project “Defective black titanium oxide nanomaterials for high-efficiency photocatalysis” CERIC (proposal ID 20212076), which was funded, and the analyzes EPR, TEM and XRD for six samples (3 white TiO2 samples and 3 black TiO2 samples) were performed at NIMP - National Institute for Materials Physics.
Task 3.5 The photocatalytic activity of the materials synthesized by UTBV and IFE was investigated by studying the degradation efficiency of imidacloprid (IMD-pesticide) and amoxicillin (AMX-antibiotic), but also mineralization tests of pollutants by investigating TOC and TN in especially for AMX photodegradation tests.
Tasks 3.6 and 3.7 Dissemination of results and communication between project partners was achieved through the online project meeting that took place on October 26, 2021, the visit between 31.10-5.11.2021 of the project director Prof Andronic Luminita to the IFE project coordinator, Norway, participating with a guest paper at an online international school, publishing 2 ISI articles and preparing another 2 articles in collaboration with IFE, LEI.
The influence of TiO2:NaBH4 ratio on the black TiO2 synthesis: A convenient and low-cost method for producing black TiO2 materials by chemical reduction of TiO2 with NaBH4, in proportions of 4: 1, 2: 1 and 1: 1, at a temperature 350°C and in an inert atmosphere of argon are investigated in the TESTIMONIES project.
SEM images of white TiO2 and black (B1, B2 and B3) powders
The elemental composition of white and black powders was analysed by EDS and XPS techniques. EDS technique obtains most of its signal from the depth of 1-2 µm and provides a more generalised composition of the powders. Whereas, XPS is a surface analysis technique and provides information only from the top 5-10 nm. Unfortunately, both methods can not warranty high quantitative precision. But their combination can provide valuable qualitative insights into the difference between the „bulk” and the top surface of the powders.
Elemental composition of powder samples.