Hydrothermal Synthesis and Phase Formation Mechanism of TiO2(B) Nanorods via Alkali Metal Titanate Phase Transformation

Titanium dioxide (B phase) with 1-D structures was successfully fabricated via a hydrothermal method with a subsequent ion-exchange process and calcination. P25, titanium isopropoxide (TTIP), rutile and also anatase were used as Ti precursors in the alkali hydrothermal system. TTIP promoted an elongation of nanorod morphology whereas the other precursors produced short nanorod structures. The different types of titanium precursors did not have any influence on the phase transformation during the fabrication process. Na2Ti6O13 was the primary intermediate product after washing the hydrothermal sample. H2Ti3O7 was the secondary intermediate phase obtained following proton-exchange of Na2Ti6O13 in HNO3 solution. Finally, the TiO2(B) phase was the product of calcination of the secondary intermediate product at 400°C for 5 hr. A phase transformation mechanism is presented based on an investigation of products at each of the steps. The effects of the synthesis conditions on tailoring of the crystal morphology are discussed. The growth direction of the TiO2(B) nanorods was investigated by HR-TEM and SADP. Finally, the metastable phase of TiO2(B) was shown to be transformed to anatase during thermal treatment at temperatures higher than 400°C

Synthesis and characterization of a mixed phase of anatase TiO2 and TiO2(B) by low pressure chemical vapour deposition (LPCVD) for high photocatalytic activity

This project is concerned with enhancing photocatalytic activity by preparing a mixed phase of nano-sized TiO2. TiO2 thin films were synthesized by using Low Pressure Chemical Vapour Deposition (LPCVD). Titanium isopropoxide and N2 gas were used as the precursor and carrier gas respectively. The effects of reaction temperature, carrier gas flow rate and deposited area were studied. TiO2 thin films with nano-sized TiO2 particles were obtained under suitable conditions and SEM, TEM, powder XRD and Raman spectroscopy were employed to characterize the phase and physical appearance of synthesized materials. Preliminary results show that a dual phase (TiO2(B) and anatase) thin film nanopowder was successfully prepared by LPCVD with needle- and polygonal plate-shape crystallites respectively. This thin film deposit produced a preferred orientation of TiO2(B) needles in the [001] direction of average crystallite size 50-80 nm in length and 5-10 nm in width, whilst the crystallite size of anatase polygonal-plates was around 200 nm. The optimal LPCVD condition for preparing this mixed phase of TiO2 was 600°C with a 1 mL/s N2 flow rate

Synthesis and characterization of mixed phase anatase TiO2 and sodium-doped TiO2(B) thin films by low pressure chemical vapour deposition (LPCVD)

TiO2 thin films were synthesized using Low Pressure Chemical Vapour Deposition (LPCVD) onto glass substrates. Titanium isopropoxide (TTIP) and N2 gas were used as the precursor and carrier gas respectively. The effects of reaction temperature, carrier gas flow rate and deposited area were studied. SEM, TEM, powder XRD and UV-Vis and Raman spectroscopy were employed to characterize the phase and morphology of the synthesized materials. The results show that a dual phase (sodium-doped TiO2(B) and anatase) nanocrystalline thin film was successfully prepared by LPCVD with needle- and polygonal plate-shape crystallites respectively. At the interface with the substrate, the thin film deposit exhibited a preferred orientation of TiO2(B) needles in the [001] direction with an average crystallite size of 50-80 nm in length and 5-10 nm in width, whilst the crystallite size of anatase polygonal-plates was around 200 nm. The optimal LPCVD condition for preparing this mixed phase of TiO2 was 550 °C (actual temperature) with a 1 mL s-1 N2 flow rate. A possible mechanism for the mixed-phase formation by LPCVD on the glass substrates is described as well as the implications for the production of self-cleaning structures

Ecofriendly alkali metal cations diffusion improves fabrication of mixed-phase titania polymorphs on fixed substrate by chemical vapor deposition (CVD) for photocatalytic degradation of azo dye

Controlling the nanoscale synthesis of semiconductor TiO2 on a fixed substrate has fascinated the curiosity of academics for decades. Synthesis development is required to give an easy-to-control technique and parameters for TiO2 manufacture, leading to advancements in prospective applications such as photocatalysts. This study, mixed-phase TiO2(B)/other titania thin films were synthesized on a fused quartz substrate utilizing a modified Chemical vapor depodition involving alkali-metal ions (Li+, Na+, and K+) solution pre-treatment. It was discovered that different cations promote dramatically varied phases and compositions of thin films. The films had a columnar structure with agglomerated irregular-shaped particles with a mean thickness of 800–2000 nm. Na+ ions can promote TiO2(B) more effectively than K+ ions, however Li+ ions cannot synthesize TiO2(B). The amounts of TiO2(B) in thin films increase with increasing alkali metal (K+ and Na+) concentration. According to experimental and DFT calculations, the hypothesized TiO2(B) production mechanism happened via the meta-stable intermediate alkaline titanate transformation caused by alkali-metal ion diffusion. The mixed phase of TiO2(B) and anatase TiO2 on the fixed substrate (1 × 1 cm2) obtained from Na+ pre-treated procedures showed significant photocatalytic activity for the degradation of methylene blue. K2Ti6O12, Li2TiO3, Rutile TiO2, and Brookite TiO2 phase formations produced by K+ and Li + pretreatment are low activity photocatalysts. Photocatalytic activities were more prevalent in NaOH pre-treated samples (59.1% dye degradation) than in LiOH and KOH pre-treated samples (49.6% and 34.2%, respectively). This revealed that our developed CVD might generate good photocatalytic thin films of mixed-phase TiO2(B)/anatase TiO2 on any substrate, accelerating progress in future applications

A New Functional Composite for Photovoltaic and Sensor Applications

As a preliminary drive to eventually develop dye-sensitized solar cell (DSSC)-powered gas sensors, many oxide-based systems have been explored to fabricate sensors that can show response at room temperature for any analyte gas. As an outcome of recent work in this endeavor, a composite nanorod of anatase TiO2 with Na0.23TiO2 is found to exhibit both photovoltaic performance and gas sensing at room temperature as demonstrated here. An interesting morphology change along with a phase change from nanoparticle to nanorod is observed during the hydrothermal synthesis of anatase TiO2 nanoparticles with sodium hydroxide under a highly basic condition. In order to understand the effect of the minor phase Na0.23TiO2 on the inherent properties of anatase TiO2, the application of nanorod composite in two unique potential application areas, DSSC and acetone sensings is investigated. The composite material exhibits an enhanced efficiency of 7.85% for a DSSC. Surprisingly, a resistive sensor fabricated with the synthesized composite material exhibits room temperature p-type sensing behavior toward different concentrations of acetone (10, 5, 3, 2, and 1 ppm) with high selectivity