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A series of titanium dioxide (TiO2) modified with 3-aminopropyltriethoxysilane (APTES) was prepared by high-temperature calcination in an argon atmosphere in the temperature range from 800 to 1,000°C. The properties of the obtained samples were compared with those of pure TiO2 annealed under the same conditions. Examining electron paramagnetic resonance (EPR) parameters at room temperature for APTES–TiO2 showed an intense resonance line from defects related to conducting electrons with g eff from 2.0028 to 2.0026 and 1.9052 for temperatures 800, 900, and 1,000°C, respectively, while for pure calcined TiO2, these ERP lines were not observed. With the increase in the calcination temperature to 900°C for APTES–TiO2 samples, the EPR increases linearly. This has been combined with a relatively high anatase content and small crystallites. The EPR line intensity at RT calculated for 1 g of sample showed an almost linear relationship with the photoactivity in removing ORANGE II dyes from water. more...

DC magnetization of a series of titania nanocomposites modified with reduced graphene oxide (rGO) has been investigated. Hysteresis loops observed at room temperature disappeared at low temperatures. At a temperature of about 100 K, a phase transition to the superferromagnetic order state was observed, probably due to the linear expansion and self-reorientation of the magnetic moments. Processes associated with magnetic moment reorientation can cause a hysteresis loop to disappear at low temperatures as well as superferromagnetic ordering. It was suggested that the isolated nanoparticle in the nanopore could be used to create a “compass” at a nanometer-sized level that would be many times more sensitive than the conventional one. Measurements of the zero-field cooling and field cooling modes do not exclude the possibility of the coexistence of a superparamagnetic state. more...

The photocatalytic reduction of CO2 to useful products is an area of active research because it shows a potential to be an efficient tool for mitigating climate change. This work investigated the modification of titania with copper(II) nitrate and its impact on improving the CO2 reduction efficiency in a gas-phase batch photoreactor under UV–Vis irradiation. The investigated photocatalysts were prepared by treating P25-copper(II) nitrate suspensions (with various Cu2+ concentrations), alkalized with ammonia water, in a microwave-assisted solvothermal reactor. The titania-based photocatalysts were characterized by SEM, EDS, ICP-OES, XRD and UV-Vis/DR methods. Textural properties were measured by the low-temperature nitrogen adsorption/desorption studies at 77 K. P25 photocatalysts modified with copper(II) nitrate used in the process of carbon dioxide reduction allowed for a higher efficiency both for the photocatalytic reduction of CO2 to CH4 and for the photocatalytic water decomposition to hydrogen as compared to a reference. Similarly, modified samples showed significantly higher selectivity towards methane in the CO2 conversion process than the unmodified sample (a change from 30% for a reference sample to 82% for the P25-R-Cu-0.1 sample after the 6 h process). It was found that smaller loadings of Cu are more beneficial for increasing the photocatalytic activity of a sample. [ABSTRACT FROM AUTHOR] more...

A whole series of titania nanocomposites modified with reduced graphene oxide (rGO) was prepared using solvothermal method followed by calcination. Modification of titania with rGO has been found to lead to better photocatalytic properties. The highest photocatalytic performance was obtained at calcination temperature of 600°C. Electron paramagnetic resonance/ferromagnetic resonance measurements showed oxygen defects and ferromagnetic ordering systems. The linewidth of resonance line of oxygen defects decreased linearly with calcination temperature increasing up to 600°C and an accompanying growth of mean crystallite size of anatase phase. The integrated resonance line intensity of oxygen defects depended on the calcination temperature and caused a very large increase in the intensity of resonance lines originating from oxygen defects, because inert atmosphere of calcination was enhanced by graphene presence. The occurrence of magnetic ordering system significantly influenced the performance of photocatalytic processes by changing the amount of oxygen defects. more...

Titanium dioxide was synthesized via hydrolysis of titanium (IV) isopropoxide using a sol–gel method, under neutral or basic conditions, and heated in the microwave-assisted solvothermal reactor and/or high-temperature furnace. The phase composition of the prepared samples was determined using the X-ray diffraction method. The specific surface area and pore volumes were determined through low-temperature nitrogen adsorption/desorption studies. The photoactivity of the samples was tested through photocatalytic reduction of carbon dioxide. The composition of the gas phase was analyzed using gas chromatography, and hydrogen, carbon oxide, and methane were identified. The influence of pH and heat treatment on the physicochemical properties of titania-based materials during photoreduction of carbon dioxide have been studied. It was found that the photocatalysts prepared in neutral environment were shown to result in a higher content of hydrogen, carbon monoxide, and methane in the gas phase compared to photocatalysts obtained under basic conditions. The highest amounts of hydrogen were detected in the processes using photocatalysts heated in the microwave reactor, and double-heated photocatalysts. [ABSTRACT FROM AUTHOR] more...

This paper presents new photocatalysts obtained by treating carbon spheres (CS) and TiO2 in a microwave reactor at a pressure of 20 atm and a temperature of up to 300 °C for 15 min and then depositing TiO2/CS composites on glass fibre cloths. Such highly CO2-adsorbing photocatalysts showed photoactivity in the simultaneous water-splitting process, generating H2, reducing CO2 to CO and CH4, and reducing N2 to NH3. In addition, calculations of the hydrogen balance involved in all reactions were performed. Adding 1 g of carbon spheres per 1 g of TiO2 maintained the high selectivity of nitrogen fixation at 95.87–99.5%, which was continuously removed from the gas phase into the water as NH4+ ions. [ABSTRACT FROM AUTHOR] more...

This paper presents the effect of fumed silica modification and calcination temperature on the physicochemical properties of photocatalysts and their activity under the UV-VIS and VIS light range. The materials were obtained by hydrolysis of titanium tetraisopropoxide (TTIP) combined with a calcination step. The obtained nanomaterials were characterized using analytical methods such as X-ray diffraction XRD, FT-IR/DRS infrared spectroscopy, UV-Vis/DRS spectroscopy and SEM scanning electron microscopy. BET specific surface area and zeta potential were also measured. It was observed that SiO2 modification inhibited the transformation phase of anatase to rutile and the increase in crystallite size during calcination. The calcination process contributed to a change in the surface character of photocatalysts under study from positively to negatively charged. The photocatalytic activity of samples was identified by determining the methylene blue decomposition under UV-VIS and VIS light. Experimental results showed that the addition of SiO2 and the calcination process increased the photoactivity. The obtained materials showed higher activity compared to the reference samples. It was found that the degree of dye removal increased along with increased calcination temperature. The highest activity was observed for photocatalyst SiO2(11.1%)/TiO2_600. [ABSTRACT FROM AUTHOR] more...

This work aimed to obtain hybrid composites based on photoactive metal oxide and carbon having adsorption properties. The materials, composed of titanium dioxide or zinc oxide and spherical carbon, were obtained from resorcinol-formaldehyde resin, treated in a solvothermal reactor heated with microwaves and then subjected to carbonization, were received. The functional groups of pure carbon spheres (unsaturated stretching C=C, stretching C−OH and C−H bending vibrations), CS/ZnO and CS/TiO2 samples were determined by FT-IR analysis. The characteristic bands for ZnO and TiO2 were observed below 1000 cm−1. The thermal oxidative properties are similar for TiO2- and ZnO-modified carbon spheres. We have observed that the increased carbon sphere content in nanocomposites results in starting the decomposition process at a lower temperature, therefore, nanocomposites have a broader combustion temperature range. The effect of the oxides' addition to carbon spheres on their adsorption properties was evaluated in detail by examining CO2 adsorption from the gas phase. The selectivity of CO2 over N2 at a temperature of 25 °C and pressure of 1 bar (a novelty in testing CS-based sorbents) calculated for 3.00 CS/TiO2 and 4.00 CS/ZnO was 15.09 and 16.95, respectively. These nanocomposites exhibit excellent cyclic stability checked over 10 consecutive adsorption–desorption cycles. [ABSTRACT FROM AUTHOR] more...

In this work, physicochemical and photocatalytic properties of titanium dioxide nanomaterial modified with 3-aminopropyltrimethoxysilane (APTMS) is presented. The photocatalyst was obtained by a two-step solvothermal and calcination method at 700°C in an argon atmosphere. The tested materials were characterized by means of X-ray diffraction, scanning electron microscopy, Fouriertransform infrared spectroscopy/diffuse reflectance spectroscopy (UV-Vis/DRS). The Brunauer- Emmett-Teller specific surface area as well as pore size distribution were also measured. It was noted that the APTMS modification played a significant role in phase transformation changes, crystallite size as well as values of the specific surface area. It was found that the transformation from anatase to rutile was suppressing after APTMS modification. The photocatalytic activity of the obtained samples was determined by the phenol photodegradation under artificial solar light. The photocatalyst after aminosilanes modification and calcination exhibited higher photoactivity than TiO2-starting and the sample obtained similarly but without the addition of APTMS. [ABSTRACT FROM AUTHOR] more...