Alexandra Teleki

Semiconductor Gas Sensors: Dry Synthesis and Application

Since the development of the first chemoresistive metal oxide based gas sensors, transducers with innovative properties have been prepared by a variety of wet- and dry-deposition methods. Among these, direct assembly of nanostructured films from the gas phase promises simple fabrication and control and with the appropriate synthesis and deposition methods nm to μm thick films, can be prepared. Dense structures are achieved by tuning chemical or vapor deposition methods whereas particulate films are obtained by deposition of airborne, mono- or polydisperse, aggregated or agglomerated nanoparticles. Innovative materials in non-equilibrium or sub-stoichiometric states are captured by rapid cooling during their synthesis. This Review presents some of the most common chemical and vapor-deposition methods for the synthesis of semiconductor metal oxide based detectors for chemical gas sensors. In addition, the synthesis of highly porous films by novel aerosol methods is discussed. A direct comparison of structural and chemical properties with sensing performance is given.

Iron from nanocompounds containing iron and zinc is highly bioavailable in rats without tissue accumulation

Effective iron fortification of foods is difficult, because water-soluble compounds that are well absorbed, such as ferrous sulphate (FeSO(4)), often cause unacceptable changes in the colour or taste of foods. Poorly water-soluble compounds, on the other hand, cause fewer sensory changes, but are not well absorbed. Here, we show that poorly water-soluble nanosized Fe and Fe/Zn compounds (specific surface area approximately 190 m(2) g(-1)) made by scalable flame aerosol technology have in vivo iron bioavailability in rats comparable to FeSO(4) and cause less colour change in reactive food matrices than conventional iron fortificants. The addition of Zn to FePO(4) and Mg to Fe/Zn oxide increases Fe absorption from the compounds, and doping with Mg also improves their colour. After feeding rats with nanostructured iron-containing compounds, no stainable Fe was detected in their gut wall, gut-associated lymphatics or other tissues, suggesting no adverse effects. Nanosizing of poorly water-soluble Fe compounds sharply increases their absorption and nutritional value.

In Situ Coating of Flame-Made TiO2 Particles with Nanothin SiO2 Films

Rutile TiO2 particles made by flame spray pyrolysis (FSP) were coated in a single step with SiO2 layers in an enclosed flame reactor. This in situ particle coating was accomplished by a hollow ring delivering hexamethyldisiloxane (HMDSO) vapor (precursor to SiO2) through multiple jets in swirl cross-flow to Al-doped nanostructured rutile TiO2 aerosol freshly made by FSP of a solution of titanium tetraisopropoxide and aluminum sec-butoxide in xylene. The as-prepared powders were characterized by (scanning) transmission electron microscopy (STEM and TEM), energy dispersive X-ray analysis, X-ray diffraction, nitrogen adsorption, electrophoretic mobility, DC plasma optical emission (DCP-OES), and Fourier transform infrared (FT-IR) spectroscopy. The coating quality was assessed further by the photocatalytic oxidation of isopropyl alcohol to acetone. The effect of HMDSO injection point and vapor concentration on product particle morphology was investigated. The titania particles were uniformly SiO2-coated with controlled and uniform thickness at a production rate of about 30 g h(-1) and exhibited limited, if any, photoactivity. In contrast, spraying and combusting equivalent mixtures of the above Si/Al/Ti precursors in the above reactor (without delivering HMDSO through the hollow ring) resulted in particles segregated in amorphous (SiO2) and crystalline (TiO2) domains which exhibited high photocatalytic activity.

Blue nano titania made in diffusion flames

Blue titanium suboxide nanoparticles (including Magneli phases) were formed directly without any post-processing or addition of dopants by combustion of titanium-tetra-isopropoxide (TTIP) vapor at atmospheric pressure. Particle size, phase composition, rutile and anatase crystal sizes as well as the blue coloration were controlled by rapid quenching of the flame with a critical flow nozzle placed at various heights above the burner. The particles showed a broad absorption in the near-infrared region and retained their blue color upon storage in ambient atmosphere. A high concentration of paramagnetic Ti3+ centres was found in the substoichiometric particles by electron paramagnetic resonance (EPR) spectroscopy. Furthermore particles with controlled band gap energy from 3.2 to 3.6 eV were made by controlling the burner-nozzle-distance from 10 to 1 cm, respectively. The color robustness and extent of suboxidation could be further enhanced by co-oxidation of TTIP with hexamethyldisiloxane in the flame resulting in SiO2-coated titanium suboxide particles. The process is cost-effective and green while the particles produced can replace traditional blue colored, cobalt-containing pigments.

Development and optimization of iron- and zinc-containing nanostructured powders for nutritional applications

Reducing the size of low-solubility iron (Fe)-containing compounds to nanoscale has the potential to improve their bioavailability. Because Fe and zinc (Zn) deficiencies often coexist in populations, combined Fe/Zn-containing nanostructured compounds may be useful for nutritional applications. Such compounds are developed here and their solubility in dilute acid, a reliable indicator of iron bioavailability in humans, and sensory qualities in sensitive food matrices are investigated. Phosphates and oxides of Fe and atomically mixed Fe/Zn-containing (primarily ZnFe2O4) nanostructured powders were produced by flame spray pyrolysis (FSP). Chemical composition and surface area were systematically controlled by varying precursor concentration and feed rate during powder synthesis to increase solubility to the level of ferrous sulfate at maximum Fe and Zn content. Solubility of the nanostructured compounds was dependent on their particle size and crystallinity. The new nanostructured powders produced minimal color changes when added to dairy products containing chocolate or fruit compared to the changes produced when ferrous sulfate or ferrous fumarate were added to these foods. Flame-made Fe- and Fe/Zn-containing nanostructured powders have solubilities comparable to ferrous and Zn sulfate but may produce fewer color changes when added to difficult-to-fortify foods. Thus, these powders are promising for food fortification and other nutritional applications.

The quality of SiO2-coatings on flame-made TiO2-based nanoparticles

Silica-coated titania nanoparticles are important in sunscreens, UV filters and optical nanocomposites. The surface characteristics (extent of coverage, texture and thickness) of in situ SiO2-coated, mostly rutiletitania nanoparticles made in one step by flame spray pyrolysis (FSP) were compared to FSP-made mixed (co-oxidized) SiO2/TiO2 ones by transmission electron microscopy (TEM), Raman, FT-IR spectroscopy, electrophoretic mobility and isopropanol chemisorption followed by mass spectroscopy. Increasing the silica content shifted the isoelectric point (IEP) toward that of pure silica for externally mixed SiO2 and TiO2, co-oxidized SiO2/TiO2 and low SiO2 content (<10 wt%) silica-coated TiO2nanoparticles. At higher SiO2 contents, SiO2-coated titania exhibited negative ζ potentials at all pH values (and thus no IEP) indicating hermetic or complete coverage of the TiO2 surface by SiO2 as was confirmed by isopropanol chemisorption. Co-oxidized particles containing segregated TiO2 and SiO2 domains exhibited Si–O–Ti and Si–O–Si bonds of higher IR intensity than hermetically-coated TiO2. The latter exhibited a peak at 1225 cm−1 attributed to Si–O–Si asymmetric vibrations in contrast to the former.

Flame-coating of titania particles with silica

Silica/titania composite particles were prepared by co-oxidation of titanium-tetra-isopropoxide and hexamethyldisiloxane in a co-flow diffusion flame reactor. The influence of precursor composition on product powder characteristics was studied by x-ray diffraction, nitrogen adsorption, electron microscopy, elemental mapping, and energy-dispersive x-ray analysis. The flame temperature was measured by Fourier transform infrared spectroscopy. The evolution of composite particle morphology from ramified agglomerates to spot- or fully coated particles was investigated by thermophoretic sampling and transmission/scanning electron microscopy. At 40–60 wt% TiO 2 , particles with segregated regions of silica and titania were formed, while at 80 wt% TiO 2 rough silica coatings were obtained. Rapid flame-quenching with a critical flow nozzle at 5 cm above the burner nearly halved the product particle size, changed its crystallinity from pure anatase to mostly rutile and resulted in smooth silica coatings on particles containing 80 wt% TiO 2 .

Incorporation of Mg and Ca into Nanostructured Fe2O3 Improves Fe Solubility in Dilute Acid and Sensory Characteristics in Foods

Iron deficiency is one of the most common micronutrient deficiencies worldwide. Food fortification can be an effective and sustainable strategy to reduce Fe deficiency but selection of iron fortificants remains a challenge. Water-soluble compounds, for example, FeSO(4), usually demonstrate high bioavailability but they often cause unacceptable sensory changes in foods. On the other hand, poorly acid-soluble Fe compounds, for example FePO(4), may cause fewer adverse sensory changes in foods but are usually not well bioavailable since they need to be dissolved in the stomach prior to absorption. The solubility and the bioavailability of poorly acid-soluble Fe compounds can be improved by decreasing their primary particle size and thereby increasing their specific surface area. Here, Fe oxide-based nanostructured compounds with added Mg or Ca were produced by scalable flame aerosol technology. The compounds were characterized by nitrogen adsorption, X-ray diffraction, transmission electron microscopy, and Fe solubility in dilute acid. Sensory properties of the Fe-based compounds were tested in 2 highly reactive, polyphenol-rich food matrices: chocolate milk and fruit yoghurt. The Fe solubility of nanostructured Fe(2)O(3) doped with Mg or Ca was higher than that of pure Fe(2)O(3). Since good solubility in dilute acid was obtained despite the inhomogeneity of the powders, inexpensive precursors, for example Fe- and Ca-nitrates, can be used for their manufacture. Adding Mg or Ca lightened powder color, while sensory changes when added to foods were less pronounced than for FeSO(4). The combination of high Fe solubility and low reactivity in foods makes these flame-made nanostructured compounds promising for food fortification. Practical Application: The nanostructured iron-containing compounds presented here may prove useful for iron fortification of certain foods; they are highly soluble in dilute acid and likely to be well absorbed in the gut but cause less severe color changes than FeSO(4) when added to difficult-to-fortify foods.

Continuous Surface Functionalization of Flame-Made TiO2 Nanoparticles

Hydrophilic TiO(2) particles made in a flame aerosol reactor were converted in situ to hydrophobic ones by silylation of their surface hydroxyl groups. So the freshly formed titania aerosol was mixed with a fine spray of octyltriethoxysilane (OTES) in water/ethanol solution and functionalized continuously at high temperature. The extent of functionalization and structure of that surface layer were assessed by thermogravimetric analysis (TGA) coupled to mass spectroscopy (MS), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR), and Raman spectroscopy. Product particles were characterized also by transmission electron microscopy (TEM), X-ray diffraction, and nitrogen adsorption. The influence of titania specific surface area (SSA) and OTES solution concentration on the functional group surface density was investigated. The titanium dioxide surface was covered with functional groups (up to 2.9 wt %) that were thermally stable up to 300 degrees C in air at an average density of 2 OTES/nm(2). Such surface-functionalized particle suspensions in 2-ethylhexanoic acid and xylene were stable over several weeks. In contrast, as-prepared hydrophilic TiO(2) precipitated within days in these solvents.

Effect of size, composition, and morphology on magnetic performance: First-order reversal curves evaluation of iron oxide nanoparticles

Superparamagnetic nanoparticles are employed in a broad range of applications that demand detailed magnetic characterization for superior performance, e.g., in drug delivery or cancer treatment. Magnetic hysteresis measurements provide information on saturation magnetization and coercive force for bulk material but can be equivocal for particles having a broad size distribution. Here, first-order reversal curves (FORCs) are used to evaluate the effective magnetic particle size and interaction between equally sized magnetic iron oxide (Fe2O3) nanoparticles with three different morphologies: (i) pure Fe2O3, (ii) Janus-like, and (iii) core/shell Fe2O3/SiO2 synthesized using flame technology. By characterizing the distribution in coercive force and interaction field from the FORC diagrams, we find that the presence of SiO2 in the core/shell structures significantly reduces the average coercive force in comparison to the Janus-like Fe2O3/SiO2 and pure Fe2O3 particles. This is attributed to the reduction in the...