Enhanced ethanol sensing properties of WO3 modified TiO2 nanorods

Pristine and WO₃ decorated TiO₂ nanorods (NRs) were synthesised to investigate n-n-type heterojunction gas sensing properties. TiO₂ NRs were fabricated via hydrothermal method on fluorine-doped tin oxide coated glass (FTO) substrates. Then, tungsten was sputtered on the TiO₂ NRs and thermally oxidised to obtain WO₃ nanoparticles. The heterostructure was characterised by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray (EDX) spectroscopy. Fabricated sensor devices were exposed to VOCs such as toluene, xylene, acetone and ethanol, and humidity at different operation temperatures. Experimental results demonstrated that the heterostructure has better sensor response toward ethanol at 200 °C. Enhanced sensing properties are attributed to the heterojunction formation by decorating TiO₂ NRs with WO₃.     

Phenolic compounds,essential oil composition,and antioxidant activity of Angelica purpurascens (Avé-Lall.) Gill

In this study, methanol extracts (MEs) and essential oil (EO) of Angelica purpurascens (Avé-Lall.) Gill obtained from different parts (root, stem, leaf, and seed) were evaluated in terms of antioxidant activity, total phenolics, compositions of phenolic compound, and essential oil with the methods of 2,2-azino-bis(3ethylbenzo-thiazoline-6-sulfonic acid (ABTS•⁺), 2,2-diphenyl-1-picrylhydrazil (DPPH•) radical scavenging activities, and ferric reducing/antioxidant power (FRAP), the Folin–Ciocalteu, liquid chromatography−tandem mass spectrometry (LC−MS/MS), and gas chromatography-mass spectrometry (GC−MS), respectively. The root extract of A. purpurascens exhibited the highest ABTS•⁺, DPPH•, and FRAP activities (IC₅₀: 0.05 ± 0.0001 mg/mL, IC₅₀: 0.06 ± 0.002 mg/mL, 821.04 ± 15.96 µM TEAC (Trolox equivalent antioxidant capacity), respectively). Moreover, EO of A. purpurascens root displayed DPPH• scavenging activity (IC₅₀: 2.95 ± 0.084 mg/mL). The root extract had the highest total phenolic content (438.75 ± 16.39 GAE (gallic acid equivalent), µg/mL)). Twenty compounds were identified by LC−MS/MS. The most abundant phenolics were ferulic acid (244.39 ± 15.64 μg/g extract), benzoic acid (138.18 ± 8.84 μg/g extract), oleuropein (78.04 ± 4.99 μg/g extract), and rutin (31.21 ± 2.00 μg/g extract) in seed, stem, root, and leaf extracts, respectively. According to the GC−MS analysis, the major components were determined as α-bisabolol (22.93%), cubebol (14.39%), α-pinene (11.63%), and α-limonene (9.41%) among 29 compounds. Consequently, the MEs and EO of A. purpurascens can be used as a natural antioxidant source.     

RE(AuAl2)nAl2(AuxSi1-x)2: a new homologous series of quaternary intermetallics grown from aluminum flux

The combination of early rare earth metals (La- to Gd and Yb), gold, and silicon in molten aluminum results in the formation of intermetallic compounds with four related structures, forming a new homologous series: RE[AuAl2]nAl2(AuxSi(1-x))2, with x approximately 0.5 for most of the compound and n = 0, 1, 2, and 3. Because of the highly reducing nature of the Al flux, rare earth oxides instead of metals can also be used in these reactions. These compounds grow as large plate-like crystals and have tetragonal structure types that can be viewed as intergrowths of the BaAl4 structure and antifluorite-type AuAl2 layers. REAuAl2Si materials form with the BaAl4 structure type in space group I4/mmm (cell parameters for the La analogue are a = 4.322(2) A, c = 10.750(4) A, and Z = 2). REAu2Al4Si forms in a new ordered superstructure of the KCu4S3 structure type, with space group P4/nmm and cell parameters of the La analogue of a = 6.0973(6) A, c = 8.206(1) A, and Z = 2. REAu3Al6Si forms in a new I4/mmm symmetry structure type with cell parameters of a = 4.2733(7) A, c = 22.582(5) A, and Z = 2 for RE = Eu. The end member of the series, REAu4Al8Si, forms in space group P4/mmm with cell parameters for the Yb analogue of a = 4.2294(4) A, c = 14.422(2) A, and Z = 1. New intergrowth structures containing two different kinds of AuAl2 layers were also observed. The magnetic behavior of all these compounds is derived from the RE ions. Comparison of the susceptibility data for the europium compounds indicates a switch from 3-D magnetic interactions to 2-D interactions as the size of the AuAl2 layer increases. The Yb ions in YbAu(2.91)Al(6)Si(1.09) and YbAu(3.86)Al(8)Si(1.14) are divalent at high temperatures.     

RE2MAl6Si4 (RE = Gd, Tb, Dy; M = Au, Pt): layered quaternary intermetallics featuring CaAl2Si2-type and YNiAl4Ge2-type slabs grown from aluminum flux

Six new intermetallic aluminum silicides--Gd(2)PtAl(6)Si(4), Gd(2)AuAl(6)Si(4), Tb(2)PtAl(6)Si(4), Tb(2)AuAl(6)Si(4), Dy(2)PtAl(6)Si(4), and Dy(2)AuAl(6)Si(4)--have been obtained from reactions carried out in aluminum flux. The structure of these compounds was determined by single-crystal X-ray diffraction. They form in space group Rthremacr;m with cell constants of a = 4.1623(3) A and c = 51.048(5) A for the Gd(2)PtAl(6)Si(4) compound. The crystal structure is comprised of hexagonal nets of rare earth atoms alternating with two kinds of layers that have been observed in other multinary aluminide intermetallic compounds (CaAl(2)Si(2) and YNiAl(4)Ge(2)). All six RE(2)MAl(6)Si(4) compounds show antiferromagnetic transitions at low temperatures (T(N) < 20 K); magnetization studies of the Dy compounds show metamagnetic behavior with reorientation of spins at 6000 G. Band structure calculations indicate that the AlSi puckered hexagonal sheets in this structure are electronically distinct from the other surrounding structural motifs.     

Siting of antimony dopants and gallium in Ba(8)Ga(16)Ge(30) clathrates grown from gallium flux

A series of antimony-doped Ba(8)Ga(16)Ge(30) clathrates was grown as large crystals from gallium flux. These compounds form in the cubic space group Pm(-)3n, with the unit cell parameter varying from 10.784(5) to 10.9008(6) A as the amount of GaSb substituting for germanium atoms in the framework is increased. It was found that more antimony than extra gallium was incorporated into the material and that a specific site (the 24k Wyckoff site) was favored by this element. (71)Ga NMR was carried out to determine the siting of gallium; it fills the 6c site preferentially.     

Structurally complex cobalt intermetallics grown from liquid aluminum: Co19Al45Si(10-x) (x = 0.13) and Co5Al14Si2

The cobalt aluminum silicides Co19Al45Si(10-x) (x = 0.13) and Co5Al14Si2 were synthesized in liquid aluminum and characterized by single-crystal X-ray diffraction. Co19Al45Si(10-x) (x = 0.13) crystallizes in the monoclinic space group C2/c with lattice parameters a = 19.991(2) A, b = 19.143(2) A, c = 12.8137(15) A, beta = 123.583(2) degrees. Co5Al14Si2 adopts the orthorhombic space group Pnma with cell parameters a = 13.8948(19) A, b = 23.039(3) A, c = 7.3397(10) A. Both structures are exceptionally complex with the Co2Si2 rhombus being a common building motif. The coordination environments of cobalt atoms resemble those of the transition metals in typical quasi-crystal approximants. Co5Al14Si2 shows oxidation resistance in air up to 1000 degrees C by forming a dense-packed Al2O3 layer on the surface of the crystal.     

CHARACTERIZATION OF NANOSTRUCTURES:TOOLS AND CHALLENGES

Apart from long-known and applied nanostructures like carbon black for tyres or pigments for coatings nanotechnology has created highly sophisticated structures used for nano/molecular electronics,diagnostics,drug delivery, UV-absorbers etc.Often the main question to be solved analytically is the local determination of tiny amounts of chemicals resulting in an ever increasing need for highly sensitive as well as locally resolved techniques.Applications of techniques like mass spectroscopy,transmission el...