Synthesis of single crystal CuAlS2 nanowires via a low temperature direct polyol route

The direct polyol method is used to prepare copper aluminium sulfide CuAlS₂ nanowires. The lattice constants of CuAlS₂ nanowires calculated from powder X-ray diffraction data indicates chalcopyrite structure. The CuAlS₂ nanowires are uniformly in shape and their dimensions are about 50 nm in diameter and several of micrometers in length. The Photoluminescence (PL) spectrum of CuAlS₂ nanowires show a sharp absorption edge at 358.96 nm and a strong near band edge emission at 3.46 eV. The direct energy gap Eg of the sample has been calculated as 3.48 eV, that corresponding to the photoluminescence study. A possible formation mechanism of copper aluminium sulfide is proposed.     

Magnetic properties of chalcogenide spinel CuCr2Se4 nanocrystals

The magnetic properties of chalcogenide spinel CuCr₂Se₄ nanocrystals have been studied as a function of crystallite size (15-30 nm). A solution-based method is used for the facile synthesis of the nanocrystals with good size control. They have close to cubic morphology with a narrow size distribution and exhibit superparamagnetic behavior at room temperature. The Curie temperature and saturation magnetization of the nanocrystals are lower as compared with the bulk and decrease with decreasing nanocrystal size. A similar trend is observed in the paramagnetic state for the Curie-Weiss temperature and effective magnetic moment. The low temperature magnetization behavior can be qualitatively explained by spin glass dynamics.     

Temperature induced size selective synthesis of hybrid Cds/pepsin nanocrystals and their photoluminescence investigation

There is growing interest in materials chemistry for taking advantage of the physical and chemical properties of biomolecules in the development of next generation nanoscale materials for opto-electronic applications. A biomimetic approach to materials synthesis offers the possibility of controlling size, shape, crystal structure, orientation, and organization. The great progress has been made in the control that can be exerted over optical materials synthesis using biomolecules (protein, nucleic acid)/mineral interfaces as templates for directed synthesis. We have synthesized the CdS nanocrystals using pepsin by biomimetic technique at four different set temperatures. X-ray diffraction (XRD) and small angle X-ray scattering (SAXS) results showed that we are able to tune the size and distribution profile just by tuning the reaction (Rx) temperature and goes towards excitonic Bhor radius (2.5 nm) at low temperature (4 °C). The narrow absorption peak at 260 nm from Cd²⁺-pepsin complex dominates and indicates the size dispersion of the modified CdS nanoparticles are fairly monodisperse. Effective mass approximation (EMA) shows large blue-shift (~1 eV) in the band gap for the cubic phase from bulk hexagonal CdS. The photoluminescence (PL) and photoluminescence excitation (PLE) spectra are dominated by a strong and narrow band-edge emission tunable in the blue region indicating a narrow size distribution. The reduction in PL efficiency is observed when the Rx temperature increases however no change in PLE spectra and temporal profiles of the band-edge PL is observed. At 4 °C, high emission efficiency with shift of PL spectrum in the violet region is observed for 1.7 nm size CdS quantum dots (QDs). Presence of pepsin has slowed the PL decay which is of the order of 100 μs.     

Synthesis of Ni-doped InTaO4 nanocrystallites by reactive pulsed laser ablation for application to visible-light-operating photocatalysts

Ni-doped InTaO₄ nanocrystallites were synthesized by a reactive pulsed laser ablation process, aiming at visible-light-operating photocatalysts. The third harmonics beam of a Nd:YAG laser was focused onto a sintered In_0.9Ni_0.1TaO_4−δ target in mixture background gases (O₂ + He). The deposited species were columnar-structured porous films consisting of primary nanocrystallites. The mean diameter of the primary nanocrystallites was 4 nm. Optical absorption characteristics, especially in low absorbance (sub-band) regions, were evaluated by photoacoustic spectroscopy. Absorption in the sub-band region decreased drastically with increasing O₂ partial pressures. It is inferred that oxygen deficiencies are suppressed, because of enough oxygen vapors in the reactive background gases. An absorption band around 420 nm appeared obviously in O₂ partial pressures above 5%, in the Ni-doped InTaO₄ nanocrystallites. The visible region absorption band is presumably attributed to the Ni 3d-eg orbitals. In contrast, pure InTaO₄ nanocrystallites showed a sharp band edge, without the visible absorption band.     

Synthesis and characterization of ZnO-Ag core-shell nanocomposites with uniform thin silver layers

This paper presents an investigation on the synthesis and characterization of ZnO-Ag core-shell nanocomposites. ZnO nanorods were employed as core material for Ag seeds, and subsequent nucleation and growth of reduced Ag by formaldehyde formed the ZnO-Ag core-shell nanocomposites. The ZnO-Ag nanocomposites were annealed at different temperature to improve the crystallinity and binding strength of Ag nanoparticles. The morphology, microstructure and optical properties of the ZnO-Ag core-shell nanocomposites were characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, energy-dispersive X-ray spectroscopy, ultraviolet-visible (UV-vis) absorption and photoluminescence measurement. It was demonstrated that very small face-center-cubic Ag nanoparticles were coated on the surface of ZnO nanorods. The ultraviolet absorption and surface plasmon absorption band of ZnO-Ag core-shell nanocomposites exhibited some redshifts relative to pure ZnO nanorods and monometallic Ag nanoparticles. The coating of Ag nanocrystals onto the ZnO nanorods completely quenched the photoluminescence. These observations reflected the strong interfacial interaction between ZnO nanorods and Ag nanoparticles. The effect of Ag coating thickness on the morphology and optical properties of ZnO-Ag core-shell nanocomposites was also investigated. Moreover, the growth mechanism of ZnO-Ag core-shell nanocomposites was also proposed and discussed in detail.     

Solution-combustion synthesis of Tb-doped Y3Al5O12 nanoparticles

Nano-sized YAG:Tb powder phosphors were prepared by a solution-combustion method, using the general inorganic salts as starting materials. The X-ray diffraction (XRD) measurements showed that the precursor can be well-crystallized at 900 °C. As-prepared particles have sizes mostly in the range between 30 and 100 nm as obtained by scanning electron microscope (SEM) and transition electron microscope (TEM). Selected area electron diffraction (SAED) patterns proved that the larger particles are monocrystalline. The effects of annealing temperature and Tb-doping concentration on the luminescence intensity were studied.     

Area-selectively sputtering the RuO2 nanorods array

The RuO₂ nanorods array is grown selectively on the SiO₂-patterned sapphire (SA) wafers using reactive sputtering. The area-selectivity is attributed to an early nucleation of RuO₂ and its fast surface coverage on SA (1 0 0) and (0 1 2), in contrast to the sluggish nucleation on glassy SiO₂ in the initial sputtering period. The growth domain is explored by investigating the temperature windows at sputtering power 40, 50, and 60 W. The low-temperature bound is limited by the mobility of precursors on SiO₂ surface, which enables the precursors to depart before aggregating into a large size to smear the non-growth region. The high-temperature bound is set by the horizontal growth which enlarges the rod width and deteriorates its one-dimensional feature. The temperature window shrinks with increasing sputtering power. The X-ray photoelectron spectra indicate the as-sputtered rod surface is ruthenium rich. The X-ray diffraction analysis shows that RuO₂ growth on SA (1 0 0) and (0 1 2) follows the epitaxial relations between RuO₂ and SA crystals.     

Nonvolatile Memory Characteristics with Embedded High Density Ruthenium Nanocrystals

Ruthenium （Ru） nanocrystals （NCs） embedded in SiO2 gate stacks are formed by rapid thermal annealing for the whole gate stacks and embedded in the memory structure, which is compatible with conventional CMOS technology. The devices exhibit a substantial and clockwise hysteresis in capacitance-voltage measurement. The Ru NCs exhibit high density （2 × 10^12cm^-2）, small size （2-4 nm） and good uniformity both in spatial distribution and morphology. The charging and long-term retention performances are explained by the Coulomb Blockade phenomena and the asymmetric electron tunnel barrier between the Ru NCs and the Si substrate, respectively.     

High-Density Stacked Ru Nanocrystals for Nonvolatile Memory Application

Stacked ruthenium （Ru） nanocrystals （NCs） are formed by rapid thermal annealing for the whole gate stacks and embedded in memory structure, which is compatible with conventional CMOS technology. Ru NCs with high density （3 × 10^12 cm-2）, small size （2 4nm） and good uniformity both in aerial distribution and morphology are formed. Attributed to the higher surface trap density, a memory window of 5.2 V is obtained with stacked Ru NCs in comparison to that of 3.5 V with single-layer samples. The stacked Ru NCs device also exhibits much better retention performance because of Coulomb blockade and vertical uniformity between stacked Ru NCs.     

Effects of organic acids on the size-controlled synthesis of rutile TiO2 nanorods

Size-controlled synthesis of pure rutile-phase TiO₂ nanorods was carried out by a hydrothermal method using different organic acids as modifiers, and metatitanic acid and concentrated sulfuric acid as raw materials. The synthesized rutile TiO₂ nanorods were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effects of organic acid modifiers on the sizes of rutile TiO₂ nanorods were investigated. It was found that the steric effect occurred by the organic modifiers and non-polarity of organic acids were beneficial to the formation of small-sized rutile TiO₂ nanorods. The strongly coordinative interaction between the carboxyl (or hydroxyl) group of the modifier and the surface of TiO₂ nanoparticles effectively inhibited the crystal growth.     

Surface acoustic phonon modes of Ge nanocrystals embedded in SiO2

Ge nanocrystals (NCs) embedded in SiO₂ are synthesized by ion implantation, and the surface vibrational modes of the Ge NCs are investigated using the low-frequency Raman scattering (LFRS) technique. LFRS studies show distinct low-frequency Raman modes in the range 6.5-21.2 cm⁻¹ for the Ge NCs depending on the implant dose and annealing temperature. These low-frequency Raman modes are attributed to the confined surface acoustic phonon modes of Ge NCs with (0,0) spheroidal mode and (0,3) torsional modes. Our results are in excellent agreement with the recent theoretical predictions of surface vibrational modes in Ge NCs.     

Magnetic properties of large-area one-dimensional WO2 and MoO2 nanorods

Large-area one-dimensional (1D) monoclinic WO₂ and MoO₂ nanorods in the space group P2₁/c were synthesized by reactive thermal evaporation. The as-synthesized 1D WO₂ and MoO₂ nanorods become soft magnetic materials at 10 K, implying that structural or magnetic transitions occur. There are large differences in saturation magnetization, the coercive field, and remanence between the 1D WO₂ and MoO₂ nanorods, although both 1D nanorods have a similar shape.     

Cobalt nanoparticles synthesis from Co(CH3COO)2 by thermal decomposition

Nontoxic cobalt acetate tetrahydrate was used as a precursor to prepare cobalt nanoparticles of 8–200 nm in average diameter by thermal decomposition. The different combinations of trioctylphosphine, oleylamine and oleic acid were added as surfactants to control the particle size. These combinations resulted in the particles with saturation magnetization and coercive force ranging from 55.0 to 100.1 emu/g and from 0 to 459.3 Oe, respectively.     

Structure and surface characterization of ZrO2-Y2O3-Cr2O3 system

3-mol% Y₂O₃ and 0.3 to 3-mol % Cr₂O₃ co-doped ZrO₂ nanopowders were synthesized using co-precipitation technique and investigated by terms of X-ray diffraction, transmission electron microscopy and X-ray photoelectron spectroscopy. Structural analysis shows no significant impact of chromium on powders structure except of presence of small amount of m-phase. Surface analysis reveals segregation of yttrium and chromium atoms to the surface along with surface enrichment by oxygen that can be attributed to residual water. Chromium surface atoms present in three oxidation states with catalytically active Cr²⁺ sites possibly controlling m-phase appearance through lattice distortion.     

Formation of V2O3 nanocrystals by thermal reduction of V2O5 thin films

We report the formation of homogeneous and stable V₂O₃ nanocrystals, directly from V₂O₅ thin films, at 600 °C, as observed by using in situ electron microscopy experiments. Thermally-induced reduction of V₂O₅ thin films in vacuum is remarkably different when compared to reduction of V₂O₅ single crystals and results in the formation of nanophase V₂O₃. Thermally grown V₂O₃ nanocrystals exhibit hexagon or square shape and are stable at higher temperature as well as room temperature. The formation of stable nanocrystals through the reduction process in a non-chemical environment (vacuum) could provide a basis for understanding the complex processes of vanadium oxide phase transitions and for controlling the chemical processes to produce oxide nanocrystals.     

Optical properties of nanocrystalline-coated Y2O3:Er, Yb obtained by mechano-chemical and combustion synthesis

Y₂O₃:Er³⁺, Yb³⁺ nanocrystals have been obtained by ball milling and using a combustion synthesis procedure. In both cases the nanocrystals have been successfully coated with SiO₂ following the Stöber method. The average size of the as-synthesized nanoparticles has been estimated from X-ray diffraction patterns and transmission electron microscopy images. The dependence of the optical properties of these samples on synthesis procedure or dopant concentration has been investigated. Emission, excitation and lifetime measurements have been carried out. Upconversion luminescence has been detected in all samples and an enhancement of the red to green emission ratio has been observed in all samples after infrared compared to visible excitation. The mechanisms responsible for the upconversion phenomena have been discussed.     

Photoelectron spectroscopy of nanocrystalline anatase TiO2 films

Nanocrystalline TiO₂ (anatase) films were prepared using either colloidal suspensions or a sol-gel route. The electronic structure of these films was analyzed using X-ray photoelectron spectroscopy (XPS) and ultraviolet photoelectron spectroscopy (UPS). Apart from pristine films, films containing defects introduced by annealing under ultra-high vacuum conditions or by ion bombardment were investigated. Generally, annealing in the temperature range up to 720 K results in no significant changes in the XPS and UPS spectra as compared to the pristine state, indicating that the amount of defect formation is too low to be observable by these techniques. On the other hand, ion irradiation causes the appearance of distinct defect states; these could be identified in agreement with previous data from photoemission studies on rutile and anatase single crystals. From UPS, a valence-band width of ∼4.6 eV was determined for the nanocrystalline anatase films.     

Interfacial Reactions and Cubic Neodymium Oxide Formation in Low Dispersed Nd2O3-SiO2 System by Wet Chemical Method

Neodymium (binary oxide) powders are synthesized by a solgel technique. Prepared powders are heat treated under different temperature for different time duration and obtained nanostructure of Nd. Metal particle have diameters in the range 7.8-21.6nm. It is found that the heat treatment plays an important role to produce different structure of Nd-doped silica matrix. The peak position shifts to lower angle as the size of the nano metal oxide particles size increases.     

In‐situ dispersion of ZrO2 nano‐particles coated with pentacene

Stable suspensions of pentacene functionalised ZrO₂ nano‐particles were synthesised using a microwave plasma process. The particles were dispersed in‐situ in ethylene glycol. The formation of coated particles with small cores and a well defined size in the range of 3–5 nm was shown by X‐ray diffraction. In difference to resublimed pure pentacene, suspensions of the coated nano‐particles remained stable for weeks, as confirmed by the observation of a small aggregate size in dynamic light scattering. Thin films of the particles on Si based substrates were obtained by drop‐casting. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Microwave plasma synthesis of nano‐crystalline YSZ

Nanocrystalline yttria‐stabilized zirconia (YSZ) powder and compacts have been successfully synthesized by microwave plasma synthesis co‐evaporating Y and Zr precursors from a single source. Both liquid and solid mixtures of chemically homologous precursors were tested. Electron micrographs and X‐ray diffraction studies reveal small crystallites in the range 3–4 nm with a narrow size distribution. Crystallite sizes smaller than 25 nm are preserved even after subsequent annealing at temperatures up to 950 °C. A comparison with other gas‐phase synthesis routes of nanocrystalline YSZ is given. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)