Large-scale synthesis of ZnSe nanoribbons on zinc substrate

ZnSe nanoribbons have been successfully synthesized on a large scale by solvothermal treatment of Zn and Se powder in the mixture of hydrazine hydrate and diethanolamine at 140 °C for 24 h and subsequent annealing in Ar. The morphology of the final products strongly depended on the volume ratio of hydrazine hydrate and diethanolamine. Scanning electron microscopy (SEM) explorations indicated that the as-prepared ZnSe nanoribbons were mostly about 40 nm in thickness, 100 nm in width, and 50 μm in length. X-ray diffraction pattern (XRD) and transmission electron microscopy (TEM) investigations confirmed that resulting ZnSe nanoribbons are wurtzite structures and have a [0 0 1] growth direction. PL (photoluminescence) spectrum of the products exhibited a visible light emission. Based on these investigations, the products were expected to find wide applications in optoelectronic, field emission and catalytic fields.     

Surfactant effects on the particle size of iron (III) oxides formed by sol-gel synthesis

In this work, we probed the effects of a common surfactant, sodium dodecylbenzene sulfonate (NaDDBS), on the particle size of iron (III) oxides formed via a modified sol-gel synthesis. The goal was to create tunable nanosized particles via a method that combines the efficiency and advantages of the sol-gel process, but inhibits the formation of a gel. Two different metal salt precursors were used, ferric nitrate nonahydrate, Fe(NO₃)₃ · 9H₂O, and ferric chlorate hexahydrate, FeCl₃ · 6H₂O. The particle size of the dried gel was 4.5 nm for Fe(NO₃)₃ · 9H₂O and 3.6 nm for FeCl₃ · 6H₂O. In the presence of the surfactant FeCl₃ · 6H₂O formed a gel and Fe(NO₃)₃ · 9H₂O was unable to gel, but the new particle sizes were 4.9 nm and 3.2 nm, respectively. The addition of the surfactant in the later stages of the process afforded the stabilization of independent nanoparticles of the same size as those obtained in the systems that gelled.     

Synthesis,morphology and phase transition of the zinc molybdates ZnMoO4·0.8H2O/α-ZnMoO4/ZnMoO4 by hydrothermal method

ZnMoO₄ with a rhombus sheet or flower-like structure, α-ZnMoO₄ and needle-like ZnMoO₄·0.8 H₂O were successfully synthesized by simple hydrothermal crystallization processes with citric acid. ZnMoO₄·0.8 H₂O was easily synthesized in a shorter reaction time (2 h) at a higher reactant concentration. It gradually transformed into ZnMoO₄ with a monoclinic wolframite tungstate structure with an increased reaction time, and pure ZnMoO₄ was obtained with a longer reaction time (8 h). Citric acid (CA) played an important role in controlling the morphology of the as-obtained molybdates. The α-ZnMoO₄ and ZnMoO₄ were synthesized by heating ZnMoO₄·0.8 H₂O at 130 °C for 4 h and 8 h, respectively, under hydrothermal conditions. With transforming of ZnMoO₄·0.8 H₂O to α-ZnMoO₄ and further to ZnMoO₄, the needle-like crystals gradually disappeared and were transformed into crystals with rhombus sheet morphology and then further to pentacle or flower-like crystals that can be ascribed to continuous splitting and growing of the rhombus sheets.     

Thermal Properties and Phase Transformation of 2 mol% Y2O3-PSZ Nanopowders Prepared by a Co-precipitation Process

Two mol% Y₂O₃-PSZ precursor powders for dental applications were synthesized using ZrOCl₂·8H₂O and Y(NO₃)₃·6H₂O by a co-precipitation process at pH 7 and 348 K for 2 h. The thermal properties and phase transformation of 2Y-PSZ nanocrystallite powder have been investigated using a thermogravimetric and difference scanning calorimeter (TG/DSC), Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy (TEM), selected area electron diffraction and dilatometric analysis. Two weaker broad exothermic peaks appear at around 618 and 718 K were explored in DSC results. The TG analysis shows that minor weight loss occurs from 298 to 348 K, followed by three major weight losses at 610, 630 and 773 K. Calcinated at 773 and 1273 K, the crystallized phases are composed of the major phase of tetragonal ZrO₂ and minor phase of monoclinic ZrO₂. TEM reveals that the tetragonal ZrO₂ with an average size of less than 20.0 nm is mainly aggregated into the secondary aggregates with a size of small than 30.0 nm. The sintering curve of the compact pellet has a significant shrinkage with a linear rate of 18.5% at about 1341 K. Maximum densification rate happened at 1473 K, demonstrating the good low temperature sinterability for dental applications.     

Energetics of CdSxSe1−x quantum dots in borosilicate glasses

The thermodynamics of CdSe quantum dots embedded in a glass matrix is of great interest because of the numerous applications as optical materials. In this study, the energetics and stability of CdSe quantum dots in a borosilicate glass matrix is investigated as a function of size using high-temperature oxide melt solution calorimetry. CdS_0.1Se_0.9 nanoparticles (1-40 nm) embedded in glass were analyzed by photoluminescence spectroscopy, electron microprobe, X-ray fluorescence, high-energy synchrotron X-ray diffraction, and (scanning) transmission electron microscopy using both electron energy loss and energy dispersive X-ray spectroscopy. As CdSe particles coarsen, their heat of formation becomes more exothermic. The interfacial energy of CdSe QDs embedded in a borosilicate glass, determined from the slope of enthalpy of drop solution versus calculated surface area, is 0.56 ± 0.01 J/m².     

Sol–gel preparation and photoluminescence properties of Ce-activated Y3Al5O12 nano-sized powders

Trivalent cerium-doped yttrium aluminum garnet (YAG:Ce³⁺) nanoparticles were successfully prepared by a facile sol–gel technique. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and photoluminescence (PL) spectroscopy were used to characterize the as-prepared phosphors. Well-crystallized fine nanoparticles were obtained at 1000 °C. Single-crystal nanoparticles with irregular shapes were obtained, with crystallite sizes ranging between 20 and 60 nm. PL intensity of the particles increased monotonically with decreasing Ce doping concentration and showed the maximum value at 0.1 at%.     

Synthesis of Nb2O5·nH2O nanoparticles by water-in-oil microemulsion

Hydrous niobium oxide (Nb₂O₅·nH₂O) nanoparticles had been successfully prepared by water-in-oil microemulsion. They were characterized by X-ray diffraction (XRD), thermal analysis (TG/DTG), Fourier transform infrared spectroscopy (FTIR), BET surface area measurement, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The results showed that the nanoparticle was exactly Nb₂O₅·nH₂O with spherical shape. Their BET surface area was 60 m² g⁻¹. XRD results showed that Nb₂O₅·nH₂O nanoparticles with crystallite size in nanometer scale were formed. The crystallinity and crystallity size increased with increasing annealing temperature. TT-phase of Nb₂O₅ was obtained when the sample is annealed at 550 °C.     

Preparation of Sb2S3 nanomaterials with different morphologies via a refluxing approach

Single-crystalline antimony trisulfide (Sb₂S₃) nanomaterials with flower-like and rod-like morphologies were successfully synthesized under refluxing conditions by the reaction of antimony trichloride (SbCl₃) and thiourea with PEG400 and OP-10 as the surfactants. X-ray diffraction (XRD) indicates that the obtained sample is orthorhombic-phase Sb₂S₃ with calculated lattice parameters a=1.124 nm, b=1.134 nm and c=0.382 nm. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images show that the flower-like Sb₂S₃ is 9–10 μm in size, which is composed of thin leaves with thickness of 0.05–0.2 μm, width of 0.8–2.2 μm and length of 2.5–3 μm, and the rod-like Sb₂S₃ is 45–360 nm in diameter and 0.7–4 μm in length, respectively. UV–Vis analysis indicates that the band gap of Sb₂S₃ nanorods is 1.52 eV, suitable for photovoltaic conversion. A possible mechanism of formation was proposed. The effects of reaction time and surfactants on the growth of nanomaterials with different morphologies were also investigated.     

Studies of Er doped germanate-oxyfluoride and tellurium-germanate-oxyfluoride transparent glass-ceramics

An erbium doped germanate-oxyfluoride glass 60GeO₂ · 20PbO · 10PbF₂ · 10CdF₂ (GPOF) and a tellurium-germanate-oxyfluoride glass 30TeO₂ · 30GeO₂ · 20PbO · 10PbF₂ · 10CdF₂ (TGPOF) were prepared in the bulk form. By appropriate heat treatment of the as-prepared glasses above, transparent glass-ceramics were obtained with the formation of β-PbF₂ nanocrystals in the glass matrix confirmed by X-ray diffraction. Optical absorption and photoluminescence measurements were performed on as-prepared glass and glass-ceramics. The luminescence of Er³⁺ ions in transparent glass-ceramics revealed sub-band splitting generally seen in a crystal host. The intensity of red and near infrared luminescence significantly increased in transparent glass-ceramic compared to that in as-prepared glass. Two luminescence bands at 758 nm from ⁴F_7/2 → ⁴I_13/2 and at 817 nm from ²H_11/2 → ⁴I_13/2 transitions were observed from transparent glass-ceramic but cannot be seen from the corresponding as-prepared glass. These results are attributed to the change of ligand field of Er³⁺ ions and the decrease of effective phonon energy when Er³⁺ ions were incorporated into the precipitated β-PbF₂ nanocrystals.     

Facile synthesis and assembly of CuS nano-flakes to novel hexagonal prism structures

Highly ordered hexagonal prism microstructures of copper sulfide (CuS) by assembling nano-flakes have been synthesized with high yield via a facile one-step route. We synthesized CuS microstructures using low cost beginning materials CuSO₄·5H₂O and Na₂S₂O₃·5H₂O under lower reaction temperature (60 °C). Hexamethylinetetramin (C₆H₁₂N₄, HMT) was introduced into the reaction system as a capped agent. The influence of reaction time and capping agent (HMT) on the final structure of products was studied systematically. The obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy-dispersive X-ray spectroscopes (EDS), and transmission electron microscopy (TEM). The possible mechanism for the formation of the interesting highly ordered hexagonal prism microstructures CuS was also proposed.     

Synthesis, modeling of the structure and kinetic study of the thermal decomposition of La(III) and Nd(III) complexes with 3-hydroxypicolinic acid

Synthesis, spectroscopic studies, prediction of the structure and thermal decomposition of the La(3-OHpic)₃ · 3H₂O and Nd(3-OHpic)₃ · 3H₂O (3-OHpic = 3-hydroxypicolinic acid) complexes are described. Elemental analysis and the IR vibrational data are consistent with the complex formulae. The absorption spectra in ethanol of the La(3-OHpic)₃ · 3H₂O and Nd(3-OHpic)₃ · 3H₂O show maximum absorptions at 214 and 211 nm, respectively, which are shifted to 225 nm in the free ligand. The ab initio method RHF/STO-3G/ECP(MWB52) was used to optimize the geometry and the INDO/S-CI model for calculating the electronic spectra of these complexes. A good agreement between theoretical and experimental UV absorption spectra has been obtained. The thermal decomposition was studied by non-isothermal thermogravimetry. Thermal decomposition reactions of the complexes La(3-OHpic)₃ · 3H₂O and Nd(3-OHpic)₃ · 3H₂O are best described by R2 and R3 kinetic models.     

Template free-solvothermaly synthesized copper selenide (CuSe,Cu2−xSe, β-Cu2Se and Cu2Se) hexagonal nanoplates from different precursors at low temperature

Nonstoichiometric (Cu_2−xSe) and stoichiometric (CuSe, β-Cu₂Se and Cu₂Se) copper selenide hexagonal nanoplates have been synthesized using different general and convenient copper sources, e.g. copper chloride, copper sulphate, copper nitrate, copper acetate, elemental copper with elemental selenium, friendly ethylene glycol and hydrazine hydrate in a defined amount of water at 100 °C within 12 h adopting the solvothermal method. Phase analysis, purity and morphology of the product have been well studied by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray diffraction (EDAX) techniques. The structural and compositional analysis revealed that the products were of pure phase with corresponding atomic ratios. SEM, TEM and HRTEM analyses revealed that the nanoplates were in the range 200–450 nm and the as-prepared products were uniform and highly crystallized. The nanoplates consisted of {0 0 1} facets of top–bottom surfaces and {1 1 0} facets of the other six side surfaces. This new approach encompasses many advantages over the conventional solvothermal method in terms of product quality (better morphology control with high yield) and reaction conditions (lower temperatures). Copper selenide hexagonal nanoplates obtained by the described method could be potential building blocks to construct functional devices and solar cell. This work may open up a new rationale on designing the solution synthesis of nanostructures for materials possessing similar intrinsic crystal symmetry. On the basis of the carefully controlled experiments mentioned herein, a plausible formation mechanism of the hexagonal nanoplates was suggested and discussed. To the best of our knowledge, this is the first report on nonstoichiometric (Cu_2−xSe) as well as stoichiometric (CuSe, β-Cu₂Se and Cu₂Se) copper selenide hexagonal nanoplates with such full control of morphologies and phases by this method under mild conditions.     

Synthesis and growth mechanism of rough PbTe polycrystalline thermoelectric nanorods

Rough PbTe polycrystalline one-dimensional nanostructure is expected to exhibit improved thermoelectric properties, compared to single-crystal one. In this article, polycrystalline PbTe thermoelectric nanorods with rough surfaces are successfully synthesized with or without surfactants by a simple alkaline reducing chemical route. Microstructural analyses show that these nanorods range from 50 to 200 nm in diameter with lengths up to 1 μm, and are composed of PbTe nanoparticles of about 30–50 nm. The formation mechanism of PbTe nanorods can be reasonably explained by tellurium template-based process from the time-dependent experiments.     

Ordered arrays of high-quality single-crystalline α-Si3N4 nanowires: Synthesis,properties and applications

Ordered arrays of high-quality single-crystalline α-Si₃N₄ nanowires (NWs) have been synthesized via thermal evaporation and detailed characteristics of the NWs have been analyzed by employing scanning electron microscope (SEM) along with energy dispersive spectroscopy (EDS), high-resolution transmission electron microscope (HRTEM), X-ray diffraction (XRD), X-ray photospectroscopy (XPS), infrared (IR), photoluminescence (PL) and in situ I–V measurements by STM/TEM holder. The microscopic results revealed that the NWs having diameter in the range of ~30–100 nm and length in microns. Furthermore, the NWs are found to be single crystalline grown along [0 0 1] direction. The elemental composition and valence states of elements are analyzed by EDS and XPS. The room temperature PL spectra exhibit a broad range visible emission band. The electron transport property of a single NW illustrates the symmetric I–V curve of a semiconductor. The possible growth mechanism is also briefly discussed.     

Effect of Y2O3 addition on the phase transition and growth of YSZ nanocrystallites prepared by a sol-gel process

The effect of Y₂O₃ addition on the phase transition and growth of yttria-stabilized zirconia (YSZ) nanocrystallites prepared by a sol-gel process with various mixtures of ZrOCl₂ · 8H₂O and Y(NO₃)₃ · 6H₂O ethanol-water solutions at low temperatures has been studied. DTA/TGA, XRD, SEM, TEM and ED have been utilized to characterize the YSZ nanocrystallites. The crystallization temperature of 3YSZ, in which Y₂O₃/(Y₂O₃ + ZrO₂) = 0.03, gel powders estimated by DTA/TG is about 427 °C. When 3YSZ and 5YSZ gels are calcined at 500-700 °C, their crystal structures as composed of coexisting tetragonal and monoclinic ZrO₂, and tetragonal phase decreases with calcination temperature increasing from 500 to 700 °C. Pure cubic ZrO₂ is obtained when added Y₂O₃ is greater than 8 mol%. A nanocrystallite size distribution between 10 and 20 nm is obtained in TEM observations.     

Green synthesis of metal sulfide nanocrystals through a general composite-surfactants-aided-solvothermal process

In this paper, we developed a generalized and greener composite-surfactants-assisted-solvothermal process (CSSP) to produce colloidal nanoparticles of metal sulfides. X-ray diffraction (XRD), transmission electron microscopy (TEM), and X-ray photoelectron spectra (XPS) revealed that single-molecular-layer type of MoS₂ nanoparticles with diameter 6–10 nm were successfully synthesized. The molecular structure model of the capped MoS₂ nanoparticles was suggested through further examination by infrared spectra. Hexagonal CdS nanocrystals with spherical, triangle, and hollow sphere shapes were controllably synthesized by varying the experimental conditions. A possible in-situ reduction–sulfidation mechanism was proposed for the formation of Ag₂S nanocrystals, where the metal ions were reduced to metallic nanoparticles before the generation of sulfides. The obtained nanocrystals through this CSSP approach could provide the building blocks for the bottom-up approach to nanoscale fabrication in nanoscience and nanotechnology.     

Tetragonal tungsten oxide nanobelts synthesized by chemical vapor deposition

Tungsten trioxide (WO₃) nanobelts in tetragonal structure were grown on Si substrates by a hot-wall chemical vapor deposition (CVD) method without using catalysts. The products were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman spectroscopy, and photoluminescence (PL) spectrum. The width of the nanobelts is in the range of 50–100 nm with width-to-thickness ratios of 5–10 and lengths of up to tens of micrometers. These nanobelts grew along the [0 0 1] direction and can be identified as the tetragonal WO₃ structures. Raman and PL measurements indicate the high quality of the nanobelts. The vapor–solid growth mechanism could be applicable in our experiment.     

Effects of temperature and carrier gas flow amount on the formation of GaN nanorods by the HVPE method

We fabricated one-dimensional GaN nanorods on AlN/Si (1 1 1) substrates at various temperatures, and carrier gas flow amount, using the hydride vapor phase epitaxy (HVPE) method. An AlN buffer layer of 50 nm thickness was deposited by RF sputtering for 25 min. Stalagmite-like GaN nanorods formed at a growth temperature of 650 °C. The diameters and lengths of GaN nanorods increase with growth time, whereas the density of nanorods decreases. And we performed the experiments by changing the carrier gas flow amount at a growth temperature of 650 °C and HCl:NH₃ flow ratio of 1:40. GaN nanorods, with an average diameter of 50 nm, were obtained at a carrier gas flow amount of 1340 sccm. The shape, structures, and optical characteristics of the nanorods were investigated by field-emission scanning electron microscopy, X-ray diffraction, and photoluminescence.     

The effect of composition on UV-vis-NIR spectra of iron doped glasses in the systems Na2O/MgO/SiO2 and Na2O/MgO/Al2O3/SiO2

Glasses with the compositions xNa₂O · 10MgO · (90 − x)SiO₂, 10Na₂O · xMgO · (90 − x)SiO₂, 5Na₂O · 15MgO · xAl₂O₃ · (80 − x)SiO₂, xNa₂O · 10MgO · 10Al₂O₃ · (80 − x)SiO₂, 10Na₂O · 10MgO · xAl₂O₃ · (80 − x)SiO₂, 10Na₂O · 5MgO · 10Al₂O₃ · (80 − x)SiO₂ were melted and studied using UV-vis-NIR spectroscopy in the wavenumber range from 5000 to 30 000 cm⁻¹. At [Al₂O₃] > [Na₂O], the UV-cut off is strongly shifted to smaller wavenumbers and the NIR peak at around 10 000 cm⁻¹ attributed to Fe²⁺ in sixfold coordination gets narrower. Furthermore, the intensity of the NIR peak at 5500 cm⁻¹ increases. This is explained by the incorporation of iron in the respective glass structures.     

Investigation of structural and compositional changes in silver-doped GeO2 thin films

The processes going on in silver-doped GeO₂ films during air-heating were investigated by XPS, TEM, IR and UV-visible spectroscopy methods. Silver was shown to interact with the GeO₂ matrix at 500-600 °C to give silver germanate which was decomposed on further heating to form GeO₂ and silver nanoparticles, 10-35 nm in size, absorbing in the plasmon resonance region (λ_max = 415 nm). The silver nanoparticles are located deep in the films and encapsulated by oxide particles.