Low-temperature electron paramagnetic resonance in silver-iron oxide nanoparticles

Water in oil microemulsion technique has been used to obtain silver nanoparticles with a mean size of 7 nm surrounded by a matrix of 2 nm γ-Fe₂O₃ nanoparticles. Magnetic measurements of the sample exhibit a cusp in the ZFC curve at 50 K, which corresponds to the blocking temperature. A detailed study of the thermal evolution of EPR spectra has been performed in the samples. It has been shown that the linewidth, the resonance field and the intensity of the EPR line show different behaviour near the blocking temperature.     

Synthesis and X-ray structural characterization of NiO nanoparticles obtained through gelatin

Nanoparticles of fcc-NiO phase were obtained by heating the dried resin resultant of a mixture of gelatin and NiCl₂ · 6H₂O in aqueous solution. The average particle size and microstrain were calculated from the line broadening of X-ray powder diffraction peaks, and these values were between 15 nm and 78 nm, and 0.056% and 0.172%, respectively. The Rietveld refinement method was applied to all diffraction patterns. The particle size, obtained from this procedure, changes as a function of temperature, heating time and the remarkable reduction due to the addition of NaOH to the solution, which can be attributed to the presence of NaCl crystals and carbon encapsulating NiO nanoparticles during the heating. The heating temperature was in the range of 350–700 °C. Thermo-gravimetric analysis showed that the majority of organic fraction starts to disappear after 300 °C.     

Synthesis and characterization of semiconductor metal sulfide nanocrystals using microemulsion technique

The semiconductor nanocrystals ZnS, PbS, CdS and CuS were synthesized via microemulsion technique involving metal acetate, reducing agent (Na₂S) and Triton X‐100 as surfactant. Nanocrystals were characterized by X‐ray diffraction (XRD), transmission electron microscopy (TEM) and dynamic light scattering (DLS). The average size of ZnS, PbS, CdS and CuS nanocrystals were found to be 5.6 nm, 13.3 nm, 11.4 nm and 6.2 nm, respectively. Different parameters like surfactant (Triton X‐100) concentration, water‐to‐surfactant ratio (ω), precursor concentration [zinc acetate, (Zn(AC)₂], reducing agent concentration [sodium sulphide, (Na₂S)] were optimized to synthesize ZnS quantum dots.     

Optical and structural characterization of nickel selenide nanoparticles synthesized by simple methods

A series of nickel selenide (NiSe₂, NiSe and Ni₃Se₄) nanoparticles have been synthesized by three different methods, i.e. the single-source precursor (method 1), the thermolysis of trioctylphosphine selenide (TOPSe) and nickel chloride in hexadecylamine (method 2) as well as the reaction of nickel chloride and selenium using sodium borohydride as a reducing agent in methanol and in water (method 3). The optical properties of nickel selenide synthesized from all the methods showed good nanometric characteristics with an observed blue-shift in absorption band-edge from bulk nickel selenide. The structural characteristics varied with the methods employed, with method 1 producing 10 nm spherical NiSe₂ particles, method 2 star-shaped NiSe particles, while method 3 produced hexagonal NiSe nanoparticles in methanol and rod-shaped Ni₃Se₄ particles in water.     

Amorphous iron-chromium oxide nanoparticles prepared by sonochemistry

Amorphous Fe₂O₃ and Fe_1.9Cr_0.1O₃ materials have been prepared by sonochemical method. X-ray diffraction patterns, transmission electron microscopy, Raman and infrared spectra, differential scanning calorimetry, Mössbauer and magnetic measurements revealed many interesting behaviors of the samples. Reaction to form the materials only occurred at the preparation temperatures of 70 °C or above. Upon heating, the sample prepared at 70°C presented a strong ferromagnetic behavior due to the presence of the magnetite phase coexisting with the hematite phase whereas the samples prepared at higher temperatures presented only the existence of the hematite phase. Thermal analyses of the sample prepared at 80°C revealed three exothermic peaks which were corresponding to the phase changes of dehydroxylation, crystallization of the maghemite phase and maghemite–hematite transition, respectively. The activation energies of the phase changes deduced from the thermal analyses showed that the presence of Cr enhanced the activation energy which can slow down the ageing effect of the amorphous state when being used in practice.     

Growth and characterization of Nd,Yb – yttrium oxide nanopowders obtained by sol‐gel method

Nanopowders of Y₂O₃ pure, doped and codoped by Nd³⁺, Yb³⁺ were obtained by sol‐gel method. Solution with ethylene glycol was choosed as the proper solution where crystallites of powder with Nd and Yb dopants had the same size. Finally the one‐phased compounds of Y₂O₃ doped 0.5 at% Nd and 1, 2 or 4 at% Yb were obtained. Grain growth and their morphology were investigated in various temperature and time of heating. The changes of crystallite sizes and lattice constants in relation to the heating time and temperature for the composition Y₂O₃ doped 0.5 at% Nd and 2 at% Yb are presented. Y₂O₃ containing 0,5 at% of Nd exhibits intense luminescence bands centered at 920 nm, 1100 nm and 1360 nm whereas a single band at about 1020 nm appears in samples co‐doped with neodymium and ytterbium. Luminescence spectra recorded did not depend on the sample preparation procedure and size of grains. OH impurity affects critically the relaxation dynamics of luminescent ion in nanopowders. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation and characterization of Si sheets by renewed SSP technique

Silicon sheets from powder (SSP) ribbons have been prepared by modified SSP technique using electronic-grade (9N purity) silicon powder. The surface morphology, crystallographic quality, composition and electric properties of the SSP ribbons were investigated by surface profiler, X-ray diffraction (XRD), scanning electron microscopy (SEM), metallurgical microscope, Auger electron spectroscopy (AES) and four-point probe apparatus, respectively. The results show that the SSP ribbon made from electronic-grade silicon powder is a suitable candidate for the substrates of crystalline silicon thin film (CSiTF) solar cells, which could meet the primary requirements of CSiTF solar cell process on the substrates, including surface smoothness, crystallographic quality, purity and electric conductivity, etc.     

Preparation and characterization of ZnO-TiO2 films obtained by sol-gel method

The sol-gel route has been applied to obtain ZnO-TiO₂ thin films. For comparison, pure TiO₂ and ZnO films are also prepared from the corresponding solutions. The films are deposited by a spin-coated method on silicon and glass substrates. Their structural and vibrational properties have been studied as a function of the annealing temperatures (400-750 °C). Pure ZnO films crystallize in a wurtzite modification at a relatively low temperature of 400 °C, whereas the mixed oxide films show predominantly amorphous structure at this temperature. XRD analysis shows that by increasing the annealing temperatures, the sol-gel Zn/Ti oxide films reveal a certain degree of crystallization and their structures are found to be mixtures of wurtzite ZnO, Zn₂TiO₄, anatase TiO₂ and amorphous fraction. The XRD analysis presumes that Zn₂TiO₄ becomes a favored phase at the highest annealing temperature of 750 °C. The obtained thin films are uniform with no visual defects. The optical properties of ZnO-TiO₂ films have been compared with those of single component films (ZnO and TiO₂). The mixed oxide films present a high transparency with a slight decrease by increasing the annealing temperature.     

Precipitation and characterization of hollow calcite nanoparticles

A method for preparation of significant amount of hollow rhombohedral calcite nanoparticles, based on carbonation of calcium hydroxide suspension, is described. The mineralogical and morphological analyses of the precipitate confirmed the existence of exclusively stable polymorphic modification, calcite, with the mean particle size of about 100 nm and the diameter of the holes observed at the surfaces that are about 50 nm. The analysis of carbonation kinetics pointed out to a complex mechanism of hollow particles formation at high initial supersaturation, that assumed nucleation of amorphous precursor calcium carbonate phase and its solution mediated transformation into nanosized crystalline calcite. The holes obtained at the calcite surfaces are most probably the imprints remained after the dissolution of amorphous calcium carbonate particles.     

Growth of YCOB single crystals by flux technique and their characterization

Nonlinear optical single crystals of YCOB with good optical quality were grown by the flux technique for the first time. Polycrystalline YCOB samples were synthesized by solid state reaction method. The thermal analysis of the sample was performed with lithium carbonate flux in different weight proportions and the growth temperature was optimised. Single crystals of YCOB with dimensions 3 × 3 × 5 mm³ were obtained by the method of ‘slow‐cooling’. The grown crystals were characterized by XRD, UV‐VIS‐NIR, EDAX, FTIR and etching studies. The powder XRD pattern revealed the formation of YCOB compound. The lattice parameters were identified through single crystal XRD studies. The UV‐VIS‐NIR results showed that the crystal has a sharp cutoff at 220 nm and is nearly 55% transparent over a wide wavelength range enabling applications in the UV region. The EDAX measurement revealed the ‘flux‐free’ crystal formation. The presence of the functional groups belonging to the YCOB crystals was identified by the FTIR results. ‘Hillock‐like’ patterns are observed in the etching studies. The primary emphasis in this study is laid to describe ‘flux technique’ as an alternative method to grow YCOB crystals. The results are presented and discussed. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Green synthesis by diethylene glycol based solution process and characterization of SnS nanoparticles

Uniform near‐spherical SnS nanoparticles were prepared by a hydrazine hydrate‐assisted diethylene glycol solution synthesis based on the reaction of tin dichloride (SnCl₂·2H₂O) with thioacetamide (H₃CCSNH₂). The as‐prepared SnS nanoparticles were characterized by XRD, FETEM, EDS, XPS and UV‐vis‐NIR spectrophotometer. The results showed that the SnS nanoparticles had orthorhombic crystal structure, good stoichiometry and indirect bandgap of ∼1.1 eV. The nanoparticle size could be controlled by changing injection temperature. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation and characterization of hcp Co-coated Fe nanoparticles

A relatively simple method was described for coating and modifying iron nanoparticles with a hexagonal close-packed (hcp) cobalt layer. It was realized by depositing cobalt onto the poly(N-vinyl-2-pyrrolidone) (PVP) modified iron particles in ethanol solution. XRD, XPS and HRTEM were used to characterize the product. The Co layers, grown as the exclusive hcp phase, were ascribed to the inducement of the body-centered cubic (bcc) iron cores. Thus-prepared hcp Co-coated Fe particles displayed a much enhanced coercivity and decreased saturation magnetization (M_S) compared with that of the uncoated sample.     

Magnetization and structural studies of Mn doped ZnO nanoparticles: Prepared by reverse micelle method

Single phase Mn (2.5 at%) doped ZnO nanocrystalline samples were synthesized by reverse micelle method as characterized by Rietveld refinement analysis of X-ray diffraction data, high resolution transmission electron microscopy and selected area electron diffraction analyses. The X-ray photoelectron spectroscopy and electron paramagnetic resonance (EPR) studies indicated that manganese exist as Mn²⁺ in ZnO lattice. DC magnetization measurements as a function of field and temperature, of 2.5 at% Mn doped ZnO nanoparticles annealed at 675 K, showed room temperature ferromagnetism (RTF). This observation is further confirmed by the EPR spectrum of the sample, which shows a distinct ferromagnetic resonance signal at room temperature. These results indicate that the observed RTF in Mn-doped ZnO may be attributed to the substitutional incorporation of Mn at Zn sites.     

Effect of Cr doping on the structural and optical properties of ZnS nanoparticles

Zn_1−xCr_x S nanoparticles with x = 0.00, 0.005, 0.01, 0.02 and 0.03 were synthesized by chemical co‐precipitation method at room temperature for the first time. Ethylene diamine tetraacetic acid was used as stabilizer. Energy dispersive analysis of X‐rays confirmed the presence of Cr in the samples. The samples were characterized by scanning electron microscopy, X‐ray diffraction (XRD), transmission electron microscopy and optical absorption studies. XRD and selected area electron diffraction results showed that the samples of all compositions crystallized in cubic structure and the lattice parameters decreased linearly with increase in Cr content following Vegard's law indicating that the Cr ions have substituted for Zn in the ZnS lattice. The particle size estimated from XRD was in the range 6–10 nm.The optical absorption studies on the doped samples indicated that the absorption edge blue shifted with respect to those of bulk and nanocrystalline ZnS. The bandgap increased with increasing Cr concentration in a narrow range 3.81–4.03 eV. Photolumonesence studies showed blue emission with appreciable luminescence quenching with increasing Cr concentration. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Comparative analysis of the structural and morphological features of biogenic and synthesized goethite nanoparticles

Crystallography Reports - A comparative analysis of the relationship between the morphological forms and magnetic properties of natural goethite particles from the crust of weathering of the Far...     

The synthesis and structural characterization of silyl-substituted fluorenes

Three silyl-substituted fluorenes have been prepared by direct synthetic methods and structurally characterized by X-ray diffraction. The three silyl-substituted fluorenes studied were 9-trimethylsilylfluorene (1), 9-(tert-butyldimethyl)silylfluorene (2), and 2,7-di-tert-butyl-9-trimethylsilylfluorene (3). Complex 1 is orthorhombic, P2₁2₁2₁, a = 6.2681(14) Å, b = 14.329(3) Å, c = 15.231(4) Å, Z = 4. Complex 2 is monoclinic, P2₁/c, a = 12.1953(10) Å, b = 6.9977(6) Å, c = 19.6536(17) Å, = 93.818(2), Z = 4. Complex 3 is monoclinic, P2₁/c, a = 11.9954(9) Å, b = 9.8978(7) Å, c = 18.5464(13) Å, = 92.456(2), Z = 4. The long carbon–silicon bonds effectively remove any significant intramolecular interactions as little distortion is exhibited around the sp ³-carbon atom and the fluorenyl backbone demonstrates near planarity. The bulky silicon substituents also prevent intermolecular interactions, as only a few close contacts less than 4.0 Å exist in all three solid state structures.     

Synthesis and structural characterization of potato starch sponges

Materials with hierarchical porous structures have attracted great attention over the past years since they have been widely used in many industrial applications. Starch stands out among the materials commonly used as sacrificial templates in environmentally friendly applications. In addition, starch is inexpensive, easy to process, and readily available. In this work we present a structural characterization of sponges prepared by freezing and thawing of a starch gel. Samples obtained in this study were examined by scanning electron microscopy (SEM) and X-ray microtomography (μ-CT). SEM tests revealed that these samples show an open macroporous framework with continuous walls. μ-CT tests revealed that it is possible to tailor the pore structure of these materials by changing the starch concentration in gels used in their processing. We noticed that increasing starch concentration from 15 wt.% to 60 wt.% leads to sponges with porosities ranging from about 28% to over 65%. It was also observed that the higher the starch concentration, the greater the mean pore size of the prepared sponge.     

Synthesis, characterization and dye adsorption of ilmenite nanoparticles

FeTiO₃ nanoparticles (nano-FeTiO₃ or nano-ilmenite) can be synthesized by the sol-gel method. In this study, the physical properties and dye adsorption characteristics of nano-FeTiO₃ are investigated. A synthesized nano-ilmenite has a particle size of approximately 20 to 60 nm with a polycrystalline structure. The FeTiO₃ nanoparticles exhibit weak ferromagnetism and show high adsorption capacity for methylene blue. Experimental data are fitted to pseudo-first-order and pseudo-second-order equations; the pseudo-first-order model is found to be more suitable. It also suggests that the Langmuir isotherm is more adequate than the Freundlich isotherm in simulating the adsorption isotherm of organic dye. The maximum adsorption capacity is 71.9 mg/g, therefore, the magnetic FeTiO₃ nanoparticles show a considerably high adsorption capacity for organic dyes in a solution. These findings indicate that the nano-ilmenite is an effective material for dye removal and can be used to alleviate environmental problems.     

Electronic conductivity and structural chemistry in Li-Te-V oxide glasses

The electronic conductivity of the Li₂O-Te₂V₂O₉ glass system reveals that, even for high lithium content, electron hopping occurs between V⁴⁺ and V⁵⁺. The study of the V⁴⁺ content versus various syntheses shows that more than lithium content, the nature of the counter ion used in Li⁺ reagent and its decomposition behavior are responsible for the efficiency of the spontaneous V⁵⁺ reduction via a ‘sprouting’ phenomenon. The electron hopping process implies interconnection of VO_n polyhedra which are accessible for both V⁴⁺ and V⁵⁺ species. Such fact gives information about short and medium range ordering in the glasses. On the basis of the LiVTeO₅ crystal structure and in agreement with wide angle X-ray scattering experiments, a possible rearrangement bringing together VO₅ square pyramids is proposed to explain the electron hopping. Such proposal corresponds to a lithium network forming effect. It could explain why for Li/V>1 the electronic conductivity increases with lithium content while the V⁴⁺ amount remains low.