Preparation and characterization of nanocrystalline powders of bismuth vanadate

The influence of mechanical activation on the formation of Bi2VO5.5 bismuth vanadate (BiV) phase, was investigated by ball-milling a stoichiometric mixture of bismuth oxide and vanadium pentoxide. The structural evolution of the desired BN phase, via an intermediate BiVO4,phase, was investigated using X-ray powder diffraction; (XRD), differential thermal analysis (DTA) and transmission electron microscopy (TEM). Milling for 54h. yielded monophasic gamma-BiV powders with an average crystallite size of 30 nm. The electron paramagnetic resonance (EPR) peaks associated with the V4+ ions are stronger and broader in nanocrystalline (n) BN than in the conventionally prepared microcrystalline (m) BN, suggesting theta significant portion of V5+ has been transformed to V4+ during milling. The optical bandgap of n-BiV was found to be higher than that of m-BiV. High density (97% of the theoretical density), fine-grained (average grain-size of 2 tun) ceramics with uniform grain-size distribution could be fabricated using n-BiV powders. These fine-grained ceramics exhibit improved dielectric, pyre and ferroelectric properties. (C) 1999 Elsevier Science S.A. All rights reserved.

The influence of Fe3+ ions at tetrahedral sites on the magnetic properties of nanocrystalline ZnFe2O4

A systematic study on the variation of Mössbauer hyperfine parameters with grain size in nanocrystalline zinc ferrite is lacking. In the present study, nanocrystalline ZnFe2O4 ferrites with different grain sizes were prepared by ball-milling technique and characterised by X-ray, EDAX, magnetisation and Mössbauer studies. The grain size decreases with increasing milling time and lattice parameter is found to be slightly higher than the bulk value. Magnetisation at room temperature (RT) and at 77 K could not be saturated with a magnetic field of 7 kOe and the observed magnetisation at these temperatures can be explained on the basis of deviation of cation distribution from normal spinel structure. The Mössbauer spectra were recorded at different temperatures between RT and 16 K. The values of quadrupole splitting at RT are higher for the milled samples indicating the disordering of ZnFe2O4 on milling. The strength of the magnetic hyperfine interactions increases with grain size reduction and this can be explained on the basis of the distribution of Fe3+ ions at both tetrahedral and octahedral sites.

Structural, optical and nanomechanical properties of (1 1 1) oriented nanocrystalline ZnTe thin films

Structural, optical and nanomechanical properties of nanocrystalline Zinc Telluride (ZnTe) films of thickness upto 10 microns deposited at room temperature on borosilicate glass substrates are reported. X-ray diffraction patterns reveal that the films were preferentially oriented along the (1 1 1) direction. The maximum refractive index of the films was 2.74 at a wavelength of 2000 nm. The optical band gap showed strong thickness dependence. The average film hardness and Young's modulus obtained from load-displacement curves and analyzed by Oliver-Pharr method were 4 and 70 GPa respectively. Hardness of (1 1 1) oriented ZnTe thin films exhibited almost 5 times higher value than bulk. The studies show clearly that the hardness increases with decreasing indentation size, for indents between 30 and 300 nm in depth indicating the existence of indentation size effect. The coefficient of friction for these films as obtained from the nanoscratch test was ~0.4.

Structural, optical and nanomechanical properties of (1 1 1) oriented nanocrystalline ZnTe thin films

Structural, optical and nanomechanical properties of nanocrystalline Zinc Telluride (ZnTe) films of thickness upto 10 microns deposited at room temperature on borosilicate glass substrates are reported. X-ray diffraction patterns reveal that the films were preferentially oriented along the (1 1 1) direction. The maximum refractive index of the films was 2.74 at a wavelength of 2000 nm. The optical band gap showed strong thickness dependence. The average film hardness and Young's modulus obtained from load-displacement curves and analyzed by Oliver-Pharr method were 4 and 70 GPa respectively. Hardness of (1 1 1) oriented ZnTe thin films exhibited almost 5 times higher value than bulk. The studies show clearly that the hardness increases with decreasing indentation size, for indents between 30 and 300 nm in depth indicating the existence of indentation size effect. The coefficient of friction for these films as obtained from the nanoscratch test was ~0.4.

Synthesis of nanocrystalline alpha-Al2O3 by ultrasonic flame pyrolysis

Nanocrystalline alpha-alumina was synthesized in an indigenously built ultrasonic flame pyrolysis (UFP) setup. This paper describes the technical aspects of the apparatus and particle formation in the flame. Ultrasonically atomized aluminium nitrate dissolved in methanol-water mixture was pyrolyzed in an oxy-propane flame for yielding nanocrystalline alpha-alumina. The formation of nanophase alumina was confirmed by powder XRD analysis. Scanning electron microscopy (SEM) analysis was carried out to study particulate morphology. (C) 2003 Elsevier Science Ltd. All rights reserved.

Effect of irradiation on the microstructure and mechanical behavior of nanocrystalline nickel

The effect of 4.0 MeV proton irradiation on the microstructure and mechanical properties of nanocrystalline (nc) nickel was investigated. The irradiation damage induced in the sample was of the order of 0.004 dpa. Transmission electron microscopy of irradiated samples indicated the presence of dislocation loops within the grains. An increase in hardness and strain-rate sensitivity (m) of nc-Ni with irradiation was noted. The rate-controlling deformation mechanism in irradiated nc-Ni was identified to be interaction of dislocations with irradiation-induced defects. (C) 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Nanocrystalline TiO(2) preparation by microwave route and nature of anatase-rutile phase transition in nano TiO(2)

Nanopowders of TiO(2) has been prepared using a microwave irradiation-assisted route, starting from a metalorganic precursor, bis(ethyl-3-oxo-butanoato)oxotitanium (IV), [TiO(etob)(2)](2). Polyvinylpyrrolidone (PVP) was used as a capping agent. The as-prepared amorphous powders crystallize into anatase phase, when calcined. At higher calcination temperature, the rutile phase is observed to form in increasing quantities as the calcination temperature is raised. The structural and physicochemical properties were measured using XRD, FT-IR, SEM, TEM and thermal analyses. The mechanisms of formation of nano-TiO(2) from the metal-organic precursor and the irreversible phase transformation of nano TiO(2) from anatase to rutile structure at higher temperatures have been discussed. It is suggested that a unique step of initiation of transformation takes place in Ti(1/2)O layers in anatase which propagates. This mechanism rationalizes several key observations associated with the anatase rutile transformation.

Size-mediated cytotoxicity of nanocrystalline titanium dioxide, pure and zinc-doped hydroxyapatite nanoparticles in human hepatoma cells

Nanoparticles are highly used in biological applications including nanomedicine. In this present study, the interaction of HepG2 hepatocellular carcinoma cells (HCC) with hydroxyapatite (HAp), zinc-doped hydroxyapatite, and titanium dioxide (TiO2) nanoparticles were investigated. Hydroxyapatite, zinc-doped hydroxyapatite and titanium dioxide nanoparticles were prepared by wet precipitation method. They were subjected to isochronal annealing at different temperatures. Particle morphology and size distribution were characterized by X-ray diffraction and transmission electron microscope. The nanoparticles were co-cultured with HepG2 cells. MTT assay was employed to evaluate the proliferation of tumor cells. The DNA damaging effect of HAp, Zn-doped HAp, and TiO2 nanoparticles in human hepatoma cells (HepG2) were evaluated using DNA fragmentation studies. The results showed that in HepG2 cells, the anti-tumor activity strongly depend on the size of nanoparticles in HCC cells. Cell cycle arrest analysis for HAp, zinc-doped HAp, and TiO2 nanoparticles revealed the influence of HAp, zinc-doped HAp, and titanium dioxide nanoparticles on the apoptosis of HepG2 cells. The results imply that the novel nano nature effect plays an important role in the biomedicinal application of nanoparticles.

Deformation-induced thermally activated grain growth in nanocrystalline nickel

Grain growth during indentation at low temperatures has been taken to imply that grain growth is largely stress induced and athermal in nanometals. Indentation experiments on electrodeposited nano-Ni indicate clearly that the load required for grain growth decreases with an increase in temperature, suggesting strongly that concurrent grain growth is thermally activated. (C) 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Structural characterization, EPR and thermoluminescence properties of Cd-1 (-) xNixSiO3 nanocrystalline phosphors

Cd-1 - xNixSiO3 (x = 1-7 mol%) nanophosphors have been prepared for the first time by the combustion method using oxylyldihydrizide as a fuel. Powder X-ray diffraction results confirm the formation of monoclinic phase. Scanning electron micrographs show that Ni2+ influences the porosity of samples. The optical energy gap is widened with increase of Ni2+ ion dopant. The electron paramagnetic resonance spectrum of Ni2+ ions in CdSiO3 exhibits a symmetric absorption at g = 2.343 and the site symmetry around Ni2+ ions is predominantly octahedral. The number of spins participating in resonance (N) and the paramagnetic susceptibility (chi) has been evaluated. The thermoluminescence intensity is found to increase up to similar to 20 min ultra-violet exposure and thereafter, decrease with further increase of ultra-violet dose. The kinetic parameters such as activation energy (E), frequency factor (s)and order of kinetics was estimated using glow peak shape method and the results are discussed. (c) 2012 Elsevier Ltd. All rights reserved.

Synthesis of free standing nanocrystalline Cu by ball milling at cryogenic temperature

This paper reports for the first time synthesis of free standing nano-crystalline copper crystals of a similar to 30-40 nm by ball milling of copper powder at 150 K under Argon atmosphere in a specially designed cryomill. The detailed characterization of these particles using multiple techniques that includes transmission electron microscopy confirms our conclusion. Careful analysis of the chemistry of these particles indicates that these particles are essentially contamination free. Through the analysis of existing models of grain size refinements during ball milling and low temperature deformation, we argue that the suppression of thermal processes and low temperature leads to formation of free nanoparticles as the process of fracture dominates over possible cold welding at low temperatures. (C) 2012 Elsevier B.V. All rights reserved.

Surface ferromagnetism and superconducting properties of nanocrystalline niobium nitride

Nanocrystalline delta-NbNx samples have been synthesized by reacting NbCl5 and urea at three different temperatures. A comparison of their structural, magnetic, transport and thermal properties is reported in the present study. The size of the particles and their agglomeration extent increase with increasing reaction temperature. The sample prepared at 900 degrees C showed the highest superconducting transition temperature (T-c) of 16.2 K with a transition width, similar to 1.8 K, as obtained from the resistivity measurement on cold-pressed bars. Above T-c, magnetization measurements revealed the presence of surface ferromagnetism which coexists with superconductivity below T-c. Heat capacity measurements confirm superconductivity with strong electron-phonon coupling constant. The sample prepared at 800 degrees C shows a lower T-c (10 K) while that prepared at 700 degrees C exhibit no superconductivity down to the lowest temperature (3 K) measured.

CMOS-Compatible and Scalable Deposition of Nanocrystalline Zinc Ferrite Thin Film to Improve Inductance Density of Integrated RF Inductor

Development towards the combination of miniaturization and improved functionality of RFIC has been stalled due to the lack of high-performance integrated inductors. To meet this challenge, integration of magnetic material with high permeability as well as low conductivity is a must. Ferrite films are excellent candidates for RF devices due to their low cost, high resistivity, and low eddy current losses. Unlike its bulk counterpart, nanocrystalline zinc ferrite, because of partial inversion in the spinel structure, exhibits novel magnetic properties suitable for RF applications. However, most scalable ferrite film deposition processes require either high temperature or expensive equipment or both. We report a novel low temperature (< 200 degrees C) solution-based deposition process for obtaining high quality, polycrystalline zinc ferrite thin films (ZFTF) on Si (100) and on CMOS-foundry-fabricated spiral inductor structures, rapidly, using safe solvents and precursors. An enhancement of up to 20% at 5 GHz in the inductance of a fabricated device was achieved due to the deposited ZFTF. Substantial inductance enhancement requires sufficiently thick films and our reported process is capable of depositing smooth, uniform films as thick as similar to 20 mu m just by altering the solution composition. The method is capable of depositing film conformally on a surface with complex geometry. As it requires neither a vacuum system nor any post-deposition processing, the method reported here has a low thermal budget, making it compatible with modern CMOS process flow.