Effect of Sm3+-Gd3+ on structural, electrical and magnetic properties of Mn-Zn ferrites synthesized via combustion route

Nanocrystalline Mn0.4Zn0.6SmxGdyFe2-(x+y)O4 (x = y = 0.01, 0.02, 0.03, 0.04 and 0.05) were synthesized by combustion route. The detailed structural studies were carried out through X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM). The results confirms the formation of mixed spine phase with cubic structure due to the distortion created with co-dopants substitution at Fe site in Mn-Zn ferrite lattice. Further, the crystallite size increases with an increase of Sm3+-Gd3+ ions concentration while lattice parameter and lattice strain decreases. Furthermore, the effect of Sm-Gd co-doping in Mn-Zn ferrite on the room temperature electrical (dielectric studies) studies were carried out in the wide frequency range 1 GHz-5 GHz. The magnetic studies were carried out using vibrating sample magnetometer (VSM) under applied magnetic field of 1.5T and also room temperature electron paramagnetic resonance (EPR) spectra's were recorded. From the results of dielectric studies, it shows that the real and imaginary part of permittivities are increasing with variation of Gd3+ and Sm3+ concentration. The magnetic studies reveal the decrease of remnant, saturation magnetization and coercivity with increasing of Sm3+-Gd3+ ion concentration. The g-value, peak-to-peak line width and spin concentration evaluated from EPR spectra correlated with cations occupancy. The electromagnetic properties clearly indicate that these materials are the good candidates which are useful at L and C band frequency. (C) 2015 Elsevier B.V. All rights reserved.

Anomalous reduction in domain wall displacement at the morphotropic phase boundary of the piezoelectric alloy system PbTiO3-BiScO3

A comparative study of field-induced domain switching and lattice strain was carried out by in situ electric-field-dependent high-energy synchrotron x-ray diffraction on a morphotropic phase boundary (MPB) and a near-MPB rhombohedral/pseudomonoclinic composition of a high-performance piezoelectric alloy (1-x) PbTiO3-(x)BiScO3. It is demonstrated that the MPB composition showing large d(33) similar to 425 pC/N exhibits significantly reduced propensity of field-induced domain switching as compared to the non-MPB rhombohedral composition (d(33) similar to 260 pC/N). These experimental observations contradict the basic premise of the martensitic-theory-based explanation which emphasizes on enhanced domain wall motion as the primary factor for the anomalous piezoelectric response in MPB piezoelectrics. Our results favor field-induced structural transformation to be the primary mechanism contributing to the large piezoresponse of the critical MPB composition of this system.

Cyclic Deformation Of Nanocrystalline And Ultrafine-Grained Nickel

The cyclic deformation behavior Of ultrafine-grained (UFG) Ni samples synthesized by the electrodeposition method was studied. Different from those made by severely plastic deformation, the UFG samples used in this study are characterized by large-angle grain boundaries. Behaviors from nanocrystalline Ni and coarse-grained Ni samples were compared with that Of Ultrafine-grained Ni. With in situ neutron diffraction. unusual evolutions of residual lattice strains as well as cyclic hardening and softening behavior were demonstrated during the cyclic deformation. The microstructural changes investigated by TEM are discussed with respect to the unusual lattice strain and cyclic hardening/softening. (C) 2008 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Scanning tunneling spectroscopic studies on high-temperature superconductors and Dirac materials

This thesis details the investigations of the unconventional low-energy quasiparticle excitations in electron-type cuprate superconductors and electron-type ferrous superconductors as well as the electronic properties of Dirac fermions in graphene and three-dimensional strong topological insulators through experimental studies using spatially resolved scanning tunneling spectroscopy (STS) experiments.

Magnetic-field- and temperature-dependent evolution of the spatially resolved quasiparticle spectra in the electron-type cuprate La_0.1Sr_0.9CuO₂ (La-112) T_C = 43 K, are investigated experimentally. For temperature (T) less than the superconducting transition temperature (TC), and in zero field, the quasiparticle spectra of La-112 exhibits gapped behavior with two coherence peaks and no satellite features. For magnetic field measurements at T < TC, first ever observation of vortices in La-112 are reported. Moreover, pseudogap-like spectra are revealed inside the core of vortices, where superconductivity is suppressed. The intra-vortex pseudogap-like spectra are characterized by an energy gap of V_PG = 8.5 ± 0.6 meV, while the inter-vortex quasiparticle spectra shows larger peak-to-peak gap values characterized by Δ_pk-pk(H) >V_PG, and Δ_pk-pk (0)=12.2 ± 0.8 meV > Δ_pk-pk (H > 0). The quasiparticle spectra are found to be gapped at all locations up to the highest magnetic field examined (H = 6T) and reveal an apparent low-energy cutoff at the V_PG energy scale.

Magnetic-field- and temperature-dependent evolution of the spatially resolved quasiparticle spectra in the electron-type "122" iron-based Ba(Fe_1-xCo_x)₂A_s2 are investigated for multiple doping levels (x = 0.06, 0.08, 0.12 with T_C= 14 K, 24 K, and 20 K). For all doping levels and the T < T_C, two-gap superconductivity is observed. Both superconducting gaps decrease monotonically in size with increasing temperature and disappear for temperatures above the superconducting transition temperature, T_C. Magnetic resonant modes that follow the temperature dependence of the superconducting gaps have been identified in the tunneling quasiparticle spectra. Together with quasiparticle interference (QPI) analysis and magnetic field studies, this provides strong evidence for two-gap sign-changing s-wave superconductivity.

Additionally spatial scanning tunneling spectroscopic studies are performed on mechanically exfoliated graphene and chemical vapor deposition grown graphene. In all cases lattice strain exerts a strong influence on the electronic properties of the sample. In particular topological defects give rise to pseudomagnetic fields (B ~ 50 Tesla) and charging effects resulting in quantized conductance peaks associated with the integer and fractional Quantum Hall States.

Finally, spectroscopic studies on the 3D-STI, Bi₂Se₃ found evidence of impurity resonance in the surface state. The impurities are in the unitary limit and the spectral resonances are localized spatially to within ~ 0.2 nm of the impurity. The spectral weight of the impurity resonance diverges as the Fermi energy approaches the Dirac point and the rapid recovery of the surface state suggests robust topological protection against perturbations that preserve time reversal symmetry.

Structural evolution of mechanically alloyed nanocrystalline FeAl intermetallics

Nanostructured FeAl intermetallics were prepared directly by mechanical alloying (MA) in a high-energy planetary ball-mill. The phase transformations and structural changes occurring in the studied material during mechanical alloying were investigated by X-ray diffraction (XRD). Transmission electron microscopy (TEM) was employed to examine the morphology of the powders. Thermal behavior of the milled powders was examined by differential scanning calorimetry (DSC). Disordered Fe(Al) solid solution was formed at the early stage. After 30 h of milling, Fe(Al) solid solution transformed into an ordered FeAl phase. The average crystallite size reduction down to about 12 nm was accompanied by the introduction of the average lattice strain up to 1.7%. The TEM picture showed that the size of milled powders was less than 30 nm. (c) 2007 Elsevier B.V. All rights reserved.

The formation and stability of Si1-xCx alloys in Si implanted with carbon

Si1-xCx alloys of carbon (C) concentration between 0.6%-1.0% were grown in Si by ion implantation and high temperature annealing. The formation of Si1-xCx alloys under different ion doses and their stability during annealing were studied. If the implanted dose was less than that for amorphizing Si crystals, the implanted C atoms would like to combine with defects produced during implantation and it was difficult to form Si1-xCx alloys after being annealed at 850 degreesC. With the increment of implanted C ion doses, the lattice damage increased and it was easier to form Si1-xCx alloys. But the lattice strain would become saturate and only part of implanted carbon atoms would occupy the substitutional positions to form Si1-xCx alloys as the implanted carbon dose increased to a certain degree. Once Si1-xCx alloys were formed, they were stable at 950 degreesC, but part of their strain would release as the annealing temperature increased to 1 000 degreesC. Stability of the alloys became worse with the increment of carbon concentration in the alloys.

Study on the oxygen concentration reduction in heavily Sb-doped silicon

It was determined that oxygen concentration in heavily Sb-doped silicon was about 40% lower than that in the lightly doped Czochralski grown silicon and decreased with increasing content of Sb by means of coincident elastic recoil detection analysis. Through thermodynamic calculation, the oxygen loss by evaporation from the free surface of melt is only due to the formation of SiO, and Sb2O3 evaporation can be neglected. The basic reason for oxygen concentration reduction in heavily Sb-doped CZSi was that oxygen solubility decreased when element Sb with larger radius doped degenerately into silicon crystal. (C) 1999 Elsevier Science B.V. All rights reserved.

Structural ordering and interface morphology in symmetrically strained (GaIn)As/Ga(PAs) superlattices grown on off-oriented GaAs(100)

In this work we investigate the structural properties of symmetrically strained (GaIn)As/GaAs/Ga(PAs)/GaAs superlattices by means of x-ray diffraction, reciprocal-space mapping, and x-ray reflectivity. The multilayers were grown by metalorganic vapor-phase epitaxy on (001) GaAs substrates intentionally off-oriented towards one of the nearest [110] directions. High-resolution triple-crystal reciprocal-space maps recorded for different azimuth angles in the vicinity of the (004) Bragg diffraction clearly show a double periodicity of the x-ray peak intensity that can be ascribed to a lateral and a vertical periodicity occurring parallel and perpendicular to the growth surface. Moreover, from the intensity modulation of the satellite peaks, a lateral-strain gradient within the epilayer unit cell is found, varying from a tensile to a compressive strain. Thus, the substrate off-orientation promotes a lateral modulation of the layer thickness (ordered interface roughness) and of the lattice strain, giving rise to laterally ordered macrosteps. In this respect, contour maps of the specular reflected beam in the vicinity of the (000) reciprocal lattice point were recorded in order to inspect the vertical and lateral interface roughness correlation, A semiquantitative analysis of our results shows that the interface morphology and roughness is greatly influenced by the off-orientation angle and the lateral strain distribution. Two mean spatial wavelengths can be determined, one corresponding exactly to the macrostep periodicity and the other indicating a further interface waviness along the macrosteps. The same spatial periodicities were found on the surface by atomic-force-microscopy images confirming the x-ray results and revealing a strong vertical correlation of the interfaces up to the outer surface.

Effects of helium and oxygen common implantation in silicon wafer

Defect engineering for SiO2] precipitation is investigated using He-ion implantation as the first stage of separation by implanted oxygen (STMOX). Cavities are created in Si by implantation with helium ions. After thermal annealing at different temperatures, the sample is implanted with 120keV 8.0 x 10(16) cm(-2) O ions. The O ion energy is chosen such that the peak of the concentration distribution is centred at the cavity band. For comparison, another sample is implanted with O ions alone. Cross-sectional transmission electron microscopy (XTEM), Fourier transform infrared absorbance spectrometry (FTIR) and atomic force microscopy (AFM) measurements are used to investigate the samples. The results show that a narrow nano-cavity layer is found to be excellent nucleation sites that effectively assisted SiO2 formation and released crystal lattice strain associated with silicon oxidation.

Enhanced shape anisotropy and magneto-optical birefringence by high energy ball milling in NixFe1−xFe2O4 ferrofluids

Ferrofluids belonging to the series NixFe1 xFe2O4 were synthesised by two different procedures—one by standard co-precipitation techniques, the other by co-precipitation for synthesis of particles and dispersion aided by high-energy ball milling with a view to understand the effect of strain and size anisotropy on the magneto-optical properties of ferrofluids. The birefringence measurements were carried out using a standard ellipsometer. The birefringence signal obtained for chemically synthesised samples was satisfactorily fitted to the standard second Langevin function. The ball-milled ferrofluids showed a deviation and their birefringence was enhanced by an order. This large enhancement in the birefringence value cannot be attributed to the increase in grain size of the samples, considering that the grain sizes of sample synthesised by both modes are comparable; instead, it can be attributed to the lattice strain-induced shape anisotropy(oblation) arising from the high-energy ball-milling process. Thus magnetic-optical (MO) signals can be tuned by ball-milling process, which can find potential applications.

Enhanced shape anisotropy and magneto-optical birefringence by high energy ball milling in NixFe1 xFe2O4 ferrofluids

Ferrofluids belonging to the series NixFe1 xFe2O4 were synthesised by two different procedures—one by standard co-precipitation techniques, the other by co-precipitation for synthesis of particles and dispersion aided by high-energy ball milling with a view to understand the effect of strain and size anisotropy on the magneto-optical properties of ferrofluids. The birefringence measurements were carried out using a standard ellipsometer. The birefringence signal obtained for chemically synthesised samples was satisfactorily fitted to the standard second Langevin function. The ball-milled ferrofluids showed a deviation and their birefringence was enhanced by an order. This large enhancement in the birefringence value cannot be attributed to the increase in grain size of the samples, considering that the grain sizes of sample synthesised by both modes are comparable; instead, it can be attributed to the lattice strain-induced shape anisotropy(oblation) arising from the high-energy ball-milling process. Thus magnetic-optical (MO) signals can be tuned by ball-milling process, which can find potential applications

Time and spatial resolution of slip and twinning in a grain embedded within a magnesium polycrystal

Plastic yielding in magnesium alloys frequently involves the initiation of both slip and twinning events. A proper understanding of the phenomenon at the grain level requires knowledge of how these two mechanisms progress and interact over both time and space and what the local resolved stresses are. To date, simultaneous collection of such information has not been achievable. To address this shortfall, we have developed a modified Laue based in situ micro X-ray diffraction technique with an unprecedented combination of time and spatial resolution. A ten-fold reduction in data collection times is realized by the refinement of rapid polychromatic Laue "single-shot" mapping. From single Laue patterns, we extract grain depth information, detect onset of yielding and achieve 2 × 10-4 lattice strain resolution. The technique is employed to examine yielding and twinning in a magnesium grain embedded ∼200 μm below the sample surface. We examine 13 time steps and reveal the following behaviour: initial onset of basal slip, subsequent onset of twinning, development of further accommodation slip and evolution of twin shape and size; along with the corresponding values of local resolved shear stresses. © 2014 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Development of a laboratory-based transmission diffraction technique for in situ deformation studies of Mg alloys

A laboratory-based transmission X-ray diffraction technique was developed to measure elastic lattice strains parallel to the loading direction during in situ tensile deformation. High-quality transmission X-ray diffraction data were acquired in a time frame suitable for in situ loading experiments by application of a polycapillary X-ray optic with a conventional laboratory Cu X-ray source. Based on the measurement of two standard reference materials [lanthanum hexaboride (NIST SRM 660b) and silicon (NIST SRM 640c)], precise instrumental alignment and calibration of the transmission diffraction geometry were realized. These results were also confirmed by the equivalent data acquired using the standard Bragg-Brentano measurement geometry. An empirical Caglioti function was employed to describe the instrumental broadening, while an axis of rotation correction was used to measure and correct the specimen displacement from the centre of the goniometer axis. For precise Bragg peak position and hkil intensity information, a line profile fitting methodology was implemented, with Pawley refinement used to measure the sample reference lattice spacings (d o (hkil)). It is shown that the relatively large X-ray probe size available (7 × 714mm) provides a relatively straightforward approach for improving the grain statistics for the study of metal alloys, where grain sizes in excess of 114μm can become problematic for synchrotron-based measurements. This new laboratory-based capability was applied to study the lattice strain evolution during the elastic-plastic transition in extruded and rolled magnesium alloys. A strain resolution of 2 × 10-4 at relatively low 2θ angles (20-65° 2θ) was achieved for the in situ tensile deformation studies. In situ measurement of the elastic lattice strain accommodation with applied stress in the magnesium alloys indicated the activation of dislocation slip and twin deformation mechanisms. Furthermore, measurement of the relative change in the intensity of 0002 and 10 3 was used to quantify {10 2} 011 tensile twin onset and growth with applied load.

Estudo da moagem de alta energia e sinterização de pós compósitos W-Cu

The Tungsten/copper composites are commonly used for electrical and thermal objectives like heat sinks and lectrical conductors, propitiating an excellent thermal and electrical conductivity. These properties are dependents of the composition, crystallite size and production process. The high energy milling of the powder of W-Cu produces an dispersion high and homogenization levels with crystallite size of W very small in the ductile Cu phase. This work discusses the effect of the HEM in preparation of the W-25Cu composite powders. Three techniques of powder preparation were utilized: milling the dry with powder of thick Cu, milling the dry with powder of fine Cu and milling the wet with powder of thick Cu. The form, size and composition of the particles of the powders milled were observed by scanning electron microscopy (SEM). The X-ray diffraction (XRD) was used to analyse the phases, lattice parameters, size and microstrain of the crystallite. The analyse of the crystalline structure of the W-25Cu powders milled made by Rietveld Method suggests the partial solid solubility of the constituent elements of the Cu in lattice of the W. This analyse shows too that the HEM produces the reduction high on the crystallite size and the increase in the lattice strain of both phases, this is more intense in the phase W

Análise do efeito do tempo da moagem de alta energia no tamanho de cristalito e microdeformação da rede cristalina do WC-Co

Hard metals are the composite developed in 1923 by Karl Schröter, with wide application because high hardness, wear resistance and toughness. It is compound by a brittle phase WC and a ductile phase Co. Mechanical properties of hardmetals are strongly dependent on the microstructure of the WC Co, and additionally affected by the microstructure of WC powders before sintering. An important feature is that the toughness and the hardness increase simultaneously with the refining of WC. Therefore, development of nanostructured WC Co hardmetal has been extensively studied. There are many methods to manufacture WC-Co hard metals, including spraying conversion process, co-precipitation, displacement reaction process, mechanochemical synthesis and high energy ball milling. High energy ball milling is a simple and efficient way of manufacturing the fine powder with nanostructure. In this process, the continuous impacts on the powders promote pronounced changes and the brittle phase is refined until nanometric scale, bring into ductile matrix, and this ductile phase is deformed, re-welded and hardened. The goal of this work was investigate the effects of highenergy milling time in the micro structural changes in the WC-Co particulate composite, particularly in the refinement of the crystallite size and lattice strain. The starting powders were WC (average particle size D50 0.87 μm) supplied by Wolfram, Berglau-u. Hutten - GMBH and Co (average particle size D50 0.93 μm) supplied by H.C.Starck. Mixing 90% WC and 10% Co in planetary ball milling at 2, 10, 20, 50, 70, 100 and 150 hours, BPR 15:1, 400 rpm. The starting powders and the milled particulate composite samples were characterized by X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) to identify phases and morphology. The crystallite size and lattice strain were measured by Rietveld s method. This procedure allowed obtaining more precise information about the influence of each one in the microstructure. The results show that high energy milling is efficient manufacturing process of WC-Co composite, and the milling time have great influence in the microstructure of the final particles, crushing and dispersing the finely WC nanometric order in the Co particles