Magneto-transport behaviour of Bi2Se3-xTex : role of disorder.

Magneto-resistance and Hall resistance measurements have been carried out in fast-cooled single crystals of Bi2Se3-xTex (x = 0 to 2) in 4-300 K temperature range, under magnetic fields up to 15 T. The variation of resistivity with temperature that points to a metallic behaviour in Bi2Se3, shows an up-turn at low temperatures in the Te doped samples. Magneto-resistance measurements in Bi2Se3 show clear signatures of Shubnikov-de Hass (SdH) oscillations that gets suppressed in the Te doped samples. In the Bi2SeTe2 sample, the magneto-resistance shows a cusp like positive magneto-resistance at low magnetic fields and low temperatures, a feature associated with weak anti-localisation (WAL), that crosses over to negative magneto-resistance at higher fields. The qualitatively different magneto-transport behaviour seen in Bi2SeTe2 as compared to Bi2Se3 is rationalised in terms of the disorder, through an estimate of the carrier density, carrier mobility and an analysis in terms of the Ioffe-Regel criterion with support from Hall Effect measurements. We demonstrate that by introducing Te, in the strongly disordered samples a smooth crossover of SdH and WAL can be seen in the Bi2Se3-xTex series, both of which provide signatures for the presence of topological surface states.

Quantification of oxide particle composition in model oxide dispersion strengthened steel alloys.

Oxide dispersion strengthened ferritic steels (ODS) are being considered for structural components of future designs of fission and fusion reactors because of their impressive high-temperature mechanical properties and resistance to radiation damage, both of which arise from the nanoscale oxide particles they contain. Because of the critical importance of these nanoscale phases, significant research activity has been dedicated to analysing their precise size, shape and composition (Odette et al., Annu. Rev. Mater. Res. 38 (2008) 471-503 [1]; Miller et al., Mater. Sci. Technol. 29(10) (2013) 1174-1178 [2]). As part of a project to develop new fuel cladding alloys in India, model ODS alloys have been produced with the compositions, Fe-0.3Y2O3, Fe-0.2Ti-0.3Y2O3 and Fe-14Cr-0.2Ti-0.3Y2O3. The oxide particles in these three model alloys have been studied by APT in their as-received state and following ion irradiation (as a proxy for neutron irradiation) at various temperatures. In order to adequately quantify the composition of the oxide clusters, several difficulties must be managed, including issues relating to the chemical identification (ranging and variable peak-overlaps); trajectory aberrations and chemical structure; and particle sizing. This paper presents how these issues can be addressed by the application of bespoke data analysis tools and correlative microscopy. A discussion follows concerning the achievable precision in these measurements, with reference to the fundamental limiting factors.

Structural investigations in BaFe(2-x)Ru(x)As2 as a function of Ru and temperature.

We present the results of synchrotron X-ray diffraction (XRD) measurements on powdered single-crystal samples of BaFe(2-x)Ru(x)As2, as a function of Ru content, and as a function of temperature, across the spin-density wave transition in BaFe(1.9)Ru(0.1)As2. The Rietveld refinements reveal that with Ru substitution, while the a-axis increases, the c-axis decreases. In addition, the variation of positional coordinates of As (z(As)), the Fe-As bond length and the As-Fe-As bond angles have also been determined. In the sample with x = 0.1, temperature-dependent XRD measurements indicate that the orthorhombicity shows the characteristic increase with a decrease in temperature, below the magnetic transition. It is seen that the c-axis, the As-Fe-As bond angles, Fe-As bond length and positional coordinates of the As show definite anomalies close to the structural transition. The observed anomalies in structural parameters are analysed in conjunction with restricted geometric optimization of the structure using ab initio electronic structure calculations.

Effect of surface stress on microcantilever resonance frequency during water adsorption: influence of microcantilever dimensions.

This paper reports the effect of dimensions of microcantilever (MC) on its resonance frequency and bending upon adsorption of water molecules. Study is conducted on three MCs having the dimensions of 450 × 40 × 2.5 µm(3) (MC1), 225 × 30 × 3 µm(3) (MC2) and 125 × 35 × 4.5 µm(3) (MC3). The measured resonant frequency showed the expected negative shift in MC1, initially positive followed by a negative shift in MC2 and only positive shift in MC3 during adsorption. This behavior is attributed to changes in the stiffness of the MC associated with the surface stress. The surface stress generated on the MC has been derived from its bending measurements upon water adsorption. The change in the stiffness of MC evaluated from an independent estimate of expected frequency shift showed that the relative stiffness change of MC increases linearly with the surface stress scaled with cube of width to height ratio of MCs, confirming the dimensional dependence of adsorption induced stiffness change.

57Fe Mössbauer studies across the spin density wave transition in BaFe2-xRuxAs2.

Mössbauer measurements have been carried out in powdered single crystalline samples of BaFe(2-x)RuxAs(2), for Ru concentration in the x = 0.0-0.5 range. The internal hyperfine field (B(hf)) measured at 5 K is found to decrease with an increase in Ru concentration, consistent with the disappearance of a magnetic ground state with Ru substitution. The temperature dependent Mössbauer measurements have been used to study the evolution of magnetic ordering at the Fe sites, in samples with a Ru fraction of x = 0.1 and 0.5. From the analysis of the data, it is surmised that the isomer shift increases with a decrease in temperature, with a characteristic slope change at the structural transition in both samples studied. In both the x = 0.1 and x = 0.5 samples, a low B(hf) centred around 0.5 Tesla is seen to occur well above the structural transition temperature, the contribution from which is suppressed with a decrease in temperature. Below the structural transition temperature, a bimodal distribution of B(hf) centred at about 3 Tesla and 5 Tesla emerges, the contribution from which increases with a further decrease in temperature. Spin polarized density functional calculations suggest the occurrence of different magnetic moments at the Fe sites in the Ru substituted compounds, and provide a rationale for the experimentally observed multimodel B(hf).

Baseline drift removal and denoising of MCG data using EEMD: role of noise amplitude and the thresholding effect.

We adopt the Ensemble Empirical Mode Decomposition (EEMD) method, with an appropriate thresholding on the Intrinsic Mode Functions (IMFs), to denoise the magnetocardiography (MCG) signal. To this end, we discuss the two associated problems that relate to: (i) the amplitude of noise added to the observed signal in the EEMD method with a view to prevent mode mixing and (ii) the effect of direct thresholding that causes discontinuities in the reconstructed denoised signal. We then denoise the MCG signals, having various signal-to-noise ratios, by using this method and compare the results with those obtained by the standard wavelet based denoising method. We also address the problem of eliminating the high frequency baseline drift such as the sudden and discontinuous changes in the baseline of the experimentally measured MCG signal using the EEMD based method. We show that the EEMD method used for denoising and the elimination of baseline drift is superior in performance to other standard methods such as wavelet based techniques and Independent Component Analysis (ICA).

Pressure-induced structural changes and insulator-metal transition in layered bismuth triiodide, BiI3: a combined experimental and theoretical study.

Noting that BiI3 and the well-known topological insulator (TI) Bi2Se3 have the same high symmetry parent structures, and that it is desirable to find a wide-band gap TI, we determine here the effects of pressure on the structure, phonons and electronic properties of rhombohedral BiI3. We report a pressure-induced insulator-metal transition near 1.5 GPa, using high pressure electrical resistivity and Raman measurements. X-ray diffraction studies, as a function of pressure, reveal a structural peculiarity of the BiI3 crystal, with a drastic drop in c/a ratio at 1.5 GPa, and a structural phase transition from rhombohedral to monoclinic structure at 8.8 GPa. Interestingly, the metallic phase, at relatively low pressures, exhibits minimal resistivity at low temperatures, similar to that in Bi2Se3. We corroborate these findings with first-principles calculations and suggest that the drop in the resistivity of BiI3 in the 1-3 GPa range of pressure arises possibly from the appearance of an intermediate crystal phase with a lower band-gap and hexagonal crystal structure. Calculated Born effective charges reveal the presence of metallic states in the structural vicinity of rhombohedral BiI3. Changes in the topology of the electronic bands of BiI3 with pressure, and a sharp decrease in the c/a ratio below 2 GPa, are shown to give rise to changes in the slope of phonon frequencies near that pressure.

Tunable resistivity in magnetic glass phase of Gd(1-x)Ca(x)BaCo2O5.5.

We present magnetization and resistance measurements carried out on pristine and Ca-doped Gd(1-x)Ca(x)BaCo2O5.5 (x = 0.02) samples using the cooling and heating in unequal field (CHUF) protocol. The measurements reveal that the high temperature ferromagnetic phase is kinetically arrested at low temperature when the sample is cooled in a magnetic field. The volume fraction of this arrested phase increases upon Ca substitution and also by increasing the field in which the sample is cooled. Since the ferromagnetic phase is less resistive when compared to the low temperature antiferromagnetic phase, a tunable resistance is achieved in the sample by cooling in different magnetic fields. By cooling in magnetic fields of 9 T a reduction in resistivity by an order of magnitude is achieved. These results are consistent with the coexistence of the low temperature equilibrium antiferromagnetic phase with kinetically arrested high temperature ferromagnetic phase in the system.

UV induced zener diode characteristic in a single n-ZnO/p++-Si nanoheterojunction.

Rectification is observed in a single n-ZnO/p++-Si nanoheterojunction using ultra high vacuum compatible scanning tunneling microscope. The nanohetrojunctions have been grown using catalyst free vapor-solid growth of ZnO nanorods on p++-Si substarte. A high rectification ratio approximately 100 at 2 V is observed in the current voltage measurements. Temperature dependent study in these nanohetero-junctions showed activation energy for carrier conduction approximately 66 meV, which is primarily associated to the presence of heterojunction induced interface states. Role of ultra violet excitation on these finite sized (approximately 500 nm) nanoheterojunction is also studied with photo-generated electron-hole pairs. A Zener breakdown is observed in this photo-excitation process. Increase in the concentration of minority carriers and corresponding decrease in barrier width and height at the junction have been identified for the observed tunneling behavior under UV illumination. The large carrier concentration in the finite sized device with large diffusion length of electron (approximately 2 microm) is made responsible for the observed voltage regulation.

Local structural studies of the cubic Cd1-xCaxO system through Cd K-edge extended X-ray absorption spectroscopic studies.

Cd K-edge extended X-ray absorption fine-structure spectroscopic studies were carried out on Cd(1-x)Ca(x)O (0 ≤ x ≤0.9) solid solutions and the first and second nearest neighbour (NN) distances and their mean square relative displacement σ(2) were estimated. The first NN distance, d(Cd-O)(x), was found to be smaller than its expected value, a(x)/2, obtained from the X-ray diffraction measurements. It increases monotonically and non-linearly with a negative curvature, comparable with that of the a(x) value variation. The variation σ(2) of the 1NN with x is consistent with a disordered solid solution model. The 2NN distances d(Cd-Cd)(x) and d(Cd-Ca)(x) are found to follow the average values obtained by X-ray diffraction with d(Cd-Ca)(x) > d(Cd-Cd)(x). From detailed analysis it is argued that the solid solution exhibits a bimodal distribution of the 1NN distances, d(Cd-O)(x) and d(Ca-O)(x), and that the system belongs to a persistent type.

Development of high field SQUID magnetometer for magnetization studies up to 7 T and temperatures in the range from 4.2 to 300 K.

We present the design, fabrication, integration, testing, and calibration of a high field superconducting quantum interference device (SQUID) magnetometer. The system is based on dc SQUID sensor with flux locked loop readout electronics. The design is modular and all the subsystems have been fabricated in the form of separate modules in order to simplify the assembly and for ease of maintenance. A novel feature of the system is that the current induced in the pickup loop is distributed as inputs to two different SQUID sensors with different strengths of coupling in order to improve the dynamic range of the system. The SQUID magnetometer has been calibrated with yttrium iron garnet (YIG) sphere as a standard reference material. The calibration factor was determined by fitting the measured flux profile of the YIG sphere to that expected for a point dipole. Gd(2)O(3) was also used as another reference material for the calibration and the effective magnetic moment of the Gd(3+) could be evaluated from the temperature dependent magnetization measurements. The sensitivity of the system has been estimated to be about 10(-7) emu at low magnetic fields and about 10(-5) emu at high magnetic fields ∼7 T.

On the design and implementation of a novel impedance chamber based variable temperature regulator at liquid helium temperatures.

A novel variable temperature regulator (VTR) based on the use of a fine impedance capillary to control the flow rate of cold helium gas into the VTR chamber is described. The capillary has a diameter of just 200 microm and the flow rate of cold helium gas through the capillary can be effectively controlled to the desired value by heating the capillary to a preset temperature and by controlling the pressure in the VTR chamber to a preset pressure using automated control circuits. Excellent temperature stability (about +/-1 mK at 10 K and +/-2 mK at 100 K) has been demonstrated in this setup with uniform rates of heating or cooling by an optimal choice of parameters. Compared to the more conventional VTR designs based on the use of mechanical long stem valves in the liquid helium reservoir to control the flow rate of liquid helium into the VTR chamber, and the use of a needle valve at the top of the cryostat to control the exchange gas pressure in the thermal isolation chamber, the present design enables temperature stability at any user desired temperature to be attained with uniform rates of cooling/heating with minimum consumption of liquid helium. The VTR has been successfully incorporated in the high field superconducting quantum interference device magnetometer setup developed in-house. It can also be incorporated in any low temperature physical property measurement system in which the temperature has to be varied in a controlled manner from 4.2 to 300 K and vice versa with uniform rates of heating and cooling.

Efficacy of surface error corrections to density functional theory calculations of vacancy formation energy in transition metals.

We calculate properties like equilibrium lattice parameter, bulk modulus and monovacancy formation energy for nickel (Ni), iron (Fe) and chromium (Cr) using Kohn-Sham density functional theory (DFT). We compare the relative performance of local density approximation (LDA) and generalized gradient approximation (GGA) for predicting such physical properties for these metals. We also make a relative study between two different flavors of GGA exchange correlation functional, namely PW91 and PBE. These calculations show that there is a discrepancy between DFT calculations and experimental data. In order to understand this discrepancy in the calculation of vacancy formation energy, we introduce a correction for the surface intrinsic error corresponding to an exchange correlation functional using the scheme implemented by Mattsson et al (2006 Phys. Rev. B 73 195123) and compare the effectiveness of the correction scheme for Al and the 3d transition metals.

Temperature dependence of phonon modes in nanocrystalline La0.67ca0.33MnO3 as observed by infrared spectroscopy.

Low temperature infrared absorption measurements have been carried out on nanocrystalline La0.67Ca0.33MnO3 powder across the magnetic and the insulator-to-metal phase transitions. Interesting changes are observed in the temperature dependence of the mid-IR polaronic background and the stretching mode of the MnO, octahedron. Upon cooling below 250 K, the overall absorbance increases, but, unlike in the case of microcrystalline LCMO, the stretching mode is not completely screened even at 5 K. The temperature dependence of the stretching mode parameters points to a much reduced phonon-polaron coupling as compared to that in the bulk material.

Studies of local structure at Zr sites in pressure amorphized zirconium tungstate.

Amorphous to crystalline transition in pressure quenched Zr(0.5)Hf(0.5)W(2)O(8) has been studied with respect to local structures of ZrO(6) using the perturbed angular correlation technique. In an untreated crystalline sample close to 0.7 fraction of the probe atoms occupy Zr sites of regular ZrO(6) while the remaining three fractions are understood to be associated with contracted and distorted octahedra. The existence of six distinct ZrO(6) could be deduced based on perturbed angular correlation studies in the pressure amorphized sample. In the amorphous sample these ZrO(6) are associated with appreciable octahedral distortions. Isochronal annealing measurements show that these octahedra remain structurally quite stable up to 800 K. Values of quadrupole frequencies tend to become close to those experienced by probe atoms in a crystalline sample for annealing at 870 K, implying that around this temperature there is an onset of amorphous to crystalline transition. Complete restoration of quadrupole parameters to those of the untreated crystalline sample is seen subsequent to annealing at 975 K.

Spectroscopic characterization of nanocrystalline chromium nitride (CrN).

Nanocrystalline chromiuim nitride has been synthesised by direct gas phase nitridation of nanocrystalline chromia at 1100 degrees C in ammonia-atmosphere. XRD of this material showed formation of single phase CrN with particle size around 20 nm. AFM studies showed particle distribution along with some soft agglomerated nanostructures. Nanocrystalline Cr2O3 and partially-as well as fully--converted nanocrystalline CrN were also investigated using various spectroscopic techniques like XPS, FT-IR, and Raman for gaining insight into the conversion pathways. Spectroscopic investigations of these materials clearly indicate that complete conversion of CrN occurs by nitriding at 1100 degrees C for 4 hrs. The salient spectroscopic features of these nanocrystalline materials with respect to their microcrystalline counterparts are discussed.

Competing magnetic phases in La(0.7)Sr(0.3)MnO(3) as deduced from Mn site hyperfine parameters.

Time differential perturbed angular correlation measurements using the (181)Ta probe in La(0.7)Sr(0.3)Mn(0.995)Hf(0.005)O(3) reveal the presence of two distinct hyperfine components, identified with probe atoms occupying Mn sites which are rich and deficient in hole concentration. The Mn(4+) rich zones exhibit ferromagnetic ordering at all temperatures below 360 K, the bulk Curie temperature. In the case of Mn(4+) deficient zones, the paramagnetic order is seen to evolve into a canted antiferromagnetic ordering below 360 K, that becomes ferromagnetic below 250 K. Concomitantly, there is a change in the fractions below 250 K. The implications of these results are discussed in terms of electronic phase separation.