Anuj Upadhyay

Angle Dispersive X-ray Diffraction Beamline on Indus-2 Synchrotron Radiation Source: Commissioning and First Results

Angle dispersive x-ray diffraction (ADXRD) is a basic non destructive tool for the determination of crystal structure. Energy tunability and high flux are added advantages in using synchrotron radiation (SR) source for ADXRD technique. We have installed an ADXRD beamline (BL-12) on Indus-2, the Indian synchrotron source. Indus-2 is a 2.5GeV, 300mA SR source. The beamline consists of a Si (311) crystal pair based double crystal monochromator with bendable focusing optics. The experimental station consists of a six circle diffractometer with scintillation detector and an image plate area detector. The beamline has been used for wide range of experiments like powder and single crystal diffraction; grazing incidence diffraction, x-ray absorption near edge structure, Anomalous XRD, high pressure XRD etc. The beamline is being utilized by users from Indian universities and research institutions.

Structural, electronic structure, and band alignment properties at epitaxial NiO/Al2O3 heterojunction evaluated from synchrotron based X-ray techniques

The valence band offset value of 2.3 ± 0.2 eV at epitaxial NiO/Al2O3 heterojunction is determined from photoelectron spectroscopy experiments. Pulsed laser deposited thin film of NiO on Al2O3 substrate is epitaxially grown along [111] direction with two domain structures, which are in-plane rotated by 60° with respect to each other. Observation of Pendellosung oscillations around Bragg peak confirms high interfacial and crystalline quality of NiO layer deposited on Al2O3 substrate. Surface related feature in Ni 2p3/2 core level spectra along with oxygen K-edge soft X-ray absorption spectroscopy results indicates that the initial growth of NiO on Al2O3 substrate is in the form of islands, which merge to form NiO layer for the larger coverage. The value of conduction band offset is also evaluated from the measured values of band gaps of NiO and Al2O3 layers. A type-I band alignment at NiO and Al2O3 heterojunction is also obtained. The determined values of band offsets can be useful in heterojunction based l...

Effect of thermal annealing and oxygen partial pressure on the swelling of HfO2/SiO2/Si metal-oxide-semiconductor structure grown by rf sputtering: A synchrotron x-ray reflectivity study

As-grown and rapid thermal annealed thin HfO2 films, deposited on Si(100) substrate by reactive rf sputtering at various partial pressures of O2 and Ar, are studied by synchrotron x-ray reflectivity. The growth of interfacial layer (IL) of SiO2 is more or less linear with the decrease in oxygen partial pressure ( pO2) in the O2/Ar mixture. The thickest oxide is found to be grown at the minimum oxygen partial pressure ( pO2). It is observed that the IL swells upon annealing at higher temperature, and swelling is maximum for the sample grown in minimum pO2. The surface roughness and thickness of the HfO2 films decrease upon annealing indicating a denser film. The HfO2/Si interface roughness is also decreased upon annealing. Therefore, lower annealing temperature and higher pO2 is to be set to reduce the IL thickness and for higher dielectric constant and larger oxide capacitance. High frequency capacitance-voltage (C–V) measurement on the devices, annealed at higher temperature, further shows the necessity ...

Structural analysis of lead magnesium niobate using synchrotron powder X‐ray diffraction and the Rietveld method

The room-temperature synchrotron powder X-ray diffraction pattern of the single phase perovskite lead magnesium niobate (PMN) has shown significant broadening in the q range ∼ 5-7 Å(-1) compared with standard LaB6 synchrotron powder X-ray diffraction data, taken under similar conditions. This broadening/asymmetry lies mainly towards the lower 2θ side of the Bragg peaks. Attempts to fit this data with the paraelectric cubic phase (Pm\bar 3m) and the local rhombohedral phase (R3m) corresponding to polar nanoregions (PNRs) are made using the Rietveld method. Rietveld refinements show that neither cubic (Pm\bar 3m) nor rhombohedral (R3m) symmetry can fit this XRD pattern satisfactorily. The two-phase refinement fits the experimental data satisfactorily and suggests that the weight percentage of the PNRs is approximately 12-16% at room temperature. The unit-cell volume of these rhombohedral PNRs is approximately 0.15% larger than that of the unit cell volume of the paraelectric cubic phase.

Effect of isochronal annealing on phase transformation studies of iron oxide nanoparticles

The effect of isochronal annealing on the phase transformation in iron oxide nanoparticles is reported in this work. Iron oxide nanoparticles were successfully synthesized using an ash supported technique followed by annealing for 2 h at various temperatures between 300 and 700°C. It was observed using X-ray diffraction (XRD) and transmission electron microscopy (TEM) that as-grown samples have mixed phases of crystalline haematite (α-Fe2O3) and a minor phase of either maghemite (γ-Fe2O3) or magnetite (Fe3O4). On annealing, the minor phase transforms gradually to haematite. The phase transformation is complete at annealing temperature of 442°C as confirmed by differential scanning calorimetric (DSC) analysis. The unresolved phases in XRD were further analysed and confirmed to be maghemite from the X-ray absorption near edge structure (XANES) studies. The magnetic measurements showed that at room temperature nano- α-Fe2O3 is weak ferromagnetic, and its magnetization is larger than the bulk value. The mixed phase sample shows higher value of magnetization because of the presence of ferromagnetic γ-Fe2O3 phase.

Study of structural disorder in Pb(Mg1/3Nb2/3)O3

Lead Magnesium Niobate (PMN) is prepared by two step solid state reaction i.e. Columbite route. X-ray diffraction pattern of powder of calcined PMN at 800 °C and powder of PMN pellet sintered at 1200 °C have shown some systematic differences in their relative intensity ratios measured by a 2D detector on Indus-2 synchrotron source. Rietveld method is used to study these differences taking split-atom approach. We have observed that statistical disorder observed in both cases is different. Such multisite disorder is consistent with other Pb based systems like PZN-PT.

High pressure structural investigation on LaGa

High pressure X-ray diffraction studies on rare-earth gallide LaGa was carried up to a pressure of ∼28 GPa using synchrotron, as well as rotating anode X-ray source in an angle dispersive mode. LaGa exhibits CrB (B33)-type orthorhombic structure (space group Cmcm) at ambient pressure. It undergoes a reversible structural phase transition from orthorhombic to tetragonal structure (Space. Group P4/mmm) at ∼5 GPa. Both the phases coexist up to the highest pressure studied. The transition to tetragonal phase has implications in predicting the new intermediate phase in the generally observed B1 to B2 transition sequence in AB type of rare-earth intermetallics. This investigation reveals that the LnX-type compounds may exhibit the structural sequence B1→ B33→ P4/mmm→ B2 under pressure. Considering the variation of lattice parameters a, b, c and also various bond lengths with pressure, the B33 to P4/mmm transition in LaGa may be displacive in nature. The zero pressure bulk modulus and its derivative for parent phase have been estimated to be B0 = 60 ± 3 GPa and  = 4.6 ± 1.5. The bulk modulus for the high pressure tetragonal phase at ∼8 GPa also has been estimated to be B8 = 77 ± 8 GPa. We have also done the non-spin-polarized total energy calculations using the full potential linearized augmented plane wave method as implemented in the WIEN2 K code which confirms the experimental results.

Enhanced water window x-ray emission from in situ formed carbon clusters irradiated by intense ultra-short laser pulses

Enhanced water window x-ray emission (23–44 A) from carbon clusters, formed in situ using a pre-pulse, irradiated by intense (I > 1017 W/cm2) ultra-short laser pulse, is demonstrated. An order of magnitude x-ray enhancement over planar graphite target is observed in carbon clusters, formed by a sub-ns pre-pulse, interacting with intense main pulse after a delay. The effect of the delay and the duration of the main pulse is studied for optimizing the x-ray emission in the water window region. This x-ray source has added advantages of being an efficient, high repetition rate, and low debris x-ray source.

Effect of electron beam irradiation on PMMA films

Polymethyl methacrylate (PMMA) is characterized for electron beam interactions in the resist layer in lithographic applications. PMMA thin films (free standing) were prepared by solvent casting method. These films were irradiated with 30keV electron beam at different doses. Structural and chemical properties of the films were studied by means of X-ray diffraction and Fourier transform infra-red (FTIR) spectroscopy The XRD results showed that the amorphization increases with electron beam irradiation dose. FTIR spectroscopic analysis reveals that electron beam irradiation promotes the scission of carbonyl group and depletes hydrogen and converts polymeric structure into hydrogen depleted carbon network.

Effect of processing parameters on microstructural properties of lead magnesium niobates

The synchrotron powder X-ray diffraction (XRD) and subsequent detailed Rietveld analysis of lead magnesium niobate (PMN) samples were performed to study the microstructural properties of polar nanoregions (PNRs) of the R3m phase. PMN samples were synthesized under different sample processing conditions. The line profile broadening analysis of room-temperature synchrotron powder XRD patterns was performed using the multi-phase Rietveld refinement method for isotropic microstructural evaluation of different PMN samples. The two phases of perovskite PMN considered in the Rietveld refinement approach for satisfactorily fitting the XRD patterns are the paraelectric cubic phase (Pm m) and the local rhombohedral phase (R3m) which corresponds to the PNRs. It is observed that the contributions of the Gaussian component of size broadening of the polar rhombohedral phase (R3m) and the Lorentzian component of strain broadening of the paraelectric cubic phase (Pm m) are apposite for satisfactory Rietveld refinement of the synchrotron XRD data for all PMN samples. The volume-average crystallite size of PNRs (R3m phase) is almost invariant (approximately 12 nm) with increasing processing temperature while their weight percentage increases. The values of the apparent microstrain in the paraelectric cubic phase (Pm m) are larger for hot-pressed samples.