Indus-2 Synchrotron Radiation Source Research Articles

Development of piezo-actuated x-ray deformable mirror for vertical focusing of synchrotron radiation at Indus-2

Piezo-actuated x-ray deformable mirrors (PXDMs) can effectively control the surface profile with sub-nanometre accuracy for adaptive focusing and correct the wavefront distortion generated due to imperfections in optical components or other extraneous effects like heat load, minor misalignments of synchrotron radiation beamline. Generating and controlling the desired shape of PXDMs with sub-nanometre accuracy is very challenging due to the presence of a large number of actuators and constraints related to nonlinearity of piezoactuator, boundary conditions, fabrication related limitations and the requirement for ex-situ as well as in-situ characterization of PXDM. To accomplish this, a PXDM of zerodur with multiple electrodes on a piezoactuator has been developed for vertical focusing of synchrotron x-rays for the first time in India. The PXDM has been fabricated and characterized by in-house developed technologies. The iterative piezo response function-based optimization technique is used to optimize the electric fields of individual piezoactuators in order to achieve the desired parabolic shape of the PXDM. The ex-situ characterization showed that the PXDM can achieve the target parabolic profile with 42 nm root-mean-square error. Furthermore, in-situ characterization at a beamline, BL-12, of Indus-2 synchrotron radiation source using PXDM has confirmed the focusing of collimated x-ray beam in the vertical direction from FWHM 235 μm to FWHM 83 μm.

Studies on thermal profile measurement and fire detection in a power supply cable of a synchrotron radiation source by Raman optical fiber distributed temperature sensor system

The paper presents the work on development and application of Raman optical fiber distributed temperature sensor (ROFDTS). ROFDTS has been used for monitoring the temperature profile and detecting the progress of unforeseen fire events anywhere in a 160 m long power supply cable (current 760 A, DC) of dipole magnets in the Indus-2 synchrotron radiation source (SRS). Indus-2 is a national facility and is being operated in round the clock mode. The sensing fiber could survive in the harsh environment of Indus-2 SRS that consists of bremsstrahlung radiation of 6.7 Rad/h, high magnetic field of 1.5 T and radio frequency (RF) field of 1.27 MV at 505.812 MHz. The fire detecting capability of ROFDTS was first tested on the mock test setup in the laboratory by artificially creating the four hot zones. Each hot zone has the width of 1.0 m in the sensing fiber at the spatial locations of 26 m, 48 m, 70 m and 92 m respectively. An audio-visual alarm was generated when the temperature of the hot zones exceeded the set temperature limit of 50 °C within 30 s of the start of the fire. Finally, ROFDTS system was deployed to measure the temperature profile of power supply cable during ‘no operation’, ‘injection’ of the electron beam current (109 mA with the energy of electrons @ 550 MeV) and at ‘normal operation’ of the electron beam current (145 mA with the energy of electrons @ 2.5 GeV) in Indus-2 SRS. The peak temperature of power cable reached from 26 °C to 44 °C from ‘no operation’ to during the ‘normal operation’ condition of the Indus-2 SRS.

Use of Synchrotron Phase-Sensitive Imaging for the Investigation of Magnetopriming and Solar UV-Exclusion Impact on Soybean (Glycine max) Leaves.

The combined response of exclusion of solar ultraviolet radiation (UV-A+B and UV-B) and static magnetic field (SMF) pre-treatment of 200 mT for 1 h were studied on soybean (Glycine max) leaves using synchrotron imaging. The seeds of soybean with and without SMF pre-treatment were sown in nursery bags kept in iron meshes where UV-A+B (280–400 nm) and UV-B (280–315 nm) from solar radiation were filtered through a polyester filters. Two controls were planned, one with polythene filter controls (FC)- which allows all the UV (280–400 nm); the other control had no filter used (open control-OC). Midrib regions of the intact third trifoliate leaves were imaged using the phase-contrast imaging technique at BL-4, Indus-2 synchrotron radiation source. The solar UV exclusion results suggest that ambient UV caused a reduction in leaf growth which ultimately reduced the photosynthesis in soybean seedlings, while SMF treatment caused enhancement of leaf growth along with photosynthesis even under the presence of ambient UV-B stress. The width of midrib and second-order veins, length of the second-order veins, leaf vein density, and the density of third-order veins obtained from the quantitative image analysis showed an enhancement in the leaves of plants that emerged from SMF pre-treated seeds as compared to untreated ones grown in open control and filter control conditions (in the presence of ambient UV stress). SMF pre-treated seeds along with UV-A+B and UV-B exclusion also showed significant enhancements in leaf parameters as compared to the UV excluded untreated leaves. Our results suggested that SMF-pretreatment of seeds diminishes the ambient UV-induced adverse effects on soybean.

Failure Analysis of a High Voltage Feedthrough of Indus-2 Synchrotron Radiation Source

Abstract In this paper, a failure analysis of a high voltage feedthrough of the Indus 2 synchrotron radiation source which brought about venting of the vacuum chamber is discussed. A detailed failure analysis demonstrated that the main cause responsible for the failure of the feedthrough was high humidity in the atmosphere surrounding the feedthrough assembly, which resulted in the corrosion of CuSil braze filler alloy at the ground terminal and also caused flashover between positive (+) and ground terminals. Thermal cycling of the insulator due to flashover resulted in spalling of glazed surface layer and assisted crack propagation from the flashover-generated surface defects. The remedial measures recommended to avoid similar failure include: thorough cleaning of feedthrough and its connectors before installation, use gasket-type sealing in the protective cover of the connector on the air side, use of metallic tubes in place of polyurethane cooling water tubes and design change of feedthrough to shift brazed joint to vacuum side.

Electronic and vibrational spectroscopy of ethyl methyl carbonate: A comparative experimental and theoretical study

A detailed spectroscopic study on ethyl methyl carbonate, a green solvent, has been carried out by recording vacuum ultraviolet and infrared spectra. The vacuum ultraviolet photoabsorption spectrum is recorded using synchrotron radiation from Photophysics beamline at the Indus-1 synchrotron radiation source at RRCAT, Indore, India in the wavelength region of 7–11.5 eV. Infrared spectra in gas phase as well as matrix isolated case are recorded using an indigenously developed laboratory low temperature experimental facility and a Fourier transform infrared spectrometer in the 500–4000 cm−1 region. Geometry optimization, vibrational frequency analysis of neutral & ionized ethyl methyl carbonate and electronic excited state energy information has been obtained using quantum chemical calculations. The observed ir spectral features could be assigned to the fundamental vibrational modes of the molecule. The vacuum ultraviolet region comprising a broad continuum is assigned to valence transitions having high oscillator strengths and overlying weak bands to ns, np, nd type Rydberg transitions. Potential energy curves of the ground and first few low lying excited states generated provided additional insights into their nature and further interpretation of observed experimental spectra. In this paper we report the first electronic absorption spectrum in 7 to 11.5 eV region, its spectroscopic analysis and identification of vibrational modes in the infrared spectra for ethyl methyl carbonate. Results of quantum chemical simulations carried out to obtain nature of excited states, energies and vibrational frequencies using GAMESS (USA) quantum chemistry code are also reported in this paper.

Development of UHV pulsed laser deposition set-up for in-situ photoelectron spectroscopic study at ARPES beamline, Indus-1 synchrotron radiation source, India

We have developed an Ultra-High Vacuum (UHV) compatible Pulsed Laser Deposition (PLD) set-up at Angle Resolved Photo Electron Spectroscopy (ARPES) beamline (BL-3) at Indus-1 synchrotron radiation source, Raja Ramanna Centre for Advanced Technology, Indore, India. The set-up is successfully tested and integrated at beamline for in-situ photoelectron spectroscopic (PES) studies of thin films. In present PLD set-up, quick in-situ transfer of deposited thin films to analysis chamber enables the surface sensitive PES measurements on atomically cleaned surfaces without the requirement of any sputtering. This set-up has the capability of thin film depositions using six number of one-inch targets with precise control of various deposition parameters at a base pressure of ∼1x10−9 mbar. To explore the capability of the system, a set of thin films of HfO2, 5 % Ga2O3 doped ZnO (GZO) and GZO/HfO2 are deposited and the band offset of GZO/HfO2 heterostructure is investigated by in-situ PES measurements using synchrotron radiation. The film surface is found to be contamination free, which demonstrates the capability of the set-up for in-situ PES studies. The Hf 4f and Zn 3d core level peaks along with valence band maxima positions are used to determine the valence band offset. The valence band offset is found to be 0.31 ± 0.08 eV, which is the first result reported on this heterostructure system.

Influence of spin orbit splitting and satellite transitions on nickel soft X-ray optical properties near its L2,3 absorption edge region.

Transition elements exhibit strong correlations and configuration interactions between core and valence excited states, which give rise to different excitations inside materials. Nickel exhibits satellite features in its emission and absorption spectra. Effects of such transitions on the optical constants of nickel have not been reported earlier and the available database of Henke et al. does not represent such fine features. In this study, the optical behaviour of ion beam sputter deposited Ni thin film near the L2,3-edge region is investigated using reflection spectroscopy techniques, and distinct signatures of various transitions are observed. The soft X-ray reflectivity measurements in the 500-1500 eV photon energy region are performed using the soft X-ray reflectivity beamline atthe Indus-2 synchrotron radiation source. Kramers-Kronig analysis of the measured reflectivity data exhibit features corresponding to spin orbital splitting and satellite transitions in the real and imaginary part of the refractive index (refraction and absorption spectra). Details of fine features observed in the optical spectra are discussed. To the best of our knowledge, this is the first study reporting fine features in the measured optical spectra of Ni near its L2,3-edge region.

X-ray Absorption Fine Structure Studies of Zirconium Complexes

Zirconium complexes derived with Schiff-base ligands take a central role in the expansion of coordination chemistry and have been receiving huge attention due to its pharmacological, dental and industrial characteristics. The present research paper deals with the characterization of Zirconium complexes with X-ray absorption spectroscopy (XAS) at Zirconium K-edge. Characterization was done at BL-9 EXAFS beamline available at Indus-2 synchrotron radiation source (2.5 GeV, 125 mA), Raja Ramanna Centre for Advanced Technology, Indore (M.P.), India. Both X-ray absorption near edge structure (XANES) and Extended X-ray absorption fine structure (EXAFS) techniques were used to explore out the local environment around the Zirconium complexes. A computer software package IFEFFIT was used to analyze physical parameters. Edge width reveals that complexes have octahedral geometry and chemical shifts of complexes from zirconium metal reveals oxidation state of Zirconium in their complexes. The bond length of first coordinating shell of the complexes has been determined by Fourier transform method and compares this bond length with different methods.

3D spatial distribution of ore mineral phases using high resolution synchrotron micro-computed tomography (μCT) combined with optical microscopy

Ore minerals in dolomites and Graphite Mica Schist (GMS) were studied by synchrotron radiation micro-computed tomography (SR-μCT) and optical microscopy. High resolution μCT images of ore minerals were obtained at Imaging Beamline (BL-4), Indus-2 synchrotron radiation source for the comprehensive volume characterization of minerals. Optical microscopy was used for mineral identification, mineral/rock characterization and quantification of ore mineral assemblages was also confirmed by XRD. 3D images from SR-μCT have shown spatial distribution of major minerals and crystals of different minerals in the volume of samples. The results obtained shows that the GMS and dolomitic hosted rocks mined from region near Udaipur, Rajasthan contains sulfide mineral phases. SR-μCT facilitates visualization of the association of the various metallic minerals with the host rock. The presence of economically important metallic minerals galena, sphalerite and pyrite found in the samples through SR-μCT has implications on exploration and processing of ores.

A simple method to overcome the limitation of hybrid monochromator in the identification of peaks in the HRXRD pattern of Al0.4Ga0.6N/Al0.6Ga0.4N multi quantum wells

Features related to AlN buffer layer, thick AlGaN bottom layer, and AlGaN quantum well structure are identified by performing High resolution X-ray diffraction (HRXRD) measurements on Al0.4Ga0.6N/Al0.6Ga0.4N multi quantum well sample. HRXRD measurements reveal an anomalous peak which is not predicted by the simulations using Takagi-Taupin equations based on the dynamical theory of X-ray diffraction. However, the peak doesn’t appear when the diffraction pattern is recorded using the HRXRD beam line of Indus-2 Synchrotron radiation source. Systematic investigations reveal that the anomalous peak is related to some unknown scattering originating from the X-ray optics used in the hybrid monochromator of commercial HRXRD system. It limits the usefulness of HRXRD technique for the investigation of AlGaN/AlGaN MQW samples. In view of this, a simple method for the elimination of anomalous peak from the HRXRD pattern is also demonstrated. In literature, similar anomalous peaks are often associated with the incorporation of metallic clusters, impurities, and additional crystallographic phases in epilayer. A word of caution is therefore necessary that the origin of anomalous peak in HRXRD pattern should be first confirmed before assigning the same to a particular physical phenomenon.

Multivariate analysis of trace elemental data obtained from blood serum of breast cancer patients using SRXRF

Abstract Synchrotron radiation based X-ray fluorescence (SRXRF) technique was utilized for the determination of serum elemental profile in breast cancer patients group and healthy subjects group. The SRXRF experiments were performed on microprobe beamline-16, Indus-2 synchrotron radiation source at Raja Ramanna Centre for Advanced Technology (RRCAT), Indore, India. The accuracy and reliability of the experimental method were validated by using International Atomic Energy Agency (IAEA) reference material-animal blood (A-13). Sixteen elements were identified and their concentrations were measured in the serum of the two studied groups. The analysis of results showed significantly elevated levels of Fe (p

Development of an experimental set-up for low-temperature spectroscopic studies of matrix-isolated molecules and molecular ices using synchrotron radiation.

An experimental set-up for studying photophysics and photochemistry of molecules in an inert gas medium (matrix-isolated) and in the ice phase at low temperatures has been developed and commissioned at the Photophysics beamline, Indus-1 synchrotron radiation source. This end-station uses an in-house-developed closed-cycle cryostat for achieving cryo-temperatures (∼10 K). Synchrotron radiation from the Photophysics beamline is used as the source of UV-VUV photons and the system is equipped with a Fourier transform infrared spectrometer for characterization of the molecular species formed at low temperature. Various individual components of the end-station like closed-cycle cryostat, experimental chamber, gas mixing and deposition systems are tested to ascertain that the desired performance criteria are satisfied. The performance of the composite system after integration with the Photophysics beamline is evaluated by recording IR and UV-VUV photoabsorption spectra of sulfur dioxide at low temperatures (10 K), both in the ice phase as well as isolated in argon matrices. Results obtained are in good agreement with earlier literature, thus validating the satisfactory performance of the system. As an off-shoot of the study, the VUV absorption spectrum of matrix-isolated SO2 in argon matrix up to 10.2 eV is reported here for the first time. This experimental end-station will provide new opportunities to study photon-induced reactions in molecules of environmental, astrochemical and industrial importance. Details of the design, development and initial experimental results obtained are presented.

Influence of the core-hole effect on optical properties of magnesium oxide (MgO) near the Mg L-edge region.

The influence of the core-hole effect on optical properties of magnesium oxide (MgO) is established through experimental determination of optical constants and first-principles density functional theory studies. Optical constants (δ and β) of MgO thin film are measured in the spectral region 40-300 eV using reflectance spectroscopy techniques at the Indus-1 synchrotron radiation source. The obtained optical constants show strong core exciton features near the Mg L-edge region, causing significant mismatch with Henke's tabulated values. On comparing the experimentally obtained optical constants with Henke's tabulated values, an edge shift of ∼3.0 eV is also observed. Distinct evidence of effects of core exciton on optical constants (δ and β) in the near Mg L-edge absorption spectra are confirmed through first-principles simulations.

Chemical shifts of L3 X-ray absorption edges on lead and thallium compounds by DEXAFS using synchrotron radiation source

The L3 absorption edges of 82Pb and 81Tl compounds have been measured using DEXAFS at INDUS-2 Synchrotron radiation source at RRCAT, Indore. The energy shift of ∼(−6 to 2) eV are observed in pre-edge of 82Pb compounds while energy shift varies ∼(−5 to 10) eV in pre-edge and ∼(2–9) eV in post-edge of 81Tl compounds. The chemical effects in both compounds have been described by calculating effective charge using Suchet and Pauling methods. A linear relation is established between chemical effect and effective charge of different compounds for the first time in literature.

X-ray diffraction and X-ray K absorption near edge studies of copper (II) complexes with amino acids

Synthesis of copper (II) complexes [CuL1L2X].nH2O, where n=1, 2,3 (X=Cl,Br,NO3) (L1is 2,2’-bipyridine and L2 is L-tyrosine) by the chemical root method. The XRD data for the samples have been recorded. EXAFS spectra have also been recorded at the K-edge of Cu using the dispersive beam line BL-8 at 2.5 Gev Indus-2 Synchrotron radiation source at RRCAT, Indore, India. XRD and EXAFS data have been analysed using the computer software. X-ray diffraction studies of all complexes indicate their crystalline nature. Lattice parameter, bond length, particle size have been determined from XRD data.

Co (II) Complexes with Schiff Base Ligands: Synthesis and EXAFS Study

Thesynthesis of transition metal Schiff base complexes of Co(II) are prepared by chemical root method. Obtained by the condensation of O-phenylenediamine, salicylaldehyde and isatin / 2-hydroxy- 1 Naphthaldehyde is presented. The complexes were characterized by Co- K- edge EXAFS measurements using the dispersive beam line at 2.5GeV energy of Indus-2 synchrotron radiation source RRCAT Indore. The recorded EXAFS data were analyzed using the computer software Athena for determine the nearest neighboring distances (bond lengths) of these complexes with conventional methods and were compared with Fourier transform (FT) analysis.

X-ray diffraction and X-ray K-absorption near edge studies of Copper (II) Micro cyclic Carbamide complexes.

Synthesis of metal complexes [Cu (Carbamide)] (X = Br, Cl, NO3, SO4,CH3COO) by the chemical root method. The XRD data have been recorded at DAE, IUC Indore.XANES spectra have been recorded at the K-edge of Cu using the dispersive beam line at 2.5GeV Indus-2 synchrotron radiation source RRCAT (Raja Ramanna Center for Advance Technology), Indore, India. XRD and XANES data have been analysed using the computer software Origin 8.0 professional and Athena. X-ray diffraction studies of all the complexes are indicative of their crystalline nature. The crystalline size of the samples is estimated using the Scherer's formula. The values of the chemical shifts suggest that copper is in oxidation state +2 in all of the complexes.

Characterization and EXAFS Studies of Cobalt Synthesized by sol-gel auto Combustion Method

The Co-Ni ferrites with general formula NiXCo1-XFe2O4 (where X=0.0, 0.1, 0.15, 2, 0.4) were prepared by Sol-gel auto combustion method. X-ray, FTIR and EXAFS measurement were carried out. Extended X ray Absorption Fine Structure (EXAFS) spectra have been recorded at the K-edge of Fe using the Dispersive EXAFS (DEXAFS) beam line-8 Indus-2 synchrotron radiation source RRCAT, Indore, India. The EXAFS data have been analysed using the computer softer Athena. These have been used to determine the Bond length in these ferrites with help of four different methods, namely, Levy's, Lytle's and Lytle, Sayers and stern's (LSS).

Optical constants of off-stoichiometric aluminum oxide thin film in 6–20 nm soft-X-ray/extreme ultraviolet region

In this study, the optical constants of a sputter-deposited aluminum oxide thin film are measured in the soft-X-ray wavelength region of 6–20 nm using an angle-dependent X-ray reflectivity technique at the Indus-1 synchrotron radiation source. The chemical composition of the aluminum oxide thin film is analyzed by an X-ray photoelectron spectroscopy technique. Grazing incidence X-ray reflectivity results indicate that the density of the film is lower (2.93 g·cm−3) than that of bulk alumina (3.97 g·cm−3). The experimentally obtained optical constants correlate with the film composition and density. It is found that the experimentally measured delta and beta values are 5–33% higher than the tabulated values except those near the Al L edge (17 nm) region, where the experimentally obtained beta values are 7–20% lower and the delta values are 50–120% higher. This large mismatch observed between the experimental values and Henke et al. data is attributed to the reduced film density and the presence of a mixed phase of AlOx and Al2O3, as evidenced by X-ray photoelectron spectroscopy.

Optical constants of e-beam-deposited zirconium dioxide measured in the 55-150 Å wavelength region using the reflectivity technique.

In the present study, optical constants of e-beam-deposited zirconium dioxide (ZrO2) thin film are determined in the 55-150 Å soft x-ray wavelength region using the angle-dependent reflectivity technique. Soft x-ray reflectivity measurements are carried out using the reflectivity beamline at the Indus-1 synchrotron radiation source. Derived optical constants (δ and β) are compared with the tabulated values of Henke et al. [http://henke.lbl.gov/optical_constants/asf.html]. It is found that the measured δ values are consistently lower than the tabulated bulk values in the 70-150 Å wavelength region. In this region, the delta values are lower by 19%-24% from the tabulated data. Below the Zr M4 edge (66.3 Å), a deviation in delta values is found as ∼2%-21%. These changes are attributed to growth-related defects (oxygen and voids) and variation in film stoichiometry. To the best of our knowledge, the present study gives the first reported experimental values of optical constants for ZrO2 in the 55-150 Å wavelength region.