Gamma-irradiation-induced micro-structural variations in flame-retardant polyurethane foam using synchrotron X-ray micro-tomography.

Flame-retardant polyurethane foams are potential packing materials for the transport casks of highly active nuclear materials for shock absorption and insulation purposes. Exposure of high doses of gamma radiation causes cross-linking and chain sectioning of macromolecules in this polymer foam, which leads to reorganization of their cellular microstructure and thereby variations in physico-mechanical properties. In this study, in-house-developed flame-retardant rigid polyurethane foam samples were exposed to gamma irradiation doses in the 0-20 kGy range and synchrotron radiation X-ray micro-computed tomography (SR-µCT) imaging was employed for the analysis of radiation-induced morphological variations in their cellular microstructure. Qualitative and quantitative analysis of SR-µCT images has revealed significant variations in the average cell size, shape, wall thickness, orientations and spatial anisotropy of the cellular microstructure in polyurethane foam.

HAXPES beamline PES-BL14 at the Indus-2 synchrotron radiation source.

The Hard X-ray Photo-Electron Spectroscopy (HAXPES) beamline (PES-BL14), installed at the 1.5 T bending-magnet port at the Indian synchrotron (Indus-2), is now available to users. The beamline can be used for X-ray photo-emission electron spectroscopy measurements on solid samples. The PES beamline has an excitation energy range from 3 keV to 15 keV for increased bulk sensitivity. An in-house-developed double-crystal monochromator [Si (111)] and a platinum-coated X-ray mirror are used for the beam monochromatization and manipulation, respectively. This beamline is equipped with a high-energy (up to 15 keV) high-resolution (meV) hemispherical analyzer with a microchannel plate and CCD detector system with SpecsLab Prodigy and CasaXPS software. Additional user facilities include a thin-film laboratory for sample preparation and a workstation for on-site data processing. In this article, the design details of the beamline, other facilities and some recent scientific results are described.

An environmental gamma spectrometry system with CsI(Tl) scintillator and FPGA based MCA for open field deployment.

Inorganic scintillator-based gamma spectrometry is typically carried out under laboratory conditions by using systems that require AC mains supply and dedicated computers for their operation. In this study, an in-house grown CsI(Tl) single crystal scintillator is optically coupled to a bialkali photomultiplier tube (PMT). The output of the PMT is fed to a pulse processing chain consisting of a preamplifier followed by an in-house designed and developed field programmable gate array (FPGA) based multichannel analyzer (MCA). Spectral data from this MCA is sent via serial communication to a microcontroller. A global system for mobile communications (GSM) modem transmits this data in the form of short message service (SMS) packets to a central receiving station, where the spectrum is reconstructed. The requirement of on-site data logging computer to store large spectral data has thereby been eliminated, which, in turn, has eliminated the requirement of AC power supply, reduced the overall power consumption and size of the system, and made it possible to develop a standalone solar-powered unit. For further reduction of overall power consumption, the spectrometer is turned-on only when a Geiger Mueller (GM) counter based gross gamma detection circuit, also included in the system, detects an ambient gamma dose rate beyond a pre-set threshold level. A mathematical methodology has also been implemented for restoration of recorded spectra, shifted due to temperature variations in the environment. All these features have been integrated and a standalone, solar-powered and battery operated field-deployable environmental gamma spectrometry system (EGSS) has been developed and tested for open field deployment. Presence of 41Ar in ambient air was successfully detected by the system.

Electrostatic ion trap and Fourier transform measurements for high-resolution mass spectrometry.

We report on the development of an electrostatic ion trap for high-resolution mass spectrometry. The trap works on purely electrostatic fields and hence trapping and storing of ions is not mass restrictive, unlike other techniques based on Penning, Paul, or radio frequency quadrupole ion traps. It allows simultaneous trapping and studying of multiple mass species over a large mass range. Mass spectra were recorded in "dispersive" and "self-bunching" modes of ions. Storage lifetimes of about 100 ms and mass resolving power of about 20,000 could be achieved from the fifth harmonic Fourier transform spectrum of Xe ions recorded in the self-bunching mode.

Development of X-ray CCD camera based X-ray micro-CT system.

Availability of microfocus X-ray sources and high resolution X-ray area detectors has made it possible for high resolution microtomography studies to be performed outside the purview of synchrotron. In this paper, we present the work towards the use of an external shutter on a high resolution microtomography system using X-ray CCD camera as a detector. During micro computed tomography experiments, the X-ray source is continuously ON and owing to the readout mechanism of the CCD detector electronics, the detector registers photons reaching it during the read-out period too. This introduces a shadow like pattern in the image known as smear whose direction is defined by the vertical shift register. To resolve this issue, the developed system has been incorporated with a synchronized shutter just in front of the X-ray source. This is positioned in the X-ray beam path during the image readout period and out of the beam path during the image acquisition period. This technique has resulted in improved data quality and hence the same is reflected in the reconstructed images.

Organic-Inorganic Composite Films Based on Gd3Ga3Al2O12:Ce Scintillator Nanoparticles for X-ray Imaging Applications.

Organic-inorganic nanocomposite self-standing films of Gd3Ga3Al2O12 (GGAG) uniformly dispersed in poly(methyl methacrylate) (PMMA) and polystyrene polymer are prepared for radiography application. GGAG:Ce nanoscintillator has been chosen because of its high light output and fast decay time. The nanopowder of GGAG is synthesized by coprecipitation method and dispersed in the polymer matrix by a simple blending technique. The nanocomposite films of thickness in the range of 150-450 µm with a very high inorganic content is achieved by this technique. These films are characterized by their uniformity, optical absorption, photoluminescence, and radioluminescence. These films are further tested for their application in radiography by recording X-ray images using a commercially available charge-coupled device camera. A resolution of 10 lp/mm is obtained using GGAG:PMMA composite film with 50% loading, confirming their application in imaging devices.

Enhanced field-emission from SnO2:WO(2.72) nanowire heterostructures.

The field-emission properties of SnO(2):WO(2.72) hierarchical nanowire heterostructure have been investigated. Nanoheterostructure consisting of SnO(2) nanowires as stem and WO(2.72) nanothorns as branches are synthesized in two steps by physical vapor deposition technique. Their field emission properties were recorded. A low turn-on field of ~0.82 V/µm (to draw an emission current density ~10 µA/cm(2)) is achieved along with stable emission for 4 h duration. The emission characteristic shows the SnO(2):WO(2.72) nanoheterostructures are extremely suitable for field-emission applications.

Luminescence properties of Eu3+ doped CaMoO4 nanoparticles.

When Eu(3+) ions occupy Ca(2+) sites of CaMoO(4), which has a body centered tetragonal structure with inversion symmetry, only the magnetic dipole transition ((5)D(0)→(7)F(1)) should be allowed according to Judd-Ofelt theory. Even if there are a few distortions in the Eu(3+) environment, its intensity should be more than that of the electric dipole transition ((5)D(0)→(7)F(2)). We report here the opposite effect experimentally and ascribe this to the polarizability effect of the MoO(4) tetrahedron, which is neighboring to EuO(8) (symmetric environment). The contribution of the energy transfer process from the Mo-O charge transfer band to Eu(3+) and the role of Eu(3+) over the surface of the particle could be distinguished when luminescence decay processes were measured at two different excitations (250 and 398 nm). Further, the luminescence intensities and lifetimes increase significantly with increasing heat-treatment temperature of the doped samples. This is attributed to the reduction of H(2)O from the surface of the particles and a non-radiative process after heat treatment.

NH3 gas sensing properties of nanocrystalline ZnO based thick films.

Zinc acetate derived precursor used in the present sol-gel synthesis of zinc oxide nanoparticles is described. The reaction product obtained before and after reflux of propanolic zinc acetate solution have been studied by UV-vis, photoluminescence and FT-IR studies which confirm the formation of oligomeric precursor Zn4O(Ac)6 (Ac=CH3COO). The formation of approximately 7 nm zinc oxide nanoparticles were confirmed by X-ray diffraction (XRD) and Transmission electron microscopic studies (TEM). The gaseous ammonia gas sensing characteristics of the nano-zinc oxide sensor showed high sensitivity compared to sensor fabricated with commercial zinc oxide powder.