Publications

An evaluation of calcium tungsten oxide (CaWO4) nanoparticles' properties was conducted using the powders generated from an all-alkoxide solvothermal (SOLVO) route. The reaction involved a toluene/pyridine mixture of tungsten(V) ethoxide ([W(OEt)5]) with calcium bis(trimethyl silyl) amide ([Ca(N(Si(CH3)3)2]) modified in situ by a series of alcohols (H-OR) including neo-pentanol (H-OCH2C(CH 3)3 or H-ONep) or sterically varied aryl alcohols (H-OC6H3R2-2,6 where R = CH3 (H-DMP), CH(CH3)2 (H-DIP), C(CH3)3 (DBP))]. Attempts to identify the intermediates generated from this series of reactions led to the crystallographic identification of [(OEt) 4W(μ-OEt)2Ca(DBP)2] (1). Each different SOLVO generated "initial" powder was found by transmission electron microscopy (TEM) and powder X-ray diffraction (PXRD) to be nanomaterials roughly assigned as the scheelite phase (PDF 00-041-1431); however, these initial powders displayed no luminescent behavior as determined by photoluminescence (PL) measurements. Thermal processing of these powders at 450, 650, and 750 C yielded progressively larger and more crystalline scheelite nanoparticles. Both PL and cathodoluminescent (CL) emission (422-425 and 429 nm, respectively) were observed for the nanomaterials processed at 750 C. Ion beam induced luminescence (IBIL, 478 nm) appeared to be in agreement with these PL and CL measurements. Further processing of the materials at 1000 C, led to a coalescence of the particles and significant improvement in the observed PL (445 nm) and CL measurements; however, the IBIL spectrum of this material was significantly altered upon exposure. These data suggest that the smaller nanoparticles were more stable to radiation effects possibly due to the lack of energy deposits based on the short track length; whereas the larger particles appear to suffer from radiation induced structural defects. © 2013 American Chemical Society.

An ideal ³He detector replacement for the near- to medium-term future will use materials that are easy to produce and well understood, while maintaining thermal neutron detection efficiency and gamma rejection close to the ³He standard. Toward this end, we investigated the use of standard alkali halide scintillators interfaced with ⁶Li and read out with photomultiplier tubes (PMTs). Thermal neutrons are captured on ⁶Li with high efficiency, emitting high-energy and triton (³H) reaction products. These particles deposit energy in the scintillator, providing a thermal neutron signal; discrimination against gamma interactions is possible via pulse shape discrimination (PSD), since heavy particles produce faster pulses in alkali halide crystals. We constructed and tested two classes of detectors based on this concept. In one case ⁶Li is used as a dopant in polycrystalline NaI; in the other case a thin Li foil is used as a conversion layer. In the configurations studied here, these systems are sensitive to both gamma and neutron radiation, with discrimination between the two and good energy resolution for gamma spectroscopy. We present results from our investigations, including measurements of the neutron efficiency and gamma rejection for the two detector types. We also show a comparison with Cs₂LiYCl₆:Ce (CLYC), which is emerging as the standard scintillator for simultaneous gamma and thermal neutron detection, and also allows PSD. We conclude that ⁶Li foil with CsI scintillating crystals has near-term promise as a thermal neutron detector in applications previously dominated by ³He detectors. The other approach, ⁶Li-doped alkali halides, has some potential, but require more work to understand material properties and improve fabrication processes.

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Scintillating nanomaterials are being investigated as replacements for fragile, difficult to synthesize single crystal radiation detectors, but greater insight into their structural stability when exposed to extreme environments is needed to determine long-term performance. An initial study using high-Z cadmium tungstate (CdWO4) nanorods and an in-situ ion irradiation transmission electron microscope (I3TEM) was performed to determine the feasibility of these extreme environment experiments. The I3TEM presents a unique capability that permits the real time characterization of nanostructures exposed to various types of ion irradiation. In this work, we investigated the structural evolution of CdWO4 nanorods exposed to 50 nA of 3 MeV copper (3+) ions. During the first several minutes of exposure, the nanorods underwent significant structural evolution. This appears to occur in two steps where the nanorods are first segmented into smaller sections followed by the sintering of adjacent particles into larger nanostructures. An additional study combined in-situ ion irradiation with electron tomography to record tilt series after each irradiation dose; which were then processed into 3D reconstructions to show radiation damage to the material over time. Analyses to understand the mechanisms and structure-property relationships involved are ongoing. © 2012 SPIE.

This work was funded by the U.S. Department of Energy Office of Nonproliferation Research to develop elpasolite materials, with an emphasis on high-atomic-number rare-earth elpasolites for gamma-ray spectrometer applications. Low-cost, high-performance gamma-ray spectrometers are needed for detection of nuclear proliferation. Cubic materials, such as some members of the elpasolite family (A2BLnX6; Ln-lanthanide and X-halogen), hold promise due to their high light output, proportionality, and potential for scale-up. Using both computational and experimental studies, a systematic investigation of the compositionstructureproperty relationships of these high-atomic-number elpasolite halides was performed. The results reduce the barrier to commercialization of large single crystals or transparent ceramics, and will facilitate economical scale-up of elpasolites for high-sensitivity gamma-ray spectroscopy.

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An ideal 3He detector replacement for the nearto medium-term future will use materials that are easy to produce and well understood, while maintaining thermal neutron detection efficiency and gamma rejection close to the 3He standard. Toward this end, we are investigating the use of standard alkali halide scintillators interfaced with 6Li and read out with photomultiplier tubes (PMTs). Thermal neutrons are captured on 6Li with high efficiency, emitting high-energy α and triton (3H) reaction products. These particles deposit energy in the scintillator, providing a thermal neutron signal; discrimination against gamma interactions is possible via pulse shape discrimination (PSD), since heavy particles produce faster pulses in inorganic scintillating crystals. We constructed and tested two classes of detectors based on this concept. In one case 6Li is used as a dopant in polycrystalline NaI; in the other case a thin Li foil is used as a conversion layer. We present results from these investigations, including measurements of the neutron efficiency and gamma rejection for the two detector types. © 2011 IEEE.

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