A high precision gas flow cell for performing in situ neutron studies of local atomic structure in catalytic materials.

Gas-solid interfaces enable a multitude of industrial processes, including heterogeneous catalysis; however, there are few methods available for studying the structure of this interface under operating conditions. Here, we present a new sample environment for interrogating materials under gas-flow conditions using time-of-flight neutron scattering under both constant and pulse probe gas flow. Outlined are descriptions of the gas flow cell and a commissioning example using the adsorption of N2 by Ca-exchanged zeolite-X (Na78-2xCaxAl78Si144O384,x ≈ 38). We demonstrate sensitivities to lattice contraction and N2 adsorption sites in the structure, with both static gas loading and gas flow. A steady-state isotope transient kinetic analysis of N2 adsorption measured simultaneously with mass spectrometry is also demonstrated. In the experiment, the gas flow through a plugged-flow gas-solid contactor is switched between N215 and N214 isotopes at a temperature of 300 K and a constant pressure of 1 atm; the gas flow and mass spectrum are correlated with the structure factor determined from event-based neutron total scattering. Available flow conditions, sample considerations, and future applications are discussed.

How a Nanostructure's Shape Affects its Lifetime in the Environment: Comparing a Silver Nanocube to a Nanoparticle When Dispersed in Aqueous Media.

Herein, we detail how the morphology of a nanomaterial affects its environmental lifetime in aquatic ecosystems. In particular, we focus on the cube and particle nanostructures of Ag and age them in various aquatic mediums including synthetic hard water, pond water, and seawater. Our results show that in the synthetic hard water and pond water cases, there was little difference in the rate of morphological changes as determined by UV-vis spectroscopy. However, when these samples were analyzed with transmission electron microscopy, radically different mechanisms in the loss of their original nanostructures were observed. Specifically, for the nanocube we observed that the corners of the cubes had become more rounded, whereas the aged nanoparticles formed large aggregates. Most interestingly, when the seawater samples were analyzed, the nanocubes showed a substantially higher stability in maintaining the nano length scale in comparison to nanoparticles overtime. Moreover, high-resolution transmission electron microscopy analysis allowed us to determine that Ag+ ions diffused away from both the edge and from the faces of the cube, whereas the nanoparticle rapidly aggregated under the harsh seawater conditions.

Potential application of fabricated sulfide-based scintillation materials for radiation detection.

In our laboratories, we have produced ZnS(Ag)/6Li sol-gel scintillation materials which produce an excellent light output with an alpha radiation (compared to commercial high temperature lithiated glass; KG-2 and a plastic scintillator; BC-400). However, when tested with a neutron radiation, the opacity of the ZnS(Ag)/6Li sol-gel scintillation materials, which were composed of a homogeneous micron-sized ZnS(Ag), prevented a clear neutron energy peak formation, thus making it difficult to set a threshold for neutron-gamma discrimination. In an effort to increase the transparency of the scintillation materials and to develop new technologies to fabricate sulfide-based scintillation materials for neutron detection, we turned to the methods of a chemical bath deposition (CBD) and a nano-particle synthesis for possible solutions.

Metastable tetragonal phase CdWO4 nanoparticles synthesized with a solvothermal method.

CdWO4 has only previously been reported in the monoclinic, or wolframite, phase. Here we report the first metastable, tetragonal or scheelite, CdWO4 nanopowder. The tetragonal CdWO4 was synthesized by a propylene glycol solvothermal method. The scheelite phase is stabilized by a combination of high surface area and surface complexation by the propylene glycol. The CdWO4 is stable at 1 bar to 300 degrees C, and converts back to the monoclinic wolframite phase between 300 and 500 degrees C. The nanopowder exhibits cubic morphology and the average particle size of the nanopowder is around 50 nm.