Publications

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This project uses advanced ceramic processes to fabricate large, optical-quality, polycrystalline lanthanum halide scintillators to replace small single crystals produced by the conventional Bridgman growth method. The new approach not only removes the size constraint imposed by the growth method, but also offers the potential advantages of both reducing manufacturing cost and increasing production rate. The project goal is to fabricate dense lanthanum halide ceramics with a preferred crystal orientation by applying texture engineering and solid-state conversion to reduce the thermal mechanical stress in the ceramic and minimize scintillation light scattering at grain boundaries. Ultimately, this method could deliver the sought-after high sensitivity and <3% energy resolution at 662 keV of lanthanum halide scintillators and unleash their full potential for advanced gamma ray detection, enabling rapid identification of radioactive materials in a variety of practical applications. This report documents processing details from powder synthesis, seed particle growth, to final densification and texture development of cerium doped lanthanum bromide (LaBr{sub 3}:Ce{sup +3}) ceramics. This investigation demonstrated that: (1) A rapid, flexible, cost efficient synthesis method of anhydrous lanthanum halides and their solid solutions was developed. Several batches of ultrafine LaBr{sub 3}:Ce{sup +3} powder, free of oxyhalide, were produced by a rigorously controlled process. (2) Micron size ({approx} 5 {micro}m), platelet shape LaBr{sub 3} seed particles of high purity can be synthesized by a vapor phase transport process. (3) High aspect-ratio seed particles can be effectively aligned in the shear direction in the ceramic matrix, using a rotational shear-forming process. (4) Small size, highly translucent LaBr{sub 3} (0.25-inch diameter, 0.08-inch thick) samples were successfully fabricated by the equal channel angular consolidation process. (5) Large size, high density, translucent LaBr{sub 3} ceramics samples (3-inch diameter, > 1/8-inch thick) were fabricated by hot pressing, demonstrating the superior manufacturability of the ceramic approach over single crystal growth methods in terms of size capability and cost. (6) Despite all these advances, evidence has shown that LaBr{sub 3} is thermally unstable at temperatures required for the densification process. This is particularly true for material near the surface where lattice defects and color centers can be created as bromine becomes volatile at high temperatures. Consequently, after densification these samples made using chemically prepared ultrafine powders turned black. An additional thermal treatment in a flowing bromine condition proved able to reduce the darkness of the surface layer for these densified samples. These observations demonstrated that although finer ceramic powders are desirable for densification due to a stronger driving force from their large surface areas, the same desirable factor can lead to lattice defects and color centers when these powders are densified at higher temperatures where material near the surface becomes thermally unstable.

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A heteroleptic titanium metal alkoxide (OPy){sub 2}Ti(4MP){sub 2}, where OPy = NC{sub 5}H{sub 4}(CH{sub 2}O)-2 and 4MP = OC{sub 6}H{sub 4}(SH)-4, was investigated as a candidate precursor for the solution-based (sol-gel) synthesis of titanium oxide via the photoactivation of intermolecular linking reactions (e.g., hydrolysis/condensation). The evolution of the electronic structure of the solution-based molecule arising from conventional (dark) chemical reaction kinetics was compared with that of samples exposed to ultraviolet (UV) radiation at wavelengths of {lambda} = 337.1 nm and 405 nm using UV-visible absorption spectroscopy. Photoinduced changes in the spectra were examined as a function of both the incident wavelength of exposure and the total fluence. Experimental results confirm the UV-induced modification of spectral absorption features, attributed to ligand-localized and charge transfer transitions accompanied by structural changes associated with hydrolysis and condensation. The photoenhancement of reaction kinetics in these processes was confirmed by the increased modification of the absorption features in the solution spectra, which saturated more rapidly under UV-illumination than under dark conditions. Similar saturation behaviors were observed for both the 337.1 nm and the 405 nm incident wavelengths with the same total deposited energy density indicating a relative insensitivity of the photoinduced response to excitation energy for the wavelengths and fluences studied.

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The global market for wireless sensor networks in 2010 will be valued close to $10 B, or 200 M units. TPL, Inc. is a small Albuquerque based business that has positioned itself to be a leader in providing uninterruptible power supplies in this growing market with projected revenues expected to exceed $26 M in 5 years. This project focused on improving TPL, Inc.'s patent-pending EnerPak{trademark} device which converts small amounts of energy from the environment (e.g., vibrations, light or temperature differences) into electrical energy that can be used to charge small energy storage devices. A critical component of the EnerPak{trademark} is the supercapacitor that handles high power delivery for wireless communications; however, optimization and miniaturization of this critical component is required. This proposal aimed to produce prototype microsupercapacitors through the integration of novel materials and fabrication processes developed at New Mexico Technology Research Collaborative (NMTRC) member institutions. In particular, we focused on developing novel ruthenium oxide nanomaterials and placed them into carbon supports to significantly increase the energy density of the supercapacitor. These improvements were expected to reduce maintenance costs and expand the utility of the TPL, Inc.'s device, enabling New Mexico to become the leader in the growing global wireless power supply market. By dominating this niche, new customers were expected to be attracted to TPL, Inc. yielding new technical opportunities and increased job opportunities for New Mexico.

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A specially designed specimen holder employing a beryllium dome has been fabricated for collection of X-ray diffraction (XRD) data from highly reactive materials. The specimen holder has a robust O-ring type seal (< 10-9 Torr) and no observed intensity artifacts in the 1° to 150° 2θ range. The design also minimizes specimen displacement errors and allows for analysis of both powders and bulk specimens (i.e., pellets). The simple design makes for straightforward assembly of the holder within the confines of a glove box. XRD analysis of hygroscopic LaBr3 powders collected with this holder are suitable for Rietveld structure refinement, yielding unit cell lattice parameters of a=7.9703(6) Å and c=4.5122(6) Å cell volume= 248.44(6) Å3; Rp =7.70%. © 2008 International Centre for Diffraction Data.

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The CSI: Dognapping Workshop is a culmination of the more than 65 Sandian staff and intern volunteers dedication to exciting and encouraging the next generation of scientific leaders. This 2 hour workshop used a 'theatrical play' and 'hands on' activities that was fun, exciting and challenging for 3rd-5th graders while meeting science curriculum standards. In addition, new pedagogical methods were developed in order to introduce nanotechnology to the public. Survey analysis indicated that the workshop had an overall improvement and positive impact on helping the students to understand concepts from materials science and chemistry as well as increased our interaction with the K-5 community. Anecdotal analyses showed that this simple exercise will have far reaching impact with the results necessary to maintain the United States as the scientific leader in the world. This experience led to the initiation of over 100 Official Junior Scientists.

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The formation of 10-nm ZnO nanopyramids using a simple synthetic route has been isolated from the reaction of Zn(OAc)2·2H2O in 1,4-butanediol followed by ripening at 90°C. This was accomplished by establishing control over the Ostwald ripening process through the use of a carboxylic acid specific adsorbate. Using a variety of analytical methods, it is proposed that the carboxylate groups in the acetate precursor stabilize the {101} habit planes, creating septahedral shapes or nanopyramids. Particle assembly into crystallographically oriented dimers was observed with high specificity, and the association mechanism is suggested to relate to the crystal polarity and the variation in specific adsorption of the carboxylic acid to the surface facets. These materials are a candidate for biological labeling applications in living cells.

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