Publications

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Arsenic ion implant energy effects on CMOS gate oxide hardness

Proposed for publication in the IEEE Transactions on Nuclear Science.

Draper, Bruce L.; Shaneyfelt, Marty R.; Young, Ralph W.; Headley, Thomas J.; Dondero, Richard D.

Under conditions that were predicted as 'safe' by well-established TCAD packages, radiation hardness can still be significantly degraded by a few lucky arsenic ions reaching the gate oxide during self-aligned CMOS source/drain ion implantation. The most likely explanation is that both oxide traps and interface traps are created when ions penetrate and damage the gate oxide after channeling or traveling along polysilicon grain boundaries during the implantation process.

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Final report : compliant thermo-mechanical MEMS actuators, LDRD #52553

Plass, R.A.; Headley, Thomas J.; Walraven, J.A.

Thermal actuators have proven to be a robust actuation method in surface-micromachined MEMS processes. Their higher output force and lower input voltage make them an attractive alternative to more traditional electrostatic actuation methods. A predictive model of thermal actuator behavior has been developed and validated that can be used as a design tool to customize the performance of an actuator to a specific application. This tool has also been used to better understand thermal actuator reliability by comparing the maximum actuator temperature to the measured lifetime. Modeling thermal actuator behavior requires the use of two sequentially coupled models, the first to predict the temperature increase of the actuator due to the applied current and the second to model the mechanical response of the structure due to the increase in temperature. These two models have been developed using Matlab for the thermal response and ANSYS for the structural response. Both models have been shown to agree well with experimental data. In a parallel effort, the reliability and failure mechanisms of thermal actuators have been studied. Their response to electrical overstress and electrostatic discharge has been measured and a study has been performed to determine actuator lifetime at various temperatures and operating conditions. The results from this study have been used to determine a maximum reliable operating temperature that, when used in conjunction with the predictive model, enables us to design in reliability and customize the performance of an actuator at the design stage.

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Containment of uranium in the proposed Egyptian geologic repository for radioactive waste using hydroxyapatite

Hasan, Ahmed H.; Larese, Kathleen C.; Headley, Thomas J.; Zhao, Hongting Z.; Salas, Fred S.

Currently, the Egyptian Atomic Energy Authority is designing a shallow-land disposal facility for low-level radioactive waste. To insure containment and prevent migration of radionuclides from the site, the use of a reactive backfill material is being considered. One material under consideration is hydroxyapatite, Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, which has a high affinity for the sorption of many radionuclides. Hydroxyapatite has many properties that make it an ideal material for use as a backfill including low water solubility (K{sub sp}>10{sup -40}), high stability under reducing and oxidizing conditions over a wide temperature range, availability, and low cost. However, there is often considerable variation in the properties of apatites depending on source and method of preparation. In this work, we characterized and compared a synthetic hydroxyapatite with hydroxyapatites prepared from cattle bone calcined at 500 C, 700 C, 900 C and 1100 C. The analysis indicated the synthetic hydroxyapatite was similar in morphology to 500 C prepared cattle hydroxyapatite. With increasing calcination temperature the crystallinity and crystal size of the hydroxyapatites increased and the BET surface area and carbonate concentration decreased. Batch sorption experiments were performed to determine the effectiveness of each material to sorb uranium. Sorption of U was strong regardless of apatite type indicating all apatite materials evaluated. Sixty day desorption experiments indicated desorption of uranium for each hydroxyapatite was negligible.

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Microtubule-templated biomimetic mineralization of lepidocrocite

Proposed for publication in Advanced Functional Materials.

Bunker, B.C.; Boal, Andrew B.; Headley, Thomas J.; Tissot, Ralph G.; Bunker, B.C.

Protein microtubules (MTs) 25 nm in diameter and tens of micrometers long have been used as templates for the biomimetic mineralization of FeOOH. Exposure of MTs to anaerobic aqueous solutions of Fe{sup 2+} buffered to neutral pH followed by aerial oxidation leads to the formation of iron oxide coated MTs. The iron oxide layer was found to grow via a two-step process: initially formed 10-30 nm thick coatings were found to be amorphous in structure and comprised of several iron-containing species. Further growth resulted in MTs coated with highly crystalline layers of lepidocrocite with a controllable thickness of up to 125 nm. On the micrometer size scale, these coated MTs were observed to form large, irregular bundles containing hundreds of individually coated MTs. Iron oxide grew selectively on the MT surface, a result of the highly charged MT surface that provided an interface favorable for iron oxide nucleation. This result illustrates that MTs can be used as scaffolds for the in-situ production of high-aspect-ratio inorganic nanowires.

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Containment of uranium in the proposed Egyptian geologic repository for radioactive waste using hydroxyapatite

Larese, Kathleen C.; Hasan, Ahmed H.; Larese, Kathleen C.; Headley, Thomas J.; Zhao, Hongting Z.; Salas, Fred S.

Currently, the Egyptian Atomic Energy Authority is designing a shallow-land disposal facility for low-level radioactive waste. To insure containment and prevent migration of radionuclides from the site, the use of a reactive backfill material is being considered. One material under consideration is hydroxyapatite, Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, which has a high affinity for the sorption of many radionuclides. Hydroxyapatite has many properties that make it an ideal material for use as a backfill including low water solubility (K{sub sp} > 10{sup -40}), high stability under reducing and oxidizing conditions over a wide temperature range, availability, and low cost. However, there is often considerable variation in the properties of apatites depending on source and method of preparation. In this work, we characterized and compared a synthetic hydroxyapatite with hydroxyapatites prepared from cattle bone calcined at 500 C, 700 C, 900 C and 1100 C. The analysis indicated the synthetic hydroxyapatite was similar in morphology to 500 C prepared cattle hydroxyapatite. With increasing calcination temperature the crystallinity and crystal size of the hydroxyapatites increased and the BET surface area and carbonate concentration decreased. Batch sorption experiments were performed to determine the effectiveness of each material to sorb uranium. Sorption of U was strong regardless of apatite type indicating all apatite materials evaluated. Sixty day desorption experiments indicated desorption of uranium for each hydroxyapatite was negligible.

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Growth and morphology of cadmium chalcogenides : the synthesis of nanorods, tetrapods, and spheres from CdO and Cd(O[2]CCH[3])[2]

Proposed for publication in the Journal of Chemistry and Materials.

Bunge, Scott D.; Bunge, Scott D.; Boyle, Timothy J.; Rodriguez, Marko A.; Headley, Thomas J.

In this work, we investigated the controlled growth of nanocrystalline CdE (E = S, Se, and Te) via the pyrolysis of CdO and Cd(O2CCH3)2 precursors, at the specific Cd to E mole ratio of 0.67 to 1. The experimental results reveal that while the growth of CdS produces only a spherical morphology, CdSe and CdTe exhibit rod-like and tetrapod-like morphologies of temporally controllable aspect ratios. Over a 7200 s time period, CdS spheres grew from 4 nm (15 s aliquot) to 5 nm, CdSe nanorods grew from dimensions of 10.8 x 3.6 nm (15 s aliquot) to 25.7 x 11.2 nm, and CdTe tetrapods with arms 15 x 3.5 nm (15 s aliquot) grew into a polydisperse mixture of spheres, rods, and tetrapods on the order of 20 to 80 nm. Interestingly, long tracks of self-assembled CdSe nanorods (3.5 x 24 nm) of over one micron in length were observed. The temporal growth for each nanocrystalline material was monitored by UV-VIS spectroscopy, transmission electron spectroscopy, and further characterized by powder X-ray diffraction. This study has elucidated the vastly different morphologies available for CdS, CdSe, and CdTe during the first 7200 s after injection of the desired chalcogenide.

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Verification, validation, and predictive capability in computational engineering and physics

Bunge, Scott D.; Bunge, Scott D.; Boyle, Timothy J.; Headley, Thomas J.; Kotula, Paul G.; Rodriguez, Marko A.

Developers of computer codes, analysts who use the codes, and decision makers who rely on the results of the analyses face a critical question: How should confidence in modeling and simulation be critically assessed? Verification and validation (V&V) of computational simulations are the primary methods for building and quantifying this confidence. Briefly, verification is the assessment of the accuracy of the solution to a computational model. Validation is the assessment of the accuracy of a computational simulation by comparison with experimental data. In verification, the relationship of the simulation to the real world is not an issue. In validation, the relationship between computation and the real world, i.e., experimental data, is the issue.

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Solidification Diagnostics for Joining and Microstructural Simulations

Robino, Charles V.; Robino, Charles V.; Hall, Aaron C.; Headley, Thomas J.; Roach, R.A.

Solidification is an important aspect of welding, brazing, soldering, LENS fabrication, and casting. The current trend toward utilizing large-scale process simulations and materials response models for simulation-based engineering is driving the development of new modeling techniques. However, the effective utilization of these models is, in many cases, limited by a lack of fundamental understanding of the physical processes and interactions involved. In addition, experimental validation of model predictions is required. We have developed new and expanded experimental techniques, particularly those needed for in-situ measurement of the morphological and kinetic features of the solidification process. The new high-speed, high-resolution video techniques and data extraction methods developed in this work have been used to identify several unexpected features of the solidification process, including the observation that the solidification front is often far more dynamic than previously thought. In order to demonstrate the utility of the video techniques, correlations have been made between the in-situ observations and the final solidification microstructure. Experimental methods for determination of the solidification velocity in highly dynamic pulsed laser welds have been developed, implemented, and used to validate and refine laser welding models. Using post solidification metallographic techniques, we have discovered a previously unreported orientation relationship between ferrite and austenite in the Fe-Cr-Ni alloy system, and have characterized the conditions under which this new relationship develops. Taken together, the work has expanded both our understanding of, and our ability to characterize, solidification phenomena in complex alloy systems and processes.

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Characterization of UOP IONSIV IE-911

Nyman, M.; Nenoff, T.M.; Headley, Thomas J.

As a participating national lab in the inter-institutional effort to resolve performance issues of the non-elutable ion exchange technology for Cs extraction, they have carried out a series of characterization studies of UOP IONSIV{reg_sign} IE-911 and its component parts. IE-911 is a bound form (zirconium hydroxide-binder) of crystalline silicotitanate (CST) ion exchanger. The crystalline silicotitanate removes Cs from solutions by selective ion exchange. The performance issues of primary concern are: (1) excessive Nb leaching and subsequent precipitation of column-plugging Nb-oxide material, and (2) precipitation of aluminosilicate on IE-911 pellet surfaces, which may be initiated by dissolution of Si from the IE-911, thus creating a supersaturated solution with respect to silica. In this work, they have identified and characterized Si- and Nb-oxide based impurity phases in IE-911, which are the most likely sources of leachable Si and Nb, respectively. Furthermore, they have determined the criteria and mechanism for removal from IE-911 of the Nb-based impurity phase that is responsible for the Nb-oxide column plugging incidents.

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Failure analysis of tungsten coated polysilicon micromachined microengines

Proceedings of SPIE - The International Society for Optical Engineering

Walraven, J.A.; Mani, Seethambal S.; Fleming, J.G.; Headley, Thomas J.; Kotula, Paul G.; Pimentel, Alejandro A.; Rye, Michael J.; Tanner, Danelle M.; Smith, Norman F.

Failure analysis (FA) tools have been applied to analyze tungsten coated polysilicon microengines. These devices were stressed under accelerated conditions at ambient temperatures and pressure. Preliminary results illustrating the failure modes of microengines operated under variable humidity and ultra-high drive frequency will also be shown. Analysis of tungsten coated microengines revealed the absence of wear debris in microengines operated under ambient conditions. Plan view imaging of these microengines using scanning electron microscopy (SEM) revealed no accumulation of wear debris on the surface of the gears or ground plane on microengines operated under standard laboratory conditions. Friction bearing surfaces were exposed and analyzed using the focused ion beam (FIB). These cross sections revealed no accumulation of debris along friction bearing surfaces. By using transmission electron microscopy (TEM) in conjunction with electron energy loss spectroscopy (EELS), we were able to identify the thickness, elemental analysis, and crystallographic properties of tungsten coated MEMS devices. Atomic force microscopy was also utilized to analyze the surface roughness of friction bearing surfaces.

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Welding Behavior of Free Machining Stainless Steel

Welding Journal Research Supplement

Robino, Charles V.; Headley, Thomas J.; Michael, Joseph R.; Robino, Charles V.

The weld solidification and cracking behavior of sulfur bearing free machining austenitic stainless steel was investigated for both gas-tungsten arc (GTA) and pulsed laser beam weld processes. The GTA weld solidification was consistent with those predicted with existing solidification diagrams and the cracking response was controlled primarily by solidification mode. The solidification behavior of the pulsed laser welds was complex, and often contained regions of primary ferrite and primary austenite solidification, although in all cases the welds were found to be completely austenite at room temperature. Electron backscattered diffraction (EBSD) pattern analysis indicated that the nature of the base metal at the time of solidification plays a primary role in initial solidification. The solid state transformation of austenite to ferrite at the fusion zone boundary, and ferrite to austenite on cooling may both be massive in nature. A range of alloy compositions that exhibited good resistance to solidification cracking and was compatible with both welding processes was identified. The compositional range is bounded by laser weldability at lower Cr{sub eq}/Ni{sub eq} ratios and by the GTA weldability at higher ratios. It was found with both processes that the limiting ratios were somewhat dependent upon sulfur content.

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Microstructures of laser deposited 304L austenitic stainless steel

Headley, Thomas J.; Robino, Charles V.; Headley, Thomas J.

Laser deposits fabricated from two different compositions of 304L stainless steel powder were characterized to determine the nature of the solidification and solid state transformations. One of the goals of this work was to determine to what extent novel microstructure consisting of single-phase austenite could be achieved with the thermal conditions of the LENS [Laser Engineered Net Shape] process. Although ferrite-free deposits were not obtained, structures with very low ferrite content were achieved. It appeared that, with slight changes in alloy composition, this goal could be met via two different solidification and transformation mechanisms.

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Comparison of electrical CD measurements and cross-section lattice-plane counts of sub-micrometer features replicated in Silicon-on-Insulator materials

Headley, Thomas J.; Everist, Sarah C.; Everist, Sarah C.

Electrical test structures of the type known as cross-bridge resistors have been patterned in (100) epitaxial silicon material that was grown on Bonded and Etched-Back Silicon-on-Insulator (BESOI) substrates. The CDs (Critical Dimensions) of a selection of their reference segments have been measured electrically, by SEM (Scanning-Electron Microscopy) cross-section imaging, and by lattice-plane counting. The lattice-plane counting is performed on phase-contrast images made by High-Resolution Transmission-Electron Microscopy (HRTEM). The reference-segment features were aligned with <110> directions in the BESOI surface material. They were defined by a silicon micromachining process which results in their sidewalls being atomically-planar and smooth and inclined at 54.737{degree} to the surface (100) plane of the substrate. This (100) implementation may usefully complement the attributes of the previously-reported vertical-sidewall one for selected reference-material applications. The SEM, HRTEM, and electrical CD (ECD) linewidth measurements that are made on BESOI features of various drawn dimensions on the same substrate is being investigated to determine the feasibility of a CD traceability path that combines the low cost, robustness, and repeatability of the ECD technique and the absolute measurement of the HRTEM lattice-plane counting technique. Other novel aspects of the (100) SOI implementation that are reported here are the ECD test-structure architecture and the making of HRTEM lattice-plane counts from both cross-sectional, as well as top-down, imaging of the reference features. This paper describes the design details and the fabrication of the cross-bridge resistor test structure. The long-term goal is to develop a technique for the determination of the absolute dimensions of the trapezoidal cross-sections of the cross-bridge resistors reference segments, as a prelude to making them available for dimensional reference applications.

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21 Results
21 Results