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DOE OSTI2023

Investigation of Theoretical Solutions to a Bottom-Raised Oscillating Surge Wave Energy Converter (OSWEC) Through Experimental and Parametric Studies

Experiments were conducted on a wave tank model of a bottom raised oscillating surge wave energy converter (OSWEC) model in regular waves. The OSWEC model shape was a thin rectangular flap, which was allowed to pitch in response to incident waves about a hinge located at the intersection of the flap and the top of the supporting foundation. Torsion springs were added to the hinge in order to position the pitch natural frequency at the center of the wave frequency range of the wave maker. The flap motion as well as the loads at the base of the foundation were measured. The OSWEC was modeled analytically using elliptic functions in order to obtain closed form expressions for added mass and radiation damping coefficients, along with the excitation force and torque. These formulations were derived and reported in a previous publication by the authors. While analytical predictions of the foundation loads agree very well with experiments, large discrepancies are seen in the pitch response close to resonance. These differences are analyzed by conducting a sensitivity study, in which system parameters, including damping and added mass values, are varied. The likely contributors to the differences between predictions and experiments are attributed to tank reflections, standing waves that can occur in long, narrow wave tanks, as well as the thin plate assumption employed in the analytical approach.

analytical↗

DOE OSTI2014

Correlation between the structural and cathodoluminescence properties in InGaN/GaN multiple quantum wells with large number of quantum wells

Cathodoluminescence (CL) characteristics on 30-period InGaN/GaN multiple quantum well (MQW) solar cell structures are investigated, revealing the relationship between optical and structural properties of the MQW structures with a large number of quantum wells. In the bottom MQW layers, a blueshift of CL peak along the growth direction is found and attributed to the decrease of indium content due to the compositional pulling effect. An obvious split of emission peak and a redshift of the main emission energy are found in the top MQW layers when the MQW grows above the critical layer thickness. They are attributed to the segregation of In-rich InGaN clusters rather than the increase of indium content in quantum well layer. The MQW structure is identified to consist of two regions: a strained one in the bottom, where the indium content is gradually decreased, and a partly relaxed one in the top with segregated In-rich InGaN clusters.

36 MATERIALS SCIENCE↗

DOE OSTI2015

TiO{sub 2} nanotube arrays for photocatalysis: Effects of crystallinity, local order, and electronic structure

To furnish insight into correlations of electronic and local structure and photoactivity, arrays of short and long TiO{sub 2} nanotubes were synthesized by electrochemical anodization of Ti foil, followed by thermal treatment in O{sub 2} (oxidizing), Ar (inert), and H{sub 2} (reducing) environments. The physical and electronic structures of these nanotubes were probed with x-ray diffraction, scanning electron microscopy, and synchrotron-based x-ray absorption spectroscopy, and correlated with their photocatalytic properties. The photocatalytic activity of the nanotubes was evaluated by monitoring the degradation of methyl orange under UV-VIS light irradiation. Results show that upon annealing at 350 °C all as-anodized amorphous TiO{sub 2} nanotube samples partially transform to the anatase structure, with variations in the degree of crystallinity and in the concentration of local defects near the nanotubes' surface (∼5 nm) depending on the annealing conditions. Degradation of methyl orange was not detectable for the as-anodized TiO{sub 2} nanotubes regardless of their length. However, the annealed long nanotubes demonstrated detectable catalytic activity, which was more significant with the H{sub 2}-annealed nanotubes than with the Ar- and O{sub 2}-annealed nanotube samples. This enhanced photocatalytic response of the H{sub 2}-annealed long nanotubes relative to the other samples is positively correlated with the presence of a larger concentration of lattice defects (such as Ti{sup 3+} and anticipated oxygen vacancies) and a slightly lower degree of crystallinity near the nanotube surface. These physical and electronic structural attributes impact the efficacy of visible light absorption; moreover, the increased concentration of surface defects is postulated to promote the generation of hydroxyl radicals and thus accelerate the photodegradation of the methyl orange. The information obtained from this study provides unique insight into the role of the near-surface electronic and defect structure, crystal structure, and the local chemical environment on the photocatalytic activity and may be employed for tailoring the materials' properties for photocatalysis and other energy-related applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Hydrogen desorption from hydrogen fluoride and remote hydrogen plasma cleaned silicon carbide (0001) surfaces

Due to the extreme chemical inertness of silicon carbide (SiC), in-situ thermal desorption is commonly utilized as a means to remove surface contamination prior to initiating critical semiconductor processing steps such as epitaxy, gate dielectric formation, and contact metallization. In-situ thermal desorption and silicon sublimation has also recently become a popular method for epitaxial growth of mono and few layer graphene. Accordingly, numerous thermal desorption experiments of various processed silicon carbide surfaces have been performed, but have ignored the presence of hydrogen, which is ubiquitous throughout semiconductor processing. In this regard, the authors have performed a combined temperature programmed desorption (TPD) and x-ray photoelectron spectroscopy (XPS) investigation of the desorption of molecular hydrogen (H{sub 2}) and various other oxygen, carbon, and fluorine related species from ex-situ aqueous hydrogen fluoride (HF) and in-situ remote hydrogen plasma cleaned 6H-SiC (0001) surfaces. Using XPS, the authors observed that temperatures on the order of 700–1000 °C are needed to fully desorb C-H, C-O and Si-O species from these surfaces. However, using TPD, the authors observed H{sub 2} desorption at both lower temperatures (200–550 °C) as well as higher temperatures (>700 °C). The low temperature H{sub 2} desorption was deconvoluted into multiple desorption states that, based on similarities to H{sub 2} desorption from Si (111), were attributed to silicon mono, di, and trihydride surface species as well as hydrogen trapped by subsurface defects, steps, or dopants. The higher temperature H{sub 2} desorption was similarly attributed to H{sub 2} evolved from surface O-H groups at ∼750 °C as well as the liberation of H{sub 2} during Si-O desorption at temperatures >800 °C. These results indicate that while ex-situ aqueous HF processed 6H-SiC (0001) surfaces annealed at <700 °C remain terminated by some surface C–O and Si–O bonding, they may still exhibit significant chemical reactivity due to the creation of surface dangling bonds resulting from H{sub 2} desorption from previously undetected silicon hydride and surface hydroxide species.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Hydrogen desorption kinetics for aqueous hydrogen fluoride and remote hydrogen plasma processed silicon (001) surfaces

The desorption kinetics of molecular hydrogen (H{sub 2}) from silicon (001) surfaces exposed to aqueous hydrogen fluoride and remote hydrogen plasmas were examined using temperature programmed desorption. Multiple H{sub 2} desorption states were observed and attributed to surface monohydride (SiH), di/trihydride (SiH{sub 2/3}), and hydroxide (SiOH) species, subsurface hydrogen trapped at defects, and hydrogen evolved during the desorption of surface oxides. The observed surface hydride species were dependent on the surface temperature during hydrogen plasma exposure with mono, di, and trihydride species being observed after low temperature exposure (150 °C), while predominantly monohydride species were observed after higher temperature exposure (450 °C). The ratio of surface versus subsurface H{sub 2} desorption was also found to be dependent on the substrate temperature with 150 °C remote hydrogen plasma exposure generally leading to more H{sub 2} evolved from subsurface states and 450 °C exposure leading to more H{sub 2} desorption from surface SiH{sub x} species. Additional surface desorption states were observed, which were attributed to H{sub 2} desorption from Si (111) facets formed as a result of surface etching by the remote hydrogen plasma or aqueous hydrogen fluoride treatment. The kinetics of surface H{sub 2} desorption were found to be in excellent agreement with prior investigations of silicon surfaces exposed to thermally generated atomic hydrogen.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Zero added oxygen for high quality sputtered ITO: A data science investigation of reduced Sn-content and added Zr

The authors demonstrate mobilities of >45 cm{sup 2}/V s for sputtered tin-doped indium oxide (ITO) films at zero added oxygen. All films were deposited with 5 wt. % SnO{sub 2}, instead of the more conventional 8–10 wt. %, and had varying ZrO{sub 2} content from 0 to 3 wt. %, with a subsequent reduction in In{sub 2}O{sub 3} content. These films were deposited by radio-frequency magnetron sputtering from nominally stoichiometric targets with varying oxygen partial pressure in the sputter ambient. Anomalous behavior was discovered for films with no Zr-added, where a bimodality of high and low mobilities was discovered for nominally similar growth conditions. However, all films showed the lowest resistivity and highest mobilities when the oxygen partial pressure in the sputter ambient was zero. This result is contrasted with several other reports of ITO transport performance having a maximum for small but nonzero oxygen partial pressure. This result is attributed to the reduced concentration of SnO{sub 2}. The addition of ZrO{sub 2} yielded the highest mobilities at >55 cm{sup 2}/V s and the films showed a modest increase in optical transmission with increasing Zr-content.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Formation of homologous In{sub 2}O{sub 3}(ZnO){sub m} thin films and its thermoelectric properties

Homologous In{sub 2}O{sub 3}(ZnO){sub 5} thin films were produced on a synthetic quartz glass substrate by thermal annealing of magnetron sputtered In{sub 2}O{sub 3}-ZnO compound films. When the annealing temperature was increased to 700 °C, the sputtered In{sub 2}O{sub 3}-ZnO film with In{sub 2}O{sub 3} microcrystalline changed to a c-oriented homologous In{sub 2}O{sub 3}(ZnO){sub 5} structure, for which the crystallization is suggested to begin from the surface and proceed along with the film thickness. The annealing temperature of 700 °C to form the In{sub 2}O{sub 3}(ZnO){sub 5} structure was substantially lower than temperatures of conventional solid state synthesis from In{sub 2}O{sub 3} and ZnO powders, which is attributed to the rapid diffusional transport of In and Zn due to the mixing of In{sub 2}O{sub 3} and ZnO in the atomic level for sputtered In{sub 2}O{sub 3}-ZnO compound films. The homologous structure collapsed at temperatures above 900 °C, which is attributed to (1) zinc vaporization from the surface and (2) a gradual increase of zinc silicate phase at the interface. This c-oriented layer structure of homologous In{sub 2}O{sub 3}(ZnO){sub 5} thin films along the film thickness allowed the thin film to reach a power factor of 1.3 × 10{sup −4} W/m K{sup 2} at 670 °C, which is comparable with the reported maximum value for the textured In{sub 2}O{sub 3}(ZnO){sub 5} powder (about 1.6 × 10{sup −4} W/m K{sup 2} at 650 °C).

36 MATERIALS SCIENCE↗

DOE OSTI2018

Assessing the manufacturing tolerances and uniformity of CMOS compatible metamaterial fabrication

The manufacturing tolerances of a stencil-lithography variant, membrane projection lithography, were investigated. In the first part of this work, electron beam lithography was used to create stencils with a range of linewidths. These patterns were transferred into the stencil membrane and used to pattern metallic lines on vertical silicon faces. Only the largest lines, with a nominal width of 84 nm, were resolved, resulting in 45 ± 10 nm (average ± standard deviation) as deposited with 135-nm spacing. Although written in the e-beam write software file as 84-nm in width, the lines exhibited linewidth bias. This can largely be attributed to nonvertical sidewalls inherent to dry etching techniques that cause proportionally larger impact with decreasing feature size. The line edge roughness can be significantly attributed to the grain structure of the aluminum nitride stencil membrane. In the second part of this work, the spatial uniformity of optically defined (as opposed to e-beam written) metamaterial structures over large areas was assessed. A Fourier transform infrared spectrometer microscope was used to collect the reflection spectra of samples with optically defined vertical split ring from 25 spatially resolved 300 × 300 μm regions in a 1-cm2 area. The technique is shown to provide a qualitative measure of the uniformity of the inclusions.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Analysis of perceived similarity between pairs of microcalcification clusters in mammograms

Purpose: Content-based image retrieval aims to assist radiologists by presenting example images with known pathology that are visually similar to the case being evaluated. In this work, the authors investigate several fundamental issues underlying the similarity ratings between pairs of microcalcification (MC) lesions on mammograms as judged by radiologists: the degree of variability in the similarity ratings, the impact of this variability on agreement between readers in retrieval of similar lesions, and the factors contributing to the readers’ similarity ratings. Methods: The authors conduct a reader study on a set of 1000 image pairs of MC lesions, in which a group of experienced breast radiologists rated the degree of similarity between each image pair. The image pairs are selected, from among possible pairings of 222 cases (110 malignant, 112 benign), based on quantitative image attributes (features) and the results of a preliminary reader study. Next, the authors apply analysis of variance (ANOVA) to quantify the level of variability in the readers’ similarity ratings, and study how the variability in individual reader ratings affects consistency between readers. The authors also measure the extent to which readers agree on images which are most similar to a given query, for which the Dice coefficient is used. To investigate how the similarity ratings potentially relate to the attributes underlying the cases, the authors study the fraction of perceptually similar images that also share the same benign or malignant pathology as the query image; moreover, the authors apply multidimensional scaling (MDS) to embed the cases according to their mutual perceptual similarity in a two-dimensional plot, which allows the authors to examine the manner in which similar lesions relate to one another in terms of benign or malignant pathology and clustered MCs. Results: The ANOVA results show that the coefficient of determination in the reader similarity ratings is 0.59. The variability level in the similarity ratings is proved to be a limiting factor, leading to only moderate correlation between the readers in their readings. The Dice coefficient, measuring agreement between readers in retrieval of similar images, can vary from 0.45 to 0.64 with different levels of similarity for individual readers, but is higher for average ratings from a group of readers (from 0.59 to 0.78). More importantly, the fraction of retrieved cases that match the benign or malignant pathology of the query image was found to increase with the degree of similarity among the retrieved images, reaching average value as high as 0.69 for the radiologists (p-value <10{sup −4} compared to random guessing). Moreover, MDS embedding of all the cases shows that cases having the same pathology tend to cluster together, and that neighboring cases in the plot tend to be similar in their clustered MCs. Conclusions: While individual readers exhibit substantial variability in their similarity ratings, similarity ratings averaged from a group of readers can achieve a high level of intergroup consistency and agreement in retrieval of similar images. More importantly, perceptually similar cases are also likely to be similar in their underlying benign or malignant pathology and image features of clustered MCs, which could be of diagnostic value in computer-aided diagnosis for lesions with clustered MCs.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

DOE OSTI2015

Determinants of the reliability of ultrasound tomography sound speed estimates as a surrogate for volumetric breast density

Purpose: High breast density, as measured by mammography, is associated with increased breast cancer risk, but standard methods of assessment have limitations including 2D representation of breast tissue, distortion due to breast compression, and use of ionizing radiation. Ultrasound tomography (UST) is a novel imaging method that averts these limitations and uses sound speed measures rather than x-ray imaging to estimate breast density. The authors evaluated the reproducibility of measures of speed of sound and changes in this parameter using UST. Methods: One experienced and five newly trained raters measured sound speed in serial UST scans for 22 women (two scans per person) to assess inter-rater reliability. Intrarater reliability was assessed for four raters. A random effects model was used to calculate the percent variation in sound speed and change in sound speed attributable to subject, scan, rater, and repeat reads. The authors estimated the intraclass correlation coefficients (ICCs) for these measures based on data from the authors’ experienced rater. Results: Median (range) time between baseline and follow-up UST scans was five (1–13) months. Contributions of factors to sound speed variance were differences between subjects (86.0%), baseline versus follow-up scans (7.5%), inter-rater evaluations (1.1%), and intrarater reproducibility (∼0%). When evaluating change in sound speed between scans, 2.7% and ∼0% of variation were attributed to inter- and intrarater variation, respectively. For the experienced rater’s repeat reads, agreement for sound speed was excellent (ICC = 93.4%) and for change in sound speed substantial (ICC = 70.4%), indicating very good reproducibility of these measures. Conclusions: UST provided highly reproducible sound speed measurements, which reflect breast density, suggesting that UST has utility in sensitively assessing change in density.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2016

SU-F-T-299: An Experimental 2D Computed Radiography (CR) Dosimeter for IMRT. Are In-Field Measurements Affected by the Low Energy Photon Overresponse?

Purpose: Computed Radiography (CR) dosimetry could offer film dosimetry resolution and flexibility but with reusability and instantaneous processing. For an experimental CR-plate, designed for radiotherapy (Zeff=18), CR’s typical out-of-field over-response to low energy photons was previously reduced to 8%. The present work assesses the impact of the residual over-response when open-fields are combined or when intensity modulated fields are used. Methods: Agfa Healthcare’s experimental CRplate was scanned and erased 4min after each irradiation using a flying-spot CR-15-X-engine based reader, which was adapted for radiotherapy dosimetry. A CR-plate specific calibration and uniformity correction was used.For open-fields two abutting half beams (5×10cm{sup 2}) captured out-offield and in-field doses in a single image. Additionally, both half beams were measured individually as well as a 3×18Gy open-field SBRT-lung treatment. For intensity modulated fields standard test patterns (Chair and Pyramid) and a clinical 5×5Gy rectal VMAT plan were captured. All measurements were compared to the corresponding dose calculations. Results: For open-fields the out-of-field overdose was clearly larger than the in-field overdose (10% vs. 4%). The sum of the individual measurements corresponded well with the combined measurement (dose difference, ΔD<−2.2%). The SBRT case had no overdose in the high dose region; ΔD=−5.6%±3.3%, the deviation was attributed to CR-fading effects (−0.3%/min) which were not corrected for.Compared to open-fields, intensity modulated deliveries had a further increased over-response out-offield (ΔD=+58% to +125% [Chair] +43% [Pyramid]), due to the increased amount of low energy photons for IMRT. However, this effect was not measured in-field where even decreased dose signals were observed (ΔD=−0.3% to +2.25% [Chair], −4.5% to −0.1% [Pyramid]). The rectal VMAT treatment had a dose difference +2.4%±6.0%. The in-field deviations were attributed to a residual non-uniformity. Conclusion: The experimental CRplate’s out-of-field over-response does not propagate in in-field overresponse errors when static or dynamic (IMRT/VMAT) abutting fields are used.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2016

SU-G-TeP3-15: Radiation Dose Enhancement by Anatase TiO2NPs

Purpose: This work investigates radiation dose enhancement caused by TiO2 nanoparticles covering entire X-ray energy ranges used in radiation therapy. Methods: Anatase TiO2NPs crystal were synthesised and modified as hydrophilic and hydrophobic to disperse in culture-medium and halocarbons (PRESAGE chemical composition) respectively. TiO2NPs were characterised using TEM, XPS, XRD, TGA and FTIR. Various Concentrations have been utilised for determination of radiation-dose enhancement. This investigation is carried out in two ways; one using PRESAGE dosimeter/phantom and the other is radiobiological and based on in vitro study using two types of cell lines, Human Keratinocyte (HaCaT) and prostate cancer cell lines. The x-ray used are both kilovoltage and megavoltage separately. The prepared PRESAGE dosimeters were scanned using optical CT scanner. Clonogenic and MTS assays were employed for cell cytotoxicity and viability measurements for determination of the levels of dose enhancement. Results: Significant about (50%, 45%) dose enhancement by TiO2-NPs for kV x-rays is measured in both ways (Presage and Cells study). Slightly more is detected with the cells. However, the dose enhancement with megavoltage beams was insignificant using Presage and under same conditions the cells survival curves indicates around 20% which is relatively high. This difference can only be attributed to some biochemical effects. Such as generation of reactive oxygen species (ROS), this can affect the cells while it can’t be detected by Presage. Elevation of hydroxyl radicals (•OH) of many orders is observed with the inclusion of TiO2-NPs in cells-medium. Conclusion: Dose enhancement inflicted by TiO2-NPs is proven to be significant with megavoltage beams and minimal with kV. The high dose enhancements obtained can be attributed to higher levels of ROS generated. Since MV beams are most commonly used, this research proves potential value for more efficient beam delivery. This has potential to be applied in future clinical radiotherapy applications The research is supported and funded by RMIT university-Melbourne/Australia.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2024

Hybrid magnon-phonon localization enhances function near ferroic glassy states

Ferroic materials on the verge of forming ferroic glasses exhibit heightened functionality that is often attributed to competing long- and short-range correlations. However, the physics underlying these enhancements is not well understood. The Ni 45 Co 5 Mn 36.6 In 13.4 Heusler alloy is on the edge of forming both spin and strain glasses and exhibits magnetic field–induced shape memory and large magnetocaloric effects, making it a candidate for multicaloric cooling applications. We show using neutron scattering that localized magnon-phonon hybrid modes, which are inherently spread across reciprocal space, act as a bridge between phonons and magnons and result in substantial magnetic field–induced shifts in the phonons, triple the caloric response, and alter phase stability. We attribute these modes to the localization of phonons and magnons by antiphase boundaries coupled to magnetic domains. Because the interplay between short- and long-range correlations is common near ferroic glassy states, our work provides general insights on how glassiness enhances function.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Ab initio investigation of a hypersonic double cone experiment

This article presents a direct molecular simulation (DMS) of a reactive Mach 8.2 oxygen flow over a double cone geometry. The free stream conditions and article configuration generate a flow with thermal and chemical nonequilibrium, which are common attributes of hypersonic flight. This scenario was first studied experimentally at Calspan University of Buffalo Research Center’s test facility. DMS is a particle method that uses quantum mechanically derived interaction potentials to simulate molecular collisions within a flow field. Since these interaction potentials are the only modeling inputs used in the simulation, all flow features can solely be attributed to the ab initio potential energy surfaces. Hence, providing a comparison of a hypersonic ground test and numerical data anchored to quantum mechanics. The fundamental nature of DMS is leveraged to investigate molecular level mechanisms prevalent in the flow, and comparisons with lower fidelity simulations are presented to highlight the role of these first principles calculations as benchmark solutions.