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At least 811 records · Page 45

Mitigating e-beam-induced hydrocarbon deposition on graphene for atomic-scale scanning transmission electron microscopy studies

Chemical vapor deposition (CVD) grown graphene used in (scanning) transmission electron microscopy [(S)TEM] studies must undergo a careful transfer of the one-atom-thick membrane from the growth surface (typically a Cu foil) to the TEM grid. During this transfer process, the graphene invariably becomes contaminated with foreign materials. This contamination proves to be very problematic in the (S)TEM because often >95% of the graphene is obscured, and imaging of the pristine areas results in e-beam-induced hydrocarbon deposition which further acts to obscure the desired imaging area. In this article, the authors examine two cleaning techniques for CVD grown graphene that mitigate both aspects of the contamination problem: visible contamination covering the graphene, and “invisible” contamination that deposits onto the graphene under e-beam irradiation. Furthermore, the visible contamination may be removed quickly by a rapid thermal annealing to 1200 °C in situ and the invisible e-beam-deposited contamination may be removed through an Ar/O 2 annealing procedure prior to imaging in the (S)TEM.

36 MATERIALS SCIENCE↗

Status Report on Design of In-situ Thermomechanical Testing at LANSCE

Nuclear fuel encounters severe thermomechanical environments in which its mechanical response is determined by its microstructure, temperature and stress level histories. Simulating the response of such microstructures is crucial for predicting both performance and transient fuel mechanical responses and experimental verification of such predictions is therefore of great interest. While most of the deformation in a nuclear fuel rod occurs in the cladding, deformation of the fuel itself is still of interest with deformation mechanisms at operating temperature and above including creep, swelling, cracking as well as pellet-clad interaction. Characterization of these properties and understanding of the underlying deformation phenomena at operating or excursion temperatures is therefore of great importance for development and ultimately licensing of improved and novel nuclear fuel forms. Diffraction techniques offer unique insight on the atomistic (e.g. crystal structure) and microstructure (e.g. phase transformations, texture, defects) length scales and have a long history of providing unique data to inform relevant deformation models that enable the required predictive capabilities. For example, dislocations lead to diffraction peak broadening that can be characterized to estimate the dislocation density and study the role of dislocations on the deformation while measuring lattice strains allows to studie load sharing in two phase materials. In this report the requirements for a sample environment for high temperature deformation of nuclear fuels are defined. The HIPPO neutron time-of-flight diffractometer at LANSCE will host this sample environment and is also described. This instrument covers diffraction angles from 140° to 40° and is also equipped with an event-mode neutron imaging detector system, enabling energy-resolved neutron imaging in parallel with the diffraction that could measure sample temperature from Doppler broadening of neutron absorption resonances or measure pore densities from changes in the attenuation. Designs of devices to characterize thermomechanical properties of nuclear fuel without diffraction are also considered to guide the design. While this report is focused on applications for nuclear fuels, the device can also characterize cladding, moderator or structural materials and therefore contribute to other fields of research and development for advanced reactors. The temperatures planned to be reached are above 2000℃, thus enabling characterization of LWR reactor fuels under accident scenarios but also reaching temperatures of fuels developed for nuclear thermal propulsion and providing opportunities to characterize those. In conjunction with the energy-resolved neutron imaging detector, this setup would allow to measure neutron cross-sections at high temperatures, filling a gap towards development of reactors operating at high temperatures.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Methods and apparatuses for self-generating fault-tolerant keys in spread-spectrum systems

Self-generating fault-tolerant keys for use in spread-spectrum systems are disclosed. At a communication device, beacon signals are received from another communication device and impulse responses are determined from the beacon signals. The impulse responses are circularly shifted to place a largest sample at a predefined position. The impulse responses are converted to a set of frequency responses in a frequency domain. The frequency responses are shuffled with a predetermined shuffle scheme to develop a set of shuffled frequency responses. A set of phase differences is determined as a difference between an angle of the frequency response and an angle of the shuffled frequency response at each element of the corresponding sets. Each phase difference is quantized to develop a set of secret-key quantized phases and a set of spreading codes is developed wherein each spreading code includes a corresponding phase of the set of secret-key quantized phases.

42 ENGINEERING↗

Multiscale spectral nanoscopy

A system and method for non-invasively tracking a particle in a sample is disclosed. The system includes a 2-photon or confocal laser scanning microscope (LSM) and a particle-holding device coupled to a stage with X-Y and Z position control. The system also includes a tracking module having a tracking excitation laser, X-Y and Z radiation-gathering components configured to detect deviations of the particle in an X-Y and Z directions. The system also includes a processor coupled to the X-Y and Z radiation gathering components, generate control signals configured to drive the stage X-Y and Z position controls to track the movement of the particle. The system may also include a synchronization module configured to generate LSM pixels stamped with stage position and a processing module configured to generate a 3D image showing the 3D trajectory of a particle using the LSM pixels stamped with stage position.

42 ENGINEERING↗

Barkhausen noise as an intrinsic fingerprint for ferromagnetic components

Here in this work, the suitability of magnetic Barkhausen noise as an intrinsic fingerprint of ferromagnetic components is determined. This technique has potential for this application because it is based inherently on the near surface microstructural features of ferromagnetic materials. All materials typically display some variation in their microstructure simply as a result of the manufacturing process (rolling, heat treating, welding, grinding), thus providing the potential that Barkhausen noise measurements between nominally similar components will be unique. In this work, we demonstrate that Barkhausen noise measurements are both repeatable in time for a single sample made from a ferromagnetic material, and unique across a number of instances of nominally similar samples. The results of this work have profound implications in a variety of applications in forensics and physical security. For example, consider the fabrication of the next generation of tamper-evident containers and devices using conventional processes for steel. In addition, since Barkhausen noise is sensitive to changes in microstructures due to grinding and welding, these measurements can be used to detect clandestine repairs and tampering. Finally, because the method inherently results in a time series measurement at each point on a sample, it is expected to have far higher dimensionality than physically similar eddy current measurement. However, the higher dimensionality of Barkhausen measurements suggest that they should be harder to counterfeit than eddy current measurements.

36 MATERIALS SCIENCE↗

Microwave heating device for internal heating convection experiments, applied to Earth's mantle dynamics

We report the design, construction, and performances of a microwave (MW) heating device for laboratory experiments with non-contact, homogeneous internal heating. The device generates MW radiation at 2.47 GHz from a commercial magnetron supplied by a pulsed current inverter using proprietary, feedback based command and control hardware and software. Specially designed MW launchers direct the MW radiation into the sample through a MW homogenizer, devised to even the MW power distribution into the sample's volume. An adjustable MW circuit adapts the MW generator to the load (i.e., the sample) placed in the experiment chamber. Dedicated heatsinks maintain the MW circuits at constant temperature throughout the experiment. Openings for laser scanning for image acquisition with a CCD camera and for the cooling circuits are protected by special MW filters. The performances of the device are analyzed in terms of heating uniformity, long term output power stability, and load matching. The device is used for small scale experiments simulating Earth's mantle convection. The 30 × 30 × 5 cm{sup 3} convection tank is filled with a water‑based viscous fluid. A uniform and constant temperature is maintained at the upper boundary by an aluminum heat exchanger and adiabatic conditions apply at the tank base. We characterize the geometry of the convective regime as well as its bulk thermal evolution by measuring the velocity field by Particle Image Velocimetry and the temperature field by using Thermochromic Liquid Crystals.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Initial experimental demonstration of the principles of a xenon gas shield designed to protect optical components from soft x-ray induced opacity (blanking) in high energy density experiments

The design principles of a xenon gas shield device that is intended to protect optical components from x-ray induced opacity (“x-ray blanking”) have been experimentally demonstrated at the OMEGA-60 Laser Facility at the Laboratory for Laser Energetics, University of Rochester. A volume of xenon gas placed in front of an optical component absorbs the incoming soft x-ray radiation but transmits optical and ultra-violet radiation. The time-resolved optical (532 nm) transmission of samples was recorded as they were exposed to soft x-rays produced by a gold sphere source (1.5 kJ sr $-$1 , 250–300 eV). Blanking of fused silica (SiO 2 ) was measured to occur over a range of time-integrated soft x-ray (<3 keV) fluence from ~0.2–2.5 J cm $-$2 . A shield test device consisting of a 30 nm silicon nitride (Si 3 N 4 ) and a 10 cm long volume of 0.04 bar xenon gas succeeded in delaying loss of transmission through a magnesium fluoride sample; optical transmission was observed over a longer period than for the unprotected sample. It is hoped that the design of this x-ray shield can be scaled in order to produce a shield device for the National Ignition Facility optical Thomson scattering collection telescope, in order to allow measurements of hohlraum plasma conditions produced in inertial confinement fusion experiments. Finally, if successful, it will also have applications in many other high energy density experiments where optical and ultra-violet measurements are desirable.

42 ENGINEERING↗

Measurement of laser absorption in underdense plasmas using near-field imaging of the incident and transmitted beams

Measurements of laser absorption in high-temperature, underdense plasmas produced at the Omega Laser Facility are made using two near-field imaging detectors that diagnose the spatial profile and energy of the port P9 beam before and after it transmits through the plasma. The incident beam is sampled using a partial reflection from a full-aperture, (30 cm-diam) uncoated wedge pickoff located before the target chamber vacuum window and final focus lens assembly. A concave mirror reduces the reflected beam size, allowing it to be recorded directly using a charged-coupled device (CCD) camera. The P9 transmitted beam diagnostic (P9TBD) characterizes the transmitted light by terminating the expanded beam on a semi-transparent diffuser and imaging the illuminated surface using a lens and CCD camera. The P9TBD samples a numerical aperture twice as large as the input beam, allowing the energy of transmitted beams with moderate levels of beam spray to be measured accurately. Calibration shots with no plasma provide a path to infer absorption without absolute photometric calibration of either detector. Lastly, the cross-calibration between the two detectors was measured to remain stable at ±200 ppm, enabling measurements of total beam absorption below 1% with ±0.07% error.

47 OTHER INSTRUMENTATION↗

Graphene metamaterial modulator for free-space thermal radiation

We proposed and demonstrated a new metamaterial architecture capable of high speed modulation of free-space space thermal infrared radiation using graphene. Our design completely eliminates channel resistance, thereby maximizing the electrostatic modulation speed, while at the same time effectively modulating infrared radiation. Experiment results verify that our device with area of 100 × 120 µm 2 can achieve a modulation speed as high as 2.6 GHz. We further highlight the utility of our graphene metamaterial modulator by reconstructing a fast infrared signal using an equivalent time sampling technique. The graphene metamaterial modulator demonstrated here is not only limited to the thermal infrared, but may be scaled to longer infrared and terahertz wavelengths. Our work provides a path forward for realization of frequency selective and all-electronic high speed devices for infrared applications.

36 MATERIALS SCIENCE↗

Nanoporous gold: a hierarchical and multiscale 3D test pattern for characterizing X-ray nano-tomography systems

Full-field transmission X-ray microscopy (TXM) is a well established technique, available at various synchrotron beamlines around the world as well as by laboratory benchtop devices. One of the major TXM challenges, due to its nanometre-scale resolution, is the overall instrument stability during the acquisition of the series of tomographic projections. The ability to correct for vertical and horizontal distortions of each projection image during acquisition is necessary in order to achieve the effective 3D spatial resolution. The effectiveness of such an image alignment is also heavily influenced by the absorption properties and strong contrast of specific features in the scanned sample. Here it is shown that nanoporous gold (NPG) can be used as an ideal 3D test pattern for evaluating and optimizing the performance of a TXM instrument for hard X-rays at a synchrotron beamline. Unique features of NPG, such as hierarchical structures at multiple length scales and high absorbing capabilities, makes it an ideal choice for characterization, which involves a combination of a rapid-alignment algorithm applied on the acquired projections followed by the extraction of a set of both 2D- and 3D-descriptive image parameters. This protocol can be used for comparing the efficiency of TXM instruments at different synchrotron beamlines in the world or benchtop devices, based on a reference library of scanned NPG samples, containing information about the estimated horizontal and vertical alignment values, 2D qualitative parameters and quantitative 3D parameters. The possibility to tailor the ligament sizes of NPG to match the achievable resolution in combination with the high electron density of gold makes NPG an ideal 3D test pattern for evaluating the status and performance of a given synchrotron-based or benchtop-based TXM setup.

36 MATERIALS SCIENCE↗

High-pressure, high-temperature magic angle spinning nuclear magnetic resonance devices and processes for making and using same

Re-usable ceramic magic angle spinning (MAS) NMR rotors constructed of high-mechanic strength ceramics are detailed that include a sample compartment that maintains high pressures up to at least about 200 atmospheres (atm) and high temperatures up to about least about 300.degree. C. during operation. The rotor designs minimize pressure losses stemming from penetration over an extended period of time. The present invention makes possible a variety of in-situ high pressure, high temperature MAS NMR experiments not previously achieved in the prior art.

42 ENGINEERING↗

Use of Electronic Hand-held Devices for Collection of Savannah River Site Environmental Data - 13329

Savannah River Nuclear Solutions has begun using Xplore Tablet PC's to collect data in the field for soil samples, groundwater samples, air samples and round sheets at the Savannah River Site (SRS). EPA guidelines for groundwater sampling are incorporated into the application to ensure the sample technician follows the proper protocol. The sample technician is guided through the process for sampling and round sheet data collection by a series of menus and input boxes. Field measurements and well stabilization information are entered into the tablet for uploading into Environmental Restoration Data Management System (ERDMS). The process helps to eliminate input errors and provides data integrity. A soil sample technician has the ability to collect information about location of sample, field parameter, describe the soil sample, print bottle labels, and print chain of custody for the sample that they have collected. An air sample technician has the ability to provide flow, pressure, hours of operation, print bottle labels and chain of custody for samples they collect. Round sheets are collected using the information provided in the various procedures. The data are collected and uploaded into ERDMS. The equipment used is weather proof and hardened for the field use. Global Positioning System (GPS) capabilities are integrated into the applications to provide the location where samples were collected and to help sample technicians locate wells that are not visited often. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

In-situ Microscopy Characterization of Cu(In,Ga)Se2 Potential-Induced Degradation

We report on the role of sodium in potentialinduced degradation (PID) of Cu(In, Ga)Se 2 (CIGS) solar cells. In-situ microscopy characterizations on AFM platform were performed on two stressed CIGS device under room temperature (RT) and high temperature (HT) at 85 degrees C. During PID stressing we observed depletion region gets wider as Na migrates, p-n junction becomes leaky at RT for over a month; and similar junction evolution was observed for HT-stressed sample, eventually the junction collapsed after 18 hours. The diode behaviors were confirmed by dark I-V measurement. Time-of Flight secondary-ion mass spectrometry reveals that the Na accumulates on ZnO and CdS side, as well as the upper layer of CIGS layer. The results indicate that Na drifted by the voltage applied on the soda-lime glass, then diffuse through the whole device. And the sodium profiles have different points of evolution due to the temperature differences between the two stressed samples. The consistent results unambiguously show how Na from substrate glass causes PID in CIGS solar cells.

14 SOLAR ENERGY↗

Lead exposure to children from consumption of backyard chicken eggs

Highlights: • Backyard chicken eggs from most households providing egg samples (98%) contained detectable concentrations of lead. • IIn prediction models, backyard egg consumption increased overall blood lead levels in children • Infants < 1 year of age experience the greatest increase in predicted blood lead levels from backyard egg consumption. • Mean household egg lead concentration was strongly positively correlated with coop soil lead concentrations. Backyard chicken ownership is rapidly increasing in urban areas in the United States, largely as a way to provide eggs for household consumption. Despite elevated levels of environmental lead contamination in many US cities, the role of backyard chicken eggs as a pathway for lead exposure, particularly for children, has received limited scrutiny. To characterize lead exposure from consumption of backyard chicken eggs for children and predict related effects on blood lead level (BLL), we conducted a cross-sectional study of backyard chicken owners in the Greater Boston area (n = 51). We interviewed participants regarding egg consumption by household members and collected backyard eggs (n = 201) and coop soil samples (n = 48) for analysis. Inductively coupled plasma mass spectrometry (ICP-MS) was used to evaluate lead concentration in homogenized eggs and an X-ray fluorescence (XRF) portable device was used to assess soil lead levels in the laboratory. We used the USEPA's Integrated Exposure Uptake Biokinetic Model for Lead in Children (IEUBK) to assess the relative contribution of backyard egg consumption to aggregate BLL in children. Four scenarios were developed in the IEUBK model to address variability in egg consumption rates and egg lead contamination. Lead was detected in egg samples from 98% of the households that provided egg samples. Mean household lead concentration was 0.10 μg/g (SD: 0.18). Egg lead concentrations ranged from below the limit of detection (0.0014 μg/g) to 1.798 μg/g (<1.4–1198 ppb). Egg lead levels were strongly positively correlated with lead concentration in coop soil (r = 0.64; p < 0.001). In modeled scenarios where a child < 7 years frequently ate eggs highly contaminated with lead, BLLs are predicted to increase by 0.9–1.5 μg/dL. In three other scenarios reflecting more moderate egg lead contamination and consumption rates, BLLs were predicted to increase from 0.1 to 0.8 μg/dL. Consumption of backyard chicken eggs can contribute to lead exposure in children. Soil lead remediation prior to chicken ownership may reduce lead exposure from backyard eggs.

54 ENVIRONMENTAL SCIENCES↗

Design and Characterization of a MEMS Probe Scanner for On-chip Atomic Force Microscopy

This paper presents the design and characterization of a microelectromechanical systems (MEMS)-based probe scanner proposed to function as an on-chip atomic force microscope (AFM). The device comprises an in-plane stage with electrostatic actuators and electrothermal displacement sensors. The stage is able to precisely position an AFM probe over a sample to perform tapping-mode AFM imaging. For implementation, a standard silicon-on-insulator (SOI) microfabrication process is used. In a previously reported design, the embedded AFM probe featured only one piezoelectric transducer for simultaneous actuation and sensing, making its use in imaging problematic. To address this issue, the new design features separate actuation and sensing AlN piezoelectric transducers. An extra electrode is also incorporated on the probe that enables canceling the electrical feedthrough from the actuation to sensing. To accommodate the extra signal routing paths, mechanical design of the probe scanner is modified. Device characterization reveals an in-plane displacement range of 8 µm×7 µm with a bandwidth of up to 2.7 kHz. The frequencydomain behavior of the AFM probe is also studied and feedthrough cancellation is performed at the resonant frequency of 127.35 kHz.

42 ENGINEERING↗

Optically activated sub-millimeter dielectric relaxation in amorphous thin film silicon at room temperature

Knowing the frequency-dependent photo-induced complex conductivity of thin films is useful in the design of photovoltaics and other semi-conductor devices. For example, annealing in the far-infrared could in principle be tailored to the specific dielectric properties of a particular sample. The frequency dependence of the conductivity (whether dark or photo-induced) also gives insight into the effective dimensionality of thin films (via the phonon density of states) as well as the presence (or absence) of free carriers, dopants, defects, etc. Ultimately, our goal is to make low-noise, phase-sensitive room temperature measurements of the frequency-dependent conductivity of thin films from microwave frequencies into the far-infrared; covering, the frequency range from ionic and dipole relaxation to atomic and electronic processes. To this end, we have developed a high-Q (quality factor) open cavity resonator capable of resolving the complex conductivity of sub-micron films in the range of 100–350 GHz (0.1–0.35 THz, or 0.4–1 meV). In this paper, we use a low-power green laser to excite bound charges in high-resistivity amorphous silicon thin film. Even at room temperature, we can resolve both the dark conductivity and photo-induced changes associated with dielectric relaxation and possibly some small portion of free carriers.

36 MATERIALS SCIENCE↗

Calculation of the Thermodynamic Voltage Limit of CdSeTe Solar Cells

The first step to understand the origin of losses in any photovoltaic solar cell is to determine the fundamental thermodynamic efficiency and voltage limits of such a device. In this contribution, we detail techniques to calculate the voltage limit in the case of cadmium selenium telluride (CdSeTe) solar cells, and how approaches based on bandgap alone—i.e., the Shockley-Queisser approach with step-function absorptance—can overestimate the thermodynamic open-circuit voltage limit Voc,ideal . This is particularly true for arsenic-doped samples, which tend to exhibit below-bandgap absorptance.

absorptance↗