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At least 523 records · Page 29

Device for residue handling minimization with vacuum-assisted separations

A device for collection of residue from separation columns. A manifold provides for multiple sample ports that are fluidly connected to a vacuum port by at least one channel. Residue from the separation columns is pulled through the sample ports, into the channel, and then to the vacuum port. From the vacuum port the residue can be moved, under the force of the vacuum, directly to a drain or to a collection vessel connected with a drain.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Investigation of properties of CdSeTe/Sb and Sb/CdSeTe stacks

The effect of Sb inclusion in CdSeTe thin films was examined. CdSeTe alloys were grown by co-evaporation, either on 5 nm thick electron-beam evaporated Sb layers (Sb/CdSeTe) or coated with Sb post-deposition (CdSeTe/Sb). Sb inclusion improved CdSeTe grain structure, a critical factor for device performance, with average grain size increasing from 0.6 to 1.5 μm. All samples crystallized on annealing to the cubic structure, with a change in film orientation from (111) to random or (220). The presence of Sb in CdSeTe/Sb or Sb/CdSeTe samples, however, had a limited effect on the carrier concentration compared to Sb-free samples. Time resolved photoluminescence showed Sb inclusion increased decay lifetimes, with τ1 = 0.8 ns for and τ2 = 6.9 ns for the Sb/CdSeTe sample.

14 SOLAR ENERGY↗

Development and characterization of a high yield transportable pulsed neutron source with efficient and compact pulsed power system

The results of characterization experiments carried out on a newly developed dense plasma focus device based intense pulsed neutron source with efficient and compact pulsed power system are reported. Its high current sealed pseudospark switch based low inductance capacitor bank with maximum stored energy of ∼10 kJ is segregated into four modules of ∼2.5 kJ each and it cumulatively delivers peak current in the range of 400 kA–600 kA (corresponding to charging voltage range of 14 kV–18 kV) in a quarter time period of ∼2 μs. The neutron yield performance of this device has been optimized by discretely varying deuterium filling gas pressure in the range of 6 mbar–11 mbar at ∼17 kV/550 kA discharge. At ∼7 kJ/8.5 mbar operation, the average neutron yield has been measured to be in the order of ∼4 × 10{sup 9} neutrons/pulse which is the highest ever reported neutron yield from a plasma focus device with the same stored energy. The average forward to radial anisotropy in neutron yield is found to be ∼2. The entire system is contained on a moveable trolley having dimensions 1.5 m × 1 m × 0.7 m and its operation and control (up to the distance of 25 m) are facilitated through optically isolated handheld remote console. The overall compactness of this system provides minimum proximity to small as well as large samples for irradiation. The major intended application objective of this high neutron yield dense plasma focus device development is to explore the feasibility of active neutron interrogation experiments by utilization of intense pulsed neutron sources.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

VitroJet: new features and case studies

Single-particle cryo-electron microscopy has become a widely adopted method in structural biology due to many recent technological advances in microscopes, detectors and image processing. Before being able to inspect a biological sample in an electron microscope, it needs to be deposited in a thin layer on a grid and rapidly frozen. The VitroJet was designed with this aim, as well as avoiding the delicate manual handling and transfer steps that occur during the conventional grid-preparation process. Since its creation, numerous technical developments have resulted in a device that is now widely utilized in multiple laboratories worldwide. It features plasma treatment, low-volume sample deposition through pin printing, optical ice-thickness measurement and cryofixation of pre-clipped Autogrids through jet vitrification. This paper presents recent technical improvements to the VitroJet and the benefits that it brings to the cryo-EM workflow. A wide variety of applications are shown: membrane proteins, nucleosomes, fatty-acid synthase, Tobacco mosaic virus, lipid nanoparticles, tick-borne encephalitis viruses and bacteriophages. These case studies illustrate the advancement of the VitroJet into an instrument that enables accurate control and reproducibility, demonstrating its suitability for time-efficient cryo-EM structure determination.

59 BASIC BIOLOGICAL SCIENCES↗

Three-Dimensional Mass Spectrometric Imaging of Biological Structures Using a Vacuum-Compatible Microfluidic Device

Three-dimensional (3D) molecular imaging of biological structures is important for a wide range of research. In recent decades, secondary ion mass spectrometry (SIMS) has been recognized as a powerful technique for both two-dimensional (2D) and 3D molecular imaging. Sample fixations (e. g., chemical fixation and cryogenic fixation methods) are necessary to adapt biological samples to the vacuum condition in the SIMS chamber, which has been demonstrated to be non-trivial and less controllable, thus limiting the wider application of SIMS on 3D molecular analysis of biological samples. Our group recently developed in situ liquid SIMS that offers great opportunities for the molecular study of various liquids and liquid interfaces. In this work, we demonstrate that a further development of the vacuum-compatible microfluidic device used in in situ liquid SIMS provides a convenient freeze-fixation of biological samples and leads to more controllable and convenient 3D molecular imaging. The special design of this new vacuum-compatible liquid chamber allows an easy determination of sputter rates of ice, which is critical for calibrating the depth scale of frozen biological samples. Sputter yield of a 20 keV Ar 1800 + ion on ice has been determined as 1500 (± 8%) water molecules per Ar 1800 + ion, consistent with our results from molecular dynamics simulations. Moreover, using the information of ice sputter yield, we successfully conduct 3D molecular imaging of frozen homogenized milk and observe network structures of interesting organic and inorganic species. Finally, taken together, our results will significantly benefit various research fields relying on 3D molecular imaging of biological structures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Reversible migration of silver on memorized pathways in Ag-Ge{sub 40}S{sub 60} films

Reversible and reproducible formation and dissolution of silver conductive filaments are studied in Ag-photodoped thin-film Ge{sub 40}S{sub 60} subjected to electric fields. A tip-planar geometry is employed, where a conductive-atomic-force microscopy tip is the tip electrode and a silver patch is the planar electrode. We highlight an inherent “memory” effect in the amorphous chalcogenide solid-state electrolyte, in which particular silver-ion migration pathways are preserved “memorized” during writing and erasing cycles. The “memorized” pathways reflect structural changes in the photodoped chalcogenide film. Structural changes due to silver photodoping, and electrically-induced structural changes arising from silver migration, are elucidated using Raman spectroscopy. Conductive filament formation, dissolution, and electron (reduction) efficiency in a lateral device geometry are related to operation of the nano-ionic Programmable Metallization Cell memory and to newly emerging chalcogenide-based lateral geometry MEMS technologies. The methods in this work can also be used for qualitative multi-parameter sampling of metal/amorphous-chalcogenide combinations, characterizing the growth/dissolution rates, retention and endurance of fractal conductive filaments, with the aim of optimizing devices.

36 MATERIALS SCIENCE↗

Plasma source development for fusion-relevant material testing

Plasma facing materials in the divertor of a magnetic fusion reactor will have to tolerate steady-state plasma heat fluxes in the range of 10 MW/m2 for ~107 sec, in addition to fusion neutron fluences, which can damage the plasma facing materials to high displacements per atom (dpa) of ~50 dpa . Material solutions needed for the plasma facing components are yet to be developed and tested. The Materials Plasma Exposure eXperiment (MPEX) is a newly proposed steady state linear plasma device that is designed to deliver the necessary plasma heat flux to a target for this material testing, including the capability to expose a-priori neutron damaged material samples to those plasmas. The requirements of the plasma source needed to deliver this plasma heat flux are being developed on the Proto-MPEX device, which is a linear high-intensity radio frequency (RF) plasma source that combines a high-density helicon plasma generator with electron and ion heating sections. It is being used to study the physics of heating over-dense plasmas in a linear configuration. The helicon plasma is operated at 13.56 MHz with RF power levels up to 120 kW. Microwaves at 28 GHz (~30 kW) are coupled to the electrons in the over-dense helicon plasma via Electron Bernstein Waves (EBW), and ion cyclotron heating at 7-9 MHz (~30 kW) is via a magnetic beach approach. High plasma densities >6x1019/m3 have been produced in deuterium, with electron temperatures that can range from 2 to >10 eV. Operation with on-axis magnetic field strengths between 0.6 and 1.4 T is typical. The plasma heat flux delivered to a target can be > 10 MW/m2, depending on the operating conditions.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

First lithium experiments in HIDRA and evidence of helium retention during quasi-steady-state stellarator plasma operations

Recent experiments in Hybrid Illinois Device for Research and Applications (HIDRA) have had operational discharges between t discharge = 60 and 1000 s using electron cyclotron resonant heating (ECRH) of the plasma. This means that quasi-steady-state plasma discharges reach conditions to study long-pulse plasma material interactions (PMIs). The newly commissioned HIDRA-Material Analysis Test-stand PMI diagnostic is used to place a drop of lithium onto a heated tungsten surface, transfer the sample in-vacuo and expose it in a helium plasma. Helium is of interest as there is an open question to whether lithium will be able to remove helium ash in real fusion devices. The introduction of the W-Li sample in HIDRA resulted in evaporation of lithium into the helium plasma during a 600 s pulse and caused a reduction of over 90% in neutral pressure during the discharge. It was also observed that the plasma density and temperature increased by over 2.5 times. Using spectroscopy and a helium collisional radiative model, the peak temperature and density of the helium plasma can be monitored during the discharge. During lithium evaporation, as significant lithium ionization occurs, there is a 85% drop in the HIDRA vessel neutral pressure, despite a constant flow rate of He gas. This reduction in neutral pressure is supported by spectroscopy data with corresponding reductions in He I line intensities (587 nm, 667 nm, 706 nm, and 728 nm), as well as those of other impurities. At one point in the discharge a lithium plasma is created, as indicated by an increase in Li + emission and a complete reduction in He + emission, but the electron density jumps from ne = 3 × 10 18 m –3 to over ne = 8 × 10 18 m –3 while the core temperature stays relatively constant between Te = 16 eV and 20 eV. Once lithium has completely evaporated from the sample and the majority of the ionized lithium has diffused from the plasma to the vessel walls, pressure and spectroscopy data paired with He collisional radiative model calculations shows a re-establishment of a helium plasma in a low recycling regime. In this regime, the density drops down to ne = 2 × 10 18 m –3 and the electron temperature increases from T e = 20 eV to over T e = 50 eV indicating an increase in helium heating efficiency. This is also indicated by the He+ emission re-establishing and having a higher intensity. Here, we show the results from the first lithium campaign in HIDRA. In the presence of lithium, and in particular when lithium ions are present, the helium disappears from the plasma via an as of yet unknown complex relationship that needs to be further studied. The most likely explanation is that the lithium ions are distributed around the vessel and able to trap helium to the surface turning HIDRA into a large gettering surface. These results have potential implications on future plasma facing component design using liquid lithium for impurity and recycling control using limiters and divertors.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Conceptual Design and Analysis of In-Vessel Components for the Materials Plasma Exposure eXperiment (MPEX)

The materials plasma exposure experiment (MPEX) is a linear plasma divertor simulator currently undergoing conceptual design. The facility will expose material samples to steady-state plasma fluxes to examine plasma–material interactions (PMIs) that are expected in the next generation of fusion devices. The plasmas will be generated by a helicon source, with electron and ion heating sources of up to 800 kW possible. The peak heat fluxes of the target are expected to be up to 10 MW/m 2 . The facility will be capable of handling low-activation neutron-irradiated samples in order to examine the multivariate effects of neutron damage and plasma fluence. Neutron-irradiated samples are planned to be roughly of 10-mm diameter; however, plasma-facing components up to 60×600 mm can be accommodated. The steady-state nature of the device will require the magnetic confinement of the plasma to be achieved with superconducting magnets, with a maximum on-axis field of 2.5 T. In addition, since MPEX will be a steady-state device, in-vessel components need to be water cooled. The primary in-vessel components will be the target, the dump plate, the limiter, the skimmers, and the microwave absorber. The conceptual design of these components is presented here, including analyses that confirm that the designs are adequate to meet the requirements of MPEX operation.

Lumsdaine, Arnold↗

Note: Optical receiver system for 152-channel magnetoencephalography

An optical receiver system composing 13 serial data restore/synchronizer modules and a single module combiner converted optical 32-bit serial data into 32-bit synchronous parallel data for a computer to acquire 152-channel magnetoencephalography (MEG) signals. A serial data restore/synchronizer module identified 32-bit channel-voltage bits from 48-bit streaming serial data, and then consecutively reproduced 13 times of 32-bit serial data, acting in a synchronous clock. After selecting a single among 13 reproduced data in each module, a module combiner converted it into 32-bit parallel data, which were carried to 32-port digital input board in a computer. When the receiver system together with optical transmitters were applied to 152-channel superconducting quantum interference device sensors, this MEG system maintained a field noise level of 3 fT/√Hz @ 100 Hz at a sample rate of 1 kSample/s per channel.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

An Efficient Algorithm for Automatic Structure Optimization in X-ray Standing-Wave Experiments

We present that x-ray standing-wave photoemission experiments involving multilayered samples are emerging as unique probes of the buried interfaces that are ubiquitous in current device and materials research. Such data require for their analysis a structure optimization process comparing experiment to theory that is not straightforward. In this work, we present a new computer program for optimizing the analysis of standing-wave data, called SWOPT, that automates this trial-and-error optimization process. The program includes an algorithm that has been developed for computationally expensive problems: so-called black-box simulation optimizations. It also includes a more efficient version of the Yang X-ray Optics Program (YXRO) [Yang, S.-H., Gray, A.X., Kaiser, A.M., Mun, B.S., Sell, B.C., Kortright, J.B., Fadley, C.S., J. Appl. Phys. 113, 1 (2013)] which is about an order of magnitude faster than the original version. Human interaction is not required during optimization. We tested our optimization algorithm on real and hypothetical problems and show that it finds better solutions significantly faster than a random search approach. The total optimization time ranges, depending on the sample structure, from minutes to a few hours on a modern laptop computer, and can be up to 100x faster than a corresponding manual optimization. Finally, these speeds make the SWOPT program a valuable tool for realtime analyses of data during synchrotron experiments.

36 MATERIALS SCIENCE↗

An in situ runaway electron diagnostic for DIII-D

We are designing a new diagnostic based on laser inverse Compton scattering to study the dynamics of runaway electron formation during killer-pellet triggered disruptions in DIII-D, and their subsequent loss. We can improve the expected S/N ratio by using a high-intensity short-pulse laser combined with gated x-ray imagers. With 80 ps sampling, time-of-flight spatial resolution within the laser chord can be obtained. We will measure the time-resolved spatial profile and energy distribution of the runaway electrons while they are in the core of the tokamak plasma.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Effect of particle size distribution on the structure, hyperfine, and magnetic properties of Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} nanopowders

Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} nano powders were synthesized by an auto combustion method and then heat treated at different temperatures in air for a fixed time. As a consequence, a distribution in particle size and strain was incorporated within the specimens, as estimated from the Rietveld refinement analysis of the powder x-ray diffraction data. The changes in the microstructure and crystal structure parameters were carefully extracted through the refinement analysis. Thermal annealing causes increment in the dispersion and mean of the size distribution. Reallocation of cations in the lattice sites occur as a consequence of the heat treatment which was manifested in their altered unit cell length (a), r.m.s. strain (〈ε{sup 2}〉{sup 1/2}), oxygen positional parameter (u), metal-oxygen bond lengths (R{sub OA} and R{sub OB}), and the band positions (ν{sub 1}and ν{sub 2}) in the vibrational spectroscopy. We also investigate the hyperfine and magnetic properties of the samples using different instrumental techniques (with different operating time scales) like Mössbauer spectroscopy, electron paramagnetic resonance spectroscopy, and superconducting quantum interference device magnetometry. Results show that the effect of particle size distribution was manifested in their hyperfine field distribution profile, paramagnetic resonance spectra, and magnetic anisotropy energy distribution profile. Co-existence of superparamagnetic and ferrimagnetic phase was recorded at room temperature in the samples when annealed at lower temperature. However, with increase in annealing temperature, the nature of the size distribution changes and ferrimagnetic ordering predominates for the larger size nanoparticles. Thus, the effect of particle size distribution on the structural, hyperfine, and magnetic properties of various Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} nanoparticles was investigated herein which hitherto has not been discussed in the literature.

36 MATERIALS SCIENCE↗

Design of smart 3D-digital X-ray microtomographic scanners for non-destructive testing of materials and components of electronic devices with a multilayered structure

The article studies the operating procedures of an X-ray microtomographic scanner and the module of reconstruction and analysis 3D-image of a test sample in particular. An algorithm for 3D-image reconstruction based on image shadow projections and mathematical methods of the processing are described. Chapter 1 describes the basic principles of X-ray tomography and general procedures of the device developed. Chapters 2 and 3 are devoted to the problem of resources saving by the system during the X-ray tomography procedure, which is achieved by preprocessing of the initial shadow projections. Preprocessing includes background noise removing from the images, which reduces the amount of shadow projections in general and increases the efficiency of the group shadow projections compression. Chapter 4 covers general procedures of defect search, which is based on vector analysis principles. In conclusion, the main applications of X-ray tomography are presented.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Improvement of the Superconducting Properties of GdBa{sub 2}Cu{sub 3}O{sub 7-δ} with Nano-Sized Ferrite Addition

We have been investigating the effect of (CoFe{sub 2}O{sub 4}){sub x} and (ZnFe{sub 2}O{sub 4}){sub x} (x is the wt%) nano-sized ferrites on the superconducting (SC) properties of the high-T{sub c} SC compound GdBa{sub 2}Cu{sub 3}O{sub 7-δ} (Gd123) prepared by the conventional solid-state reaction technique. In this work, the magnetic hysteresis for pure Gd123 samples and samples added with nano-sized ferrites was measured using a superconducting quantum interference device (SQUID) magnetometer using a dc field up to 30,000 Oe. The magnetic J{sub c} was estimated using the extended Bean model. While a clear increase in J{sub c} values with the addition of (CoFe{sub 2}O{sub 4}){sub x} nano-sized ferrites is observed, a less clear positive effect on the J{sub c} values is observed with the addition of (ZnFe{sub 2}O{sub 4}){sub x} nano-sized ferrites. These results indicate an improvement of grain connectivity, decrease of voids between the grains, and decrease of porosity in Gd123 compound resulting from CoFe{sub 2}O{sub 4} addition consistent with the mechanical properties measured before. (CoFe{sub 2}O{sub 4}){sub x} nano-sized ferrite addition has thus resulted in an improvement in the SC properties of Gd123 high-T{sub c} SC compound making it more convenient for applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Preparation of RE(DBM){sub 3}·Phen (RE=Eu{sup 3+},Tb{sup 3+}) Plate-Loading Fe{sub 3}O{sub 4} Nanospheres and their Magnetic-Optic Bifunctional Property

A facile wet chemical method has been used to synthesize bifunctional core-shell nanoparticles of Fe{sub 3}O{sub 4}@RE(DBM){sub 3}·Phen (RE=Eu{sup 3+},Tb{sup 3+}) showing an interesting combination of magnetic and luminescent properties. This method is convenient, cheap, and efficient. The morphology, structure, luminescent, and magnetic properties of the nanoparticles were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis absorption, fluorescence emission, and superconducting quantum interference device magnetometer (SQUID-VSM). The maximum emission peaks of novel Eu{sup 3+} and Tb{sup 3+} nanocomposites are at 618 nm and at 514 nm, respectively. And their corresponding special saturation magnetization Ms. are 25.853 emu/g and 24.015 emu/g, respectively. For the nanoparticles, it is shown that there have better magnetic behavior and they may act as red- and green-emitting material with potential application for fluorescent magnetic particle testing. Moreover, this chemical route could be used to obtain the development of several bifunctional systems of other rare earth ions for practical application.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Large-Grained Cylindrical Block Copolymer Morphologies by One-Step Room-Temperature Casting

We report a facile method of ordering block copolymer (BCP) morphologies in which the conventional two-step casting and annealing steps are replaced by a single-step process where microphase separation and grain coarsening are seamlessly integrated within the casting protocol. This is achieved by slowing down solvent evaporation during casting by introducing a non-volatile solvent into the BCP casting solution what effectively prolongs the duration of the grain-growth phase. We demonstrate the utility of this solvent evaporation annealing (SEA) method by producing well-ordered large molecular-weight BCP thin films in a total processing time shorter than 3 minutes without resorting to any extra laboratory equipment other than a basic casting-device i.e., spin- or blade-coater. By analyzing the morphologies of the quenched samples, we identify a relatively narrow range of polymer concentration in the wet film, just above the order-disorder concentration, to be critical for obtaining large-grained morphologies. This finding is corroborated by the analysis of the grain-growth kinetics of horizontally-oriented cylindrical domains where relatively large growth exponents (1/2) are observed, indicative of a more rapid defect-annihilation mechanism in the concentrated BCP solution than in thermally-annealed BCP melts. Furthermore, the analysis of temperature-resolved kinetics data allows us to calculate the Arrhenius activation energy of the grain-coarsening in this one-step BCP ordering process.

36 MATERIALS SCIENCE↗

Ionic electroactive polymer actuators as active microfluidic mixers

On-chip sample processing is integral to the continued development of lab-on-a-chip devices for various applications. An active microfluidic mixer prototype is proposed using ionic electroactive polymer actuators (IEAPAs) as artificial cilia. A proof-of-concept experiment was performed in which the actuators were shown to produce localized flow pattern disruptions in the laminar flow regime. Suggestions for further engineering and optimization of a scaled-down, complete device are provided. Furthermore, the device in its current state of development necessitates further engineering, the use of IEAPAs addresses issues currently associated with the use of electromechanical actuators as active microfluidic mixers and may prove to be a useful alternative to other similar materials.

36 MATERIALS SCIENCE↗