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At least 1,441 records · Page 80

Atom Probe Tomography of Molecular Organic Materials: Sub-Dalton Nanometer-Scale Quantification

In this article, we demonstrate that atom probe tomography (APT) can be applied to small-molecule organic materials. We show that APT can provide an unprecedented combination of mass resolution of <1 Da, spatial resolution of ~0.3 nm in z and ~1 nm in x–y, and analytic sensitivity of ~50 ppm with no evidence of molecular fragmentation. We discuss two systems that demonstrate the power of APT to uncover structure–property relationships in organic systems that have proven extremely difficult to probe using existing techniques: (1) a previously published model organic photovoltaic system in which we show a chemical reaction occurs at the heterointerface; and (2) a model organic light-emitting diode system in which we show molecular segregation occurs in the emissive layer bulk. Lastly, these examples illustrate the power of APT to enable new insights into organic molecular materials.

36 MATERIALS SCIENCE↗

Understanding Fragmentation of Organic Small Molecules in Atom Probe Tomography

In atom probe tomography of molecular organic materials, field ionization of either entire molecules or molecular fragments can occur, but the mechanism governing this behavior was not previously understood. This work explains when a doubly ionized small molecule organic material is expected to undergo fragmentation. Here, we find that multiple detection events arising from post-ionization fragmentation of a parent molecular dication into two daughter ions is well explained by the free energy and geometries of the molecules computed using density functional theory. Of the systems studied, exergonic free energies for formation of the daughter ions, smaller activation energies for dissociation, and increases in bond length are all found to be quantitative predictors for ion fragmentation. This work expands the applicability of atom probe tomography to organic materials by increasing the fundamental understanding of processes occurring during this analysis technique.

36 MATERIALS SCIENCE↗

Decoupling Mesoscale Functional Response in PLZT across the Ferroelectric–Relaxor Phase Transition with Contact Kelvin Probe Force Microscopy and Machine Learning

Relaxor ferroelectrics exhibit a range of interesting material behavior, including high electromechanical response, polarization rotations, as well as temperature and electric field-driven phase transitions. The origin of this unusual functional behavior remains elusive due to limited knowledge on polarization dynamics at the nanoscale. Piezoresponse force microscopy and associated switching spectroscopy provide access to local electromechanical properties on the micro- and nanoscale, which can help to address some of these gaps in our knowledge. However, these techniques are inherently prone to artefacts caused by signal contributions emanating from electrostatic interactions between tip and sample. Understanding functional behavior of complex, disordered systems like relaxor materials with unknown electromechanical properties therefore requires a technique that allows distinguishing between electromechanical and electrostatic response. Here, contact Kelvin probe force microscopy (cKPFM) is used to gain insight into the evolution of local electromechanical and capacitive properties of a representative relaxor material lead lanthanum zirconate across the phase transition from a ferroelectric to relaxor state. The obtained multidimensional data set was processed using an unsupervised machine learning algorithm to detect variations in functional response across the probed area and temperature range. Further analysis showed the formation of two separate cKPFM response bands below 50 °C, providing evidence for polarization switching. At higher temperatures only one band is observed, indicating an electrostatic origin of the measured response. In addition, the junction potential difference, which was extracted from the cKPFM data, becomes independent of the temperature in the relaxor state. As a result, the combination of this multidimensional voltage spectroscopy technique and machine learning allows to identify the origin of the measured functional response and to decouple ferroelectric from electrostatic phenomena necessary to understand the functional behavior of complex, disordered systems like relaxor materials.

36 MATERIALS SCIENCE↗

Nanoscale Probing of Elastic–Electronic Response to Vacancy Motion in NiO Nanocrystals

Measuring the diffusion of ions and vacancies at nanometer length scales is crucial to understanding fundamental mechanisms driving technologies as diverse as batteries, fuel cells, and memristors; yet such measurements remain extremely challenging. Here in this paper, we employ a multimodal scanning probe microscopy (SPM) technique to explore the interplay between electronic, elastic, and ionic processes via first-order reversal curve I–V measurements in conjunction with electrochemical strain microscopy (ESM). The technique is employed to investigate the diffusion of oxygen vacancies in model epitaxial nickel oxide (NiO) nanocrystals with resistive switching characteristics. Results indicate that opening of the ESM hysteresis loop is strongly correlated with changes to the resonant frequency, hinting that elastic changes stem from the motion of oxygen (or cation) vacancies in the probed volume of the SPM tip. These changes are further correlated to the current measured on each nanostructure, which shows a hysteresis loop opening at larger (~2.5 V) voltage windows, suggesting the threshold field for vacancy migration. This study highlights the utility of local multimodal SPM in determining functional and chemical changes in nanoscale volumes in nanostructured NiO, with potential use to explore a wide variety of materials including phase-change memories and memristive devices in combination with site-correlated chemical imaging tools.

36 MATERIALS SCIENCE↗

Automated data extraction from in situ protein stable isotope probing studies

Protein stable isotope probing (protein-SIP) has strong potential for revealing key metabolizing taxa in complex microbial communities. While most protein-SIP work to date has been performed under controlled laboratory conditions to allow extensive isotope labeling of the target organism, a key application will be in situ studies of microbial communities under conditions that result in small degrees of partial labeling. One hurdle restricting large scale in situ protein-SIP studies is the lack of algorithms and software for automated data processing of the massive data sets resulting from such studies. In response, we developed Stable Isotope Probing Protein Extraction Resources software (SIPPER) and applied it for large scale extraction and visualization of data from short term (3 h) protein-SIP experiments performed in situ on Yellowstone phototrophic bacterial mats. Several metrics incorporated into the software allow it to support exhaustive analysis of the complex composite isotopic envelope observed as a result of low amounts of partial label incorporation. SIPPER also enables the detection of labeled molecular species without the need for any prior identification.

13C labeling↗

What Causes Radiation Belt Enhancements: A Survey of the Van Allen Probes Era

We survey radiation belt enhancement events during the Van Allen Probes era to determine what mechanism is the dominant cause of enhancements and where it is most effective. Two primary mechanisms have been proposed: (1) betatron/Fermi acceleration due to the Earthward radial transport of electrons, which produces monotonic gradients in phase space density (PSD), and (2) “local acceleration” due to gyro/Landau resonant interaction with electromagnetic waves, which produces radially localized growing peaks in PSD. Here, to differentiate between these processes, we examine radial profiles of PSD in adiabatic coordinates using data from the Van Allen Probes and Time History of Events and Macroscale Interactions during Substorms satellites for 80 outer belt enhancement events from October 2012 to April 2017. Here, this study shows that local acceleration is the dominant acceleration mechanism for MeV electrons in the outer belt, with 87% of the enhancement events exhibiting growing peaks. The strong correlation of the location of these with geomagnetic activity further supports this conclusion.

79 ASTRONOMY AND ASTROPHYSICS↗

Time, momentum, and energy resolved pump-probe tunneling spectroscopy of two-dimensional electron systems

Abstract Real-time probing of electrons can uncover intricate relaxation mechanisms and many-body interactions in strongly correlated materials. Here, we introduce time, momentum, and energy resolved pump-probe tunneling spectroscopy (Tr-MERTS). The method allows the injection of electrons at a particular energy and observation of their subsequent decay in energy-momentum space. Using Tr-MERTS, we visualize electronic decay processes, with lifetimes from tens of nanoseconds to tens of microseconds, in Landau levels formed in a GaAs quantum well. Although most observed features agree with simple energy-relaxation, we discovered a splitting in the nonequilibrium energy spectrum in the vicinity of a ferromagnetic state. An exact diagonalization study suggests that the splitting arises from a maximally spin-polarized state with higher energy than a conventional equilibrium skyrmion. Furthermore, we observe time-dependent relaxation of the splitting, which we attribute to single-flipped spins forming skyrmions. These results establish Tr-MERTS as a powerful tool for studying the properties of a 2DES beyond equilibrium.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Design and testing of ultrasound probe adapters for a robotic imaging platform

Medical imaging-based triage is a critical tool for emergency medicine in both civilian and military settings. Ultrasound imaging can be used to rapidly identify free fluid in abdominal and thoracic cavities which could necessitate immediate surgical intervention. However, proper ultrasound image capture requires a skilled ultrasonography technician who is likely unavailable at the point of injury where resources are limited. Instead, robotics and computer vision technology can simplify image acquisition. As a first step towards this larger goal, here, we focus on the development of prototypes for ultrasound probe securement using a robotics platform. The ability of four probe adapter technologies to precisely capture images at anatomical locations, repeatedly, and with different ultrasound transducer types were evaluated across more than five scoring criteria. Testing demonstrated two of the adapters outperformed the traditional robot gripper and manual image capture, with a compact, rotating design compatible with wireless imaging technology being most suitable for use at the point of injury. Next steps will integrate the robotic platform with computer vision and deep learning image interpretation models to automate image capture and diagnosis. This will lower the skill threshold needed for medical imaging-based triage, enabling this procedure to be available at or near the point of injury.

47 OTHER INSTRUMENTATION↗

Probing electron acceleration and x-ray emission in laser-plasma accelerators

While laser-plasma accelerators have demonstrated a strong potential in the acceleration of electrons up to giga-electronvolt energies, few experimental tools for studying the acceleration physics have been developed. In this paper, we demonstrate a method for probing the acceleration process. A second laser beam, propagating perpendicular to the main beam, is focused on the gas jet few nanosecond before the main beam creates the accelerating plasma wave. This second beam is intense enough to ionize the gas and form a density depletion, which will locally inhibit the acceleration. The position of the density depletion is scanned along the interaction length to probe the electron injection and acceleration, and the betatron X-ray emission. To illustrate the potential of the method, the variation of the injection position with the plasma density is studied.

43 PARTICLE ACCELERATORS↗

Electron energy distribution function by using probe method in electron cyclotron resonance multicharged ion source

We are constructing a tandem type electron cyclotron resonance (ECR) ion source (ECRIS). High-energy electrons in ECRIS plasma affect electron energy distribution and generate multicharged ion. In this study, we measure electron energy distribution function (EEDF) of low energy region (≦100 eV) in ECRIS plasma at extremely low pressures (10{sup −3}–10{sup −5} Pa) by using cylindrical Langmuir probe. From the result, it is found that the EEDF correlates with the electron density and the temperature from the conventional probe analysis. In addition, we confirm that the tail of EEDF spreads to high energy region as the pressure rises and that there are electrons with high energy in ECR multicharged ion source plasma. The effective temperature estimated from the experimentally obtained EEDF is larger than the electron temperature obtained from the conventional method.

43 PARTICLE ACCELERATORS↗

Ultrafast supercontinuum fiber-laser based pump-probe scanning magneto-optical Kerr effect microscope for the investigation of electron spin dynamics in semiconductors at cryogenic temperatures with picosecond time and micrometer spatial resolution

We describe a two-color pump-probe scanning magneto-optical Kerr effect microscope which we have developed to investigate electron spin phenomena in semiconductors at cryogenic temperatures with picosecond time and micrometer spatial resolution. The key innovation of our microscope is the usage of an ultrafast “white light” supercontinuum fiber-laser source which provides access to the whole visible and near-infrared spectral range. Our Kerr microscope allows for the independent selection of the excitation and detection energy while avoiding the necessity to synchronize the pulse trains of two separate picosecond laser systems. The ability to independently tune the pump and probe wavelength enables the investigation of the influence of excitation energy on the optically induced electron spin dynamics in semiconductors. We demonstrate picosecond real-space imaging of the diffusive expansion of optically excited electron spin packets in a (110) GaAs quantum well sample to illustrate the capabilities of the instrument.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

A diamond-based scanning probe spin sensor operating at low temperature in ultra-high vacuum

We present the design and performance of an ultra-high vacuum (UHV) low temperature scanning probe microscope employing the nitrogen-vacancy color center in diamond as an ultrasensitive magnetic field sensor. Using this center as an atomic-size scanning probe has enabled imaging of nanoscale magnetic fields and single spins under ambient conditions. In this article we describe an experimental setup to operate this sensor in a cryogenic UHV environment. This will extend the applicability to a variety of molecular systems due to the enhanced target spin lifetimes at low temperature and the controlled sample preparation under UHV conditions. The instrument combines a tuning-fork based atomic force microscope (AFM) with a high numeric aperture confocal microscope and the facilities for application of radio-frequency (RF) fields for spin manipulation. We verify a sample temperature of <50 K even for strong laser and RF excitation and demonstrate magnetic resonance imaging with a magnetic AFM tip.

36 MATERIALS SCIENCE↗

Interaction between O{sub 2} and ZnO films probed by time-dependent second-harmonic generation

The interaction between O{sub 2} and ZnO thin films prepared by atomic layer deposition has been investigated by time-dependent second-harmonic generation, by probing the electric field induced by adsorbed oxygen molecules on the surface. The second-harmonic generated signal decays upon laser exposure due to two-photon assisted desorption of O{sub 2}. Blocking and unblocking the laser beam for different time intervals reveals the adsorption rate of O{sub 2} onto ZnO. The results demonstrate that electric field induced second-harmonic generation provides a versatile non-contact probe of the adsorption kinetics of molecules on ZnO thin films.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

A pulsed eddy current probe for inspection of support plates from within Alloy-800 steam generator tubes

Support plate degradation and fouling in nuclear steam generators (SGs) can lead to SG tube corrosion and loss of efficiency. Inspection and monitoring of these conditions can be integrated with preventive maintenance programs, thereby advancing station-life management processes. A prototype pulsed eddy current (PEC) probe, targeting inspection issues associated with SG tubes in SS410 tube support plate structures, has been developed using commercial finite element (FE) software. FE modeling was used to identify appropriate driver and pickup coil configurations for optimum sensitivity to changes in gap and offset for Alloy-800 SG tubes passing through 25 mm thick SS410 support plates. Experimental measurements using a probe that was manufactured based on the modeled configuration, were used to confirm the sensitivity of differential PEC signals to changes in relative position of the tube within the tube support plate holes. Models investigated the effect of shift and tilt of tube with respect to hole centers. Near hole centers and for small shifts, modeled signal amplitudes from the differentially connected coil pairs were observed to change linearly with tube shift. This was in agreement with experimentally measured TEC coil response. The work paves the way for development of a system targeting the inspection and evaluation of support plate structures in steam generators.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Note: Switching crosstalk on and off in Kelvin probe force microscopy

In Kelvin Probe Force Microscopy (KPFM) electronic crosstalk can occur between the excitation signal and probe deflection signal. Here, we demonstrate how a small modification to our commercial instrument enables us to literally switch the crosstalk on and off. We study in detail the effect of crosstalk on open-loop KPFM and compare with closed-loop KPFM. We measure the pure crosstalk signal and verify that we can correct for it in the data-processing required for open-loop KPFM. We also demonstrate that open-loop KPFM results are independent of the frequency and amplitude of the excitation signal, provided that the influence of crosstalk has been eliminated.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Note: On the measurement of plasma potential fluctuations using emissive probes

In this Note, it is pointed out that emissive probes cannot be used to directly and reliably measure plasma potential fluctuations. An experimentally validated model demonstrates indeed that the floating potential fluctuations of an emissive probe which floats at the mean plasma potential depend not only on the plasma potential fluctuations but also on electron density and temperature fluctuations.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Probes for investigating the effect of magnetic field, field orientation, temperature and strain on the critical current density of anisotropic high-temperature superconducting tapes in a split-pair 15 T horizontal magnet

We present the designs of probes for making critical current density (J{sub c}) measurements on anisotropic high-temperature superconducting tapes as a function of field, field orientation, temperature and strain in our 40 mm bore, split-pair 15 T horizontal magnet. Emphasis is placed on the design of three components: the vapour-cooled current leads, the variable temperature enclosure, and the springboard-shaped bending beam sample holder. The vapour-cooled brass critical-current leads used superconducting tapes and in operation ran hot with a duty cycle (D) of ∼0.2. This work provides formulae for optimising cryogenic consumption and calculating cryogenic boil-off, associated with current leads used to make J{sub c} measurements, made by uniformly ramping the current up to a maximum current (I{sub max}) and then reducing the current very quickly to zero. They include consideration of the effects of duty cycle, static helium boil-off from the magnet and Dewar (b{sup ′}), and the maximum safe temperature for the critical-current leads (T{sub max}). Our optimized critical-current leads have a boil-off that is about 30% less than leads optimized for magnet operation at the same maximum current. Numerical calculations show that the optimum cross-sectional area (A) for each current lead can be parameterized by LI{sub max}/A=[1.46D{sup −0.18}L{sup 0.4}(T{sub max}−300){sup 0.25D{sup −{sup 0{sup .{sup 0{sup 9}}}}}}+750(b{sup ′}/I{sub max})D{sup 10{sup −{sup 3I{sub m}{sub a}{sub x}−2.87b{sup ′}}}}]× 10{sup 6}A m{sup −1} where L is the current lead's length and the current lead is operated in liquid helium. An optimum A of 132 mm{sup 2} is obtained when I{sub max} = 1000 A, T{sub max} = 400 K, D = 0.2, b{sup ′} = 0.3 l h{sup −1} and L = 1.0 m. The optimized helium consumption was found to be 0.7 l h{sup −1}. When the static boil-off is small, optimized leads have a boil-off that can be roughly parameterized by: b/I{sub max } ≈ (1.35 × 10{sup −3})D{sup 0.41} l h{sup ‑1} A{sup −1}. A split-current-lead design is employed to minimize the rotation of the probes during the high current measurements in our high-field horizontal magnet. The variable-temperature system is based on the use of an inverted insulating cup that operates above 4.2 K in liquid helium and above 77.4 K in liquid nitrogen, with a stability of ±80 mK to ±150 mK. Uniaxial strains of −1.4% to 1.0% can be applied to the sample, with a total uncertainty of better than ±0.02%, using a modified bending beam apparatus which includes a copper beryllium springboard-shaped sample holder.

43 PARTICLE ACCELERATORS↗

Langmuir probes for SPIDER (source for the production of ions of deuterium extracted from radio frequency plasma) experiment: Tests in BATMAN (Bavarian test machine for negative ions)

A prototype system of the Langmuir probes for SPIDER (Source for the production of Ions of Deuterium Extracted from RF plasma) was manufactured and experimentally qualified. The diagnostic was operated in RF (Radio Frequency) plasmas with cesium evaporation on the BATMAN (BAvarian Test MAchine for Negative ions) test facility, which can provide plasma conditions as expected in the SPIDER source. A RF passive compensation circuit was realised to operate the Langmuir probes in RF plasmas. The sensors’ holder, designed to better simulate the bias plate conditions in SPIDER, was exposed to a severe experimental campaign in BATMAN with cesium evaporation. No detrimental effect on the diagnostic due to cesium evaporation was found during the exposure to the BATMAN plasma and in particular the insulation of the electrodes was preserved. The paper presents the system prototype, the RF compensation circuit, the acquisition system (as foreseen in SPIDER), and the results obtained during the experimental campaigns.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗