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Dynamic surface and subsurface morphology and chemistry of socketed nanoparticles is monitored in situ for an important emerging class of nanoparticles.
Lead halide perovskites have emerged as promising absorber materials over the last decade to increase the efficiency of photovoltaics beyond its current limits. However, to further optimize the performance of perovskites, more detailed studies need to be performed which allow for the correlation of film morphology and local electronic properties at the nanoscale. In this paper, we present a scanning tunneling microscopy (STM) approach to probe the effect of an applied electric field of a methylammonium formamidinium lead triiodide perovskite thin film on the film response by current-voltage spectroscopy, current imaging tunneling spectroscopy, differential conductance mapping and X-ray absorption spectroscopy (XAS) by means of synchrotron X-ray STM (SX-STM). We find a strong correlation between the measurement conditions and the obtained current-voltage characteristics when imaging under opposite applied bias polarities. In particular, we find similarities to already observed poling effects for perovskites which result in either a positively or negatively charged interface due to ion and vacancy migration. Our results provide insight into the influence of measurement conditions such as bias polarity on the performance assessment of perovskite thin films by STM.
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In situ high-pressure ultrasonic velocity measurements of CaAl 2 O 4 glass reveal abrupt irreversible discontinuities in the elastic wave velocities at ~8–10 GPa. Total structure factor and pair distribution functions measured by synchrotron x-ray diffraction show a rapid change in the intermediate range structure attributed to a rearrangement of calcium ions over this narrow pressure region. Atomistic models obtained from molecular dynamics simulations reveal that this intermediate range structure is explained by a transition of Ca–O void radius distribution from a bimodal distribution with peaks at ~2.1 and ~2.4 Å to a single distribution centered at ~2.1 Å. Further, these abrupt structural changes involving the rapid increase in elastic wave velocity are markedly different to the continuous transformations observed in conventional network-forming glasses, such as SiO 2 .
In recent years, there have been numerous efforts worldwide to develop the synchrotron X-ray scanning tunneling microscopy (SX-STM) technique. Here, the inauguration of XTIP, the world's first beamline fully dedicated to SX-STM, is reported. The XTIP beamline is located at Sector 4 of the Advanced Photon Source at Argonne National Laboratory. It features an insertion device that can provide left- or right-circular as well as horizontal- and vertical-linear polarization. XTIP delivers monochromatic soft X-rays of between 400 and 1900 eV focused into an environmental enclosure that houses the endstation instrument. This article discusses the beamline system design and its performance.
An ultra-high-vacuum compatible X-ray chopper system has been designed, constructed and integrated into the XTIP beamline at the Advanced Photon Source at Argonne National Laboratory. The XTIP beamline can operate at soft X-ray energies from 400 eV to 1900 eV while providing a focused beam down to about 10 µm × 10 µm into the synchrotron X-ray scanning tunneling microscopy (SX-STM) endstation instrument. The X-ray chopper is a critical component for separating topographic information from chemical information in SX-STM through phase-sensitive current detection. Depending on the experimental needs, the modulation frequency can be controlled from 100 Hz to 10 kHz. In addition, the chopper system is fully bakeable and can achieve a base pressure of 10 -10 mbar. Facilities for active water cooling have been designed, but passive cooling through copper braids has been shown to be sufficient at standard chopping frequencies. Using an Fe/Al 2 O 3 /CoAl(111) sample, the separation of the SX-STM current into a chemical component and a stable feedback signal is demonstrated.
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Abstract not provided.
Knowledge of the structural behavior of silicate melts and/or glasses at high pressures provides fundamental information for discussing the nature and properties of silicate magmas in the Earth’s interior. The behavior of Si-O structures under high-pressure conditions has been widely studied, while the effect of cation atoms on the high-pressure structural behavior of silicate melts or glasses has not been well investigated. Here, in this study, we investigated the structures of MgSiO 3 and CaSiO 3 glasses up to 5.4 GPa by in situ X-ray pair distribution function measurements to understand the effect of different cations (Mg 2+ and Ca 2+ ) on high-pressure structural behavior of silicate glasses. We found that the structural behavior of MgSiO 3 and CaSiO 3 glasses are different at high pressures. The structure of MgSiO 3 glass changes by shrinking of Si-O-Si angle with increasing pressures, which is consistent with previous studies for SiO 2 and MgSiO 3 glasses. On the other hand, CaSiO 3 glass shows almost no change in Si-Si distance at high pressures, while the intensities of two peaks at ~3.0 and ~3.5 Å change with increasing pressure. The structural change in CaSiO 3 glass at high pressure is interpreted as the change in the fraction of the edge-shared and corner-shared CaO 6 -SiO 4 structures. The different high-pressure structural behavior observed in MgSiO 3 and CaSiO 3 glasses may be the origin of differences in properties, such as viscosity between MgSiO 3 and CaSiO 3 melts at high pressures. This signifies the importance of different structural behaviors due to different cations in investigations of the nature and properties of silicate magmas in Earth’s interior.
Abstract not provided.
Introduction Amplification of human chromosome 3q26-29, which encodes oncoprotein ΔNp63 among other isoforms of the p63 family, is a feature common to squamous cell carcinomas (SCCs) of multiple tissue origins. Along with overexpression of ΔNp63, activation of the protooncogene, RAS , whether by overexpression or oncogenic mutation, is frequently observed in many cancers. In this study, analysis of transcriptome data from The Cancer Genome Atlas (TCGA) demonstrated that expression of TP63 mRNA , particularly ΔNp63 isoforms, and HRAS are significantly elevated in advanced squamous cell carcinomas of the head and neck (HNSCCs), suggesting pathological significance. However, how co-overexpressed ΔNp63 and HRAS affect the immunosuppressive tumor microenvironment (TME) is incompletely understood. Methods Here, we established and characterized an immune competent mouse model using primary keratinocytes with retroviral-mediated overexpression of ΔNp63α and constitutively activated HRAS (v-ras Ha G12R) to evaluate the role of these oncogenes in the immune TME. Results In this model, orthotopic grafting of wildtype syngeneic keratinocytes expressing both v-ras Ha and elevated levels of ΔNp63α consistently yield carcinomas in syngeneic hosts, while cells expressing v-ras Ha alone yield predominantly papillomas. We found that polymorphonuclear (PMN) myeloid cells, experimentally validated to be immunosuppressive and thus representing myeloid-derived suppressor cells (PMN-MDSCs), were significantly recruited into the TME of carcinomas arising early following orthotopic grafting of ΔNp63α/v-ras Ha -expressing keratinocytes. ΔNp63α/v-ras Ha -driven carcinomas expressed higher levels of chemokines implicated in recruitment of MDSCs compared to v-ras Ha -initiated tumors, providing a heretofore undescribed link between ΔNp63α/HRAS-driven carcinomas and the development of an immunosuppressive TME. Conclusion These results support the utilization of a genetic carcinogenesis model harboring specific genomic drivers of malignancy to study mechanisms underlying the development of local immunosuppression.
Ten of the proteinogenic amino acids can be generated abiotically while the remaining thirteen require biology for their synthesis. Paradoxically, the biosynthesis pathways observed in nature require enzymes that are made with the amino acids they produce. For example, Escherichia coli produces cysteine from serine via two enzymes that contain cysteine. Here, we substituted alternate amino acids for cysteine and also methionine, which is biosynthesized from cysteine, in serine acetyl transferase (CysE) and O-acetylserine sulfhydrylase (CysM). CysE function was rescued by cysteine-and-methionine-free enzymes and CysM function was rescued by cysteine-free enzymes. Structural modeling suggests that methionine stabilizes CysM and is present in the active site of CysM. Cysteine is not conserved among CysE and CysM protein orthologs, suggesting that cysteine is not functionally important for its own synthesis. Engineering biosynthetic enzymes that lack the amino acids being synthesized provides insights into the evolution of amino acid biosynthesis and pathways for bioengineering.
The X-ray astronomy satellite ASTRO-H are equipped with two equivalent soft X-ray telescopes (SXT-I and SXT-S) which cover the energy band 0.3-12 keV. The X-ray reflectors of the SXTs are coated with a gold monolayer by means of the replication technique. A series of gold M absorption edges in the 2-4 keV band causes complex structures in the energy response of the SXTs. In the same band, there are astrophysically important emission lines from Si, Ar and S. Since the SXS has unprecedentedly high spectral resolution, we have measured the reflectivity around the gold M-edges in an extremely fine energy pitch at the synchrotron radiation facility KEK PF BL11-B, with the 2 eV pitch in 2100 eV to 4100 eV band that covers the entire series of the absorption edges (M-I through M-V) at grazing incident angles to the reflectors of 0.5, 0.8, 1.0, 1.2, 1.4 degree, and with a finer pitch of 0.25 eV in the 2200 eV to 2350 eV band where the two deepest M-IV and M-V edges are included. In the resultant reflectivity curves, we have clearly identified the fine structures associated with all the M-edges. Using these data, we calculated atomic scattering factor f1 as a function of X-ray energy, with which we have built the mirror response function which can be applied to the Suzaku spectra. As a result, we have found that discrepancy of the spectral model to the Suzaku data of 4U1630-472 (a black hole transient) and the Crab nebula around the M-edges are significantly reduced from those with the official Suzaku response.
ASTRO-H (Hitomi) is a Japanese X-ray astrophysics satellite just launched in February, 2016, from Tanegashima, Japan by a JAXA's H-IIA launch vehicle. It has two Soft X-ray Telescopes (SXTs), among other instruments, that were developed by the NASA Goddard Space Flight Center in collaboration with ISAS/JAXA and Nagoya University. One is for an X-ray micro-calorimeter instrument (Soft X-ray Spectrometer, SXS) and the other for an X-ray CCD camera (Soft X-ray Imager, SXI), both covering the X-ray energy band up to 15 keV. The two SXTs were fully characterized at the 30-m X-ray beam line at ISAS/JAXA. The combined SXT+SXS system effective area is about 250 and 300 cm(exp 2) at 1 and 6 keV, respectively, although observations were performed with the gate valve at the dewar entrance closed, which blocks most of low energy X-rays and some of high energy ones. The angular resolution for SXS is 1.2 arcmin (Half Power Diameter, HPD). The combined SXT+SXI system effective area is about 370 and 350 cm (exp 2) at 1 and 6 keV, respectively. The angular resolution for SXI is 1.3 arcmin (HPD). The both SXTs have a field of view of about 16 arcmin (FWHM of their vignetting functions).The SXT+SXS field of view is limited to 3 x 3 arcmin by the SXS array size. In-flight data available to the SXT team was limited at the time of this conference and a point-like source data is not available for the SXT+SXS. Although due to lack of attitude information we were unable to reconstruct a point spread function of SXT+SXI, according to RXJ1856.5-3754 data, the SXT seems to be working as expected in terms of imaging capability. As for the overall effective area response for both SXT+SXS and SXT+SXI, consistent spectral model fitting parameters with the previous measurements were obtained for Crab and G21.5-0.9 data. On the other hand, their 2-10 keV fluxes differ by about 20% at this point. Calibration work is still under progress. The SXT is the latest version of the aluminum foil X-ray mirror, which is extremely light-weight and very low cost, yet produces large effective area over a wide energy-band. Its area-mass ratio is the largest, 16 cm(exp 2)/kg, among ASTRO-H, Chandra, and XMM-Newton mirrors. The aluminum foil mirror is a still compelling technology depending on the mission science goal.
The X-ray astronomy satellite ASTRO-H, which is the 6th Japanese X-ray astronomy satellite and is renamed Hitomi after launch, is designed to observe celestial X-ray objects in a wide energy band from a few hundred eV to 600 keV. The Soft X-ray Telescopes (SXTs) onboard ASTRO-H play a role of collecting and imaging X-rays up to approximately 12 keV. Although the field of view of the SXT is approximately 15' (FWHM), due to the thin-foil-nested Wolter-I type optics adopted in the SXTs, X-rays out of the field of view can reach the focal plane without experiencing a normal double reflection. This component is referred to as 'stray light'. Owing to investigation of the stray light so far, 'secondary reflection' is now identified as the main component of the stray light, which is composed of X-rays reflected only by secondary reflectors. In order to cut the secondary reflections, a 'pre-collimator' is equipped on top of the SXTs. However, we cannot cut all the stray lights with the pre-collimator in some off-axis angle domain. In this study, we measure the brightness of the stray light of the SXTs at some representative off-axis angles by using the ISAS X-ray beam line. ASTRO-H is equipped with two modules of the SXT; one is for the Soft X-ray Spectrometer (SXS), an X-ray calorimeter, and the other is for the Soft X-ray Imager (SXI), an X-ray CCD camera. These SXT modules are called SXT-S and SXT-I, respectively. Of the two detector systems, the SXI has a large field of view, a square with 38' on a side. To cope with this, we have made a mosaic mapping of the stray light at a representative off-axis angle of 30' in the X-ray beam line at the Institute of Space and Astronautical Science. The effective area of the brightest secondary reflection is found of order approximately 0.1% of the on-axis effective area at the energy of 1.49 keV. The other components are not so bright (less than 5 x 10(exp -4) times smaller than the on-axis effective area). On the other hand, we have found that the effective area of the stray light in the SXS field of view (approximately 3' x 3') at large off-axis angles (greater than 15') are approximately 1(exp -4) times smaller than the on-axis effective area (approximately 590 sq cm at 1.49 keV).
ASTRO-H (Hitomi) satellite equips two Soft X-ray Telescopes (SXTs), one of which (SXT-S) is coupled to Soft-X-ray Spectrometer (SXS) while the other (SXT-I) is coupled to Soft X-ray Imager (SXI). Although SXTs are lightweight of approximately 42 kgmodule1 and have large on-axis effective area (EA) of approximately 450 cm(exp 2) at 4.5 keV module(sub 1) by themselves, their angular resolutions are moderate approximately 1.2 arcmin in half power diameter. The amount of contamination into the SXS FOV (3.05 times 3.05 arcmin(exp 2) from nearby sources was measured in the ground-based calibration at the beamline in Institute of Space and Astronautical Science. The contamination at 4.5 keV were measured with sources distant from the SXS center by one width of the FOV in perpendicular and diagonal directions, that is, 3 and 4.5 arcmin-off, respectively. The average EA of the contamination in the four directions with the 3 and 4.5 arcmin-off were measured to be 2 and 0.6% of the on-axis EA of 412 cm (exp) for the SXS FOV, respectively. The contamination from a source distant by two FOV widths in a diagonal direction, that is, 8.6 arcmin-off was measured to be 0.1% of the on-axis at 4.5 keV. The contamination amounts were also measured at 1.5 keV and 8.0 keV which indicated that the ratio of the contamination EA to that of on-axis hardly depended on the source energy. The off-axis SXT-I images from 4.5 to 27 arcmin were acquired at intervals of -4.5 arcmin for the SXI FOV of 38 times 38 arcmin(exp 2). The image shrinked as the off-axis angle increased. Above 13.5 arcmin of off-angle, a stray appeared around the image center in the off-axis direction. As for the on-axis image, a ring-shaped stray appeared at the edge of SXI of approximately 18 arcmin distant from the image center.
The international x-ray observatory ASTRO-H was renamed Hitomi after launch. It covers a wide energy range from a few hundred eV to 600 keV. It is equipped with two soft x-ray telescopes (SXTs: SXT-I and SXT-S) for imaging the soft x-ray sky up to 12 keV, which focus an image onto the respective focal-plane detectors: CCD camera (SXI) and a calorimeter (SXS). The SXTs are fabricated in a quadrant unit. The angular resolution in half-power diameter (HPD) of each quadrant of the SXTs ranges between 1.1 and 1.4 arc min at 4.51 keV. It was also found that one quadrant has an energy dependence on the HPD. We examine the angular resolution with spot scan measurements. In order to understand the cause of imaging capability deterioration and to reflect it to the future telescope development, we carried out spot scan measurements, in which we illuminate all over the aperture of each quadrant with a square beam 8 mm on a side. Based on the scan results, we made maps of image blurring and a focus position. The former and the latter reflect figure error and positioning error, respectively, of the foils that are within the incident 8 mm x 8 mm beam. As a result, we estimated those errors in a quadrant to be approx. 0.9 to 1.0 and approx. 0.6 to 0.9 arc min, respectively. We found that the larger the positioning error in a quadrant is, the larger its HPD is. The HPD map, which manifests the local image blurring, is very similar from quadrant to quadrant, but the map of the focus position is different from location to location in each telescope. It is also found that the difference in local performance causes energy dependence of the HPD.
Reliable results when fitting X-ray data require proper consideration of the statistics involved. We probe the impact of Gaussian versus Poisson statistics at low count levels using both the standard χ^(2) method and maximum likelihood based on Poisson (C) statistics. The difference is studied and quantified through simulated spectra with known properties. We then test the results through analysis of Mn Kα calibration data taken with the flight spare microcalorimeter for the Hitomi soft X-ray spectrometer. Through comparison with simulations, our results show that the χ^(2) method tends to give overly optimistic estimates of the detector energy resolution, in particular when there are few counts. Given an energy resolution of ∼5 eV and a line with about 100 photons, the line width becomes ∼10% lower in the χ^(2) method than in Poisson statistics. This is a consequence of the uncertainties being dominated by counting statistics, and therefore highlights the need to choose the appropriate fit statistic.