We present sample transfer instrumentation and integrated protocols for the preparation and atom probe characterization of environmentally-sensitive materials. Ultra-high vacuum cryogenic suitcases ...allow specimen transfer between preparation, processing and several imaging platforms without exposure to atmospheric contamination. For expedient transfers, we installed a fast-docking station equipped with a cryogenic pump upon three systems; two atom probes, a scanning electron microscope / Xe-plasma focused ion beam and a N2-atmosphere glovebox. We also installed a plasma FIB with a solid-state cooling stage to reduce beam damage and contamination, through reducing chemical activity and with the cryogenic components as passive cryogenic traps. We demonstrate the efficacy of the new laboratory protocols by the successful preparation and transfer of two highly contamination- and temperature-sensitive samples-water and ice. Analysing pure magnesium atom probe data, we show that surface oxidation can be effectively suppressed using an entirely cryogenic protocol (during specimen preparation and during transfer). Starting with the cryogenically-cooled plasma FIB, we also prepared and transferred frozen ice samples while avoiding significant melting or sublimation, suggesting that we may be able to measure the nanostructure of other normally-liquid or soft materials. Isolated cryogenic protocols within the N2 glove box demonstrate the absence of ice condensation suggesting that environmental control can commence from fabrication until atom probe analysis.
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DOBA, IZUM, KILJ, NUK, PILJ, PNG, SAZU, SIK, UILJ, UKNU, UL, UM, UPUK
To determine long-term clinical outcomes in survivors of severe acute respiratory syndrome (SARS) and Middle East respiratory syndrome (MERS) coronavirus infections after hospitalization or intensive ...care unit admission.
Ovid MEDLINE, EMBASE, CINAHL Plus, and PsycINFO were searched.
Original studies reporting clinical outcomes of adult SARS and MERS survivors 3 months after admission or 2 months after discharge were included.
Studies were graded using the Oxford Centre for Evidence-Based Medicine 2009 Level of Evidence Tool. Meta-analysis was used to derive pooled estimates for prevalence/severity of outcomes up to 6 months after hospital discharge, and beyond 6 months after discharge.
Of 1,169 identified studies, 28 were included in the analysis. Pooled analysis revealed that common complications up to 6 months after discharge were: impaired diffusing capacity for carbon monoxide (prevalence 27%, 95% confidence interval (CI) 15–45%); and reduced exercise capacity (mean 6-min walking distance 461 m, CI 450–473 m). The prevalences of post-traumatic stress disorder (39%, 95% CI 31–47%), depression (33%, 95% CI 20–50%) and anxiety (30%, 95% CI 10–61) beyond 6 months after discharge were considerable. Low scores on Short-Form 36 were identified beyond 6 months after discharge.
Lung function abnormalities, psychological impairment and reduced exercise capacity were common in SARS and MERS survivors. Clinicians should anticipate and investigate similar long-term outcomes in COVID-19 survivors.
•Al, Ni and Zr alloys used to compare Cameca Invizo 6000 atom probe to LEAPs.•Field-of-view, mass resolving power, sample yield are greater on Invizo 6000.•Routine analysis of metal-oxide interfaces ...demonstrated.
The CAMECA Invizo 6000 atom probe microscope uses ion optics that differ significantly from the local electrode atom probe (LEAP). It uses dual antiparallel deep ultraviolet lasers, a flat counter electrode, and a series of accelerating and decelerating lenses to increase the field-of-view of the specimen without reducing the mass resolving power. In this work we characterise the performance of the Invizo 6000 using three material case studies: a model Al-Mg-Si alloy, a commercially-available Ni-based superalloy, and a Zr alloy, using a combination of air and vacuum-transfer between instruments. The ion optics of the Invizo 6000 significantly increase the field-of-view compared to the same specimen on a LEAP 4000 X Si. We also observe a significant increase in specimen yield, especially for the Zr alloy. These results combine to make the Invizo 6000 well-suited to research projects requiring large analysis volumes, particularly so for traditionally difficult samples such as oxides.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UILJ, UL, UM, UPUK, ZAGLJ, ZRSKP
Analysis and understanding of the role of hydrogen in metals is a significant challenge for the future of materials science, and this is a clear objective of recent work in the atom probe tomography ...(APT) community. Isotopic marking by deuteration has often been proposed as the preferred route to enable quantification of hydrogen by APT. Zircaloy-4 was charged electrochemically with hydrogen and deuterium under the same conditions to form large hydrides and deuterides. Our results from a Zr hydride and a Zr deuteride highlight the challenges associated with accurate quantification of hydrogen and deuterium, in particular associated with the overlap of peaks at a low mass-to-charge ratio and of hydrogen/deuterium containing molecular ions. We discuss possible ways to ensure that appropriate information is extracted from APT analysis of hydrogen in zirconium alloy systems that are important for nuclear power applications.
•Reconstruction method for APT requiring information from only a single crystallographic pole•Accounts for dynamic variations in reconstruction parameters•Single pole crystallography mediated ...reconstruction protocol is largely automated
Spatially accurate atom probe tomography reconstructions are vitally important when quantitative spatial measurements such as distances, volumes and morphologies etc. of nanostructural features are required information for the researcher. It is well known that the crystallographic information contained within the atom probe data of crystalline materials can be used to calibrate the tomographic reconstruction. Specifically, the crystallographic information projected into the field evaporation images is used. This offers a powerful and accurate enhancement of the atom probe technique. However, this is often difficult to do in practice. In previously reported approaches, it was necessary to index at least two poles to compute the image compression factor ‘ξ’ and observe crystallographic planes in at least one of the pole regions to obtain a measure of the field factor ‘kf’ while also manually accounting for a change in reconstruction parameters throughout the dataset. Not only is this error-prone and time consuming, it does not work for materials that exhibit limited crystallographic information in their field evaporation image. Here, we extend the applicability of the crystallographic calibration of atom probe data by proposing a reconstruction methodology where only one pole with observable lattice planes is required in the projected detector image. Our proposal also accounts for dynamic variations in the reconstruction parameters throughout the 3D dataset. The method is simpler and significantly faster to implement and is applicable to more atom probe situations than previously approaches. Our single-pole crystallography mediated reconstruction (SP-CMR) utilizes the Hawkes-Kasper projection model (equivalent to the equidistant-azimuthal projection model) and the direct fourier (DF) fit algorithm to determine the precise reconstruction parameters required to produce flat atomic planes. It is applied to experimental Al and highly Sb-doped Si data. The discrepancies between the spatial dimensions of the SP-CMR reconstructions compared to uncalibrated reconstructions are visually apparent. Consistent plane spacings and angles between crystallographic directions matching the theoretically known values for each crystal structure are demonstrated.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPUK, ZRSKP
The large fraction of material residing at grain boundaries in nanocrystalline metals and alloys is responsible for their ultrahigh strength, but also undesirable microstructural instability under ...thermal and mechanical loads. However, the underlying mechanism of stress-driven microstructural evolution is still poorly understood and precludes rational alloy design. Here we combine quantitative in situ electron microscopy with three-dimensional atom-probe tomography to directly link the mechanics and kinetics of grain boundary migration in nanocrystalline Al films with the excess of O atoms at the boundaries. Site-specific nanoindentation leads to grain growth that is retarded by impurities, and enables quantification of the critical stress for the onset of grain boundary migration. Our results show that a critical excess of impurities is required to stabilize interfaces in nanocrystalline materials against mechanical driving forces, providing new insights to guide control of deformation mechanisms and tailoring of mechanical properties apart from grain size alone.
Silicon nanocrystals (Si NCs) are intensively studied for optoelectronic and biological applications due to having highly attractive features such as band engineering. Although doping is often used ...to control the optical and electrical properties, the related structural properties of solely doped and codoped Si NCs are not well-understood. In this study, we report the boron (B) and/or phosphorus (P) distribution in Si NCs embedded in borosilicate glass (BSG), phosphosilicate glass (PSG), and borophosphosilicate glass (BPSG) using atom probe tomography (APT). We compared solely and codoped Si NCs grown at different temperatures so that we may compare the effects of codoping and temperature on the B and/or P distribution. Proximity histograms and cluster analyses reveal that there exist boron-rich layers surrounding Si NCs and also B–P clusters within the Si NCs. Raman spectra also show a structural change between codoped Si NCs in solids and free-standing codoped Si NCs. These results lead us to understand that codoped Si NCs disperse in polar solvents.
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IJS, KILJ, NUK, PNG, UL, UM
Microscopy encompasses a wide variety of forms and scales. So too does the array of simulation techniques developed that correlate to and build upon microstructural information. Nevertheless, a true ...nexus between microscopy and atomistic simulations is lacking. Atom probe has emerged as a potential means of achieving this goal. Atom probe generates three-dimensional atomistic images in a format almost identical to many atomistic simulations. However, this data is imperfect, preventing input into computational algorithms to predict material properties. Here we describe a methodology to overcome these limitations, based on a hybrid data format, blending atom probe and predictive Monte Carlo simulations. We create atomically complete and lattice-bound models of material specimens. This hybrid data can then be used as direct input into density functional theory simulations to calculate local energetics and elastic properties. This research demonstrates the role that atom probe combined with theoretical approaches can play in modern materials engineering.
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Atom probe tomography is known for its accurate compositional analysis at the nanoscale. However, the patterns created by successive hits on the single particle detector during ...experiments often contain complementary information about the specimen’s crystallography, including structure and orientation. This information remains in most cases unexploited because it is, up to now, retrieved predominantly manually. Here, we propose an approach combining image analysis techniques for feature selection and deep-learning to automatically interpret the patterns. Application of unsupervised machine learning techniques allows to build and train a deep neural network, based on a library generated from theoretically known crystallographic angular relationships. This approach enables direct interpretation of the detector hit maps, as shown here on the example of numerous pure-Al, and is robust enough to function under various conditions of base temperature, pulsing mode and pulse fraction. We benchmark our approach against recent attempts to automate the pattern identification via Hough-transform and discuss the current limitations of our approach. This new automated approach renders crystallographic atom probe tomography analysis more efficient, feature-sensitive, robust, user-independent and reliable. With that, deep-learning algorithms show a great potential to give access to combined atom probe crystallographic and compositional analysis to a large community of users.
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GEOZS, IJS, IMTLJ, KILJ, KISLJ, NLZOH, NUK, OILJ, PNG, SAZU, SBCE, SBJE, UL, UM, UPUK, ZRSKP
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