The segregation of reactive elements (REs) along thermally grown oxide (TGO) grain boundaries has been associated to slower oxide growth kinetics and improved creep properties. However, the incorporation and diffusion of these elements into the TGO during oxidation of Ni alloys remains an open question. In this work, electron backscatter diffraction in transmission mode (t-EBSD) was used to investigate the microstructure of TGO within the thermal barrier coating on a Ni-based superalloy, and atom probe tomography (APT) was used to quantify the segregation behavior of REs to α-Al2O3 grain boundaries. Integrating the two techniques enables a higher level of site-specific analysis compared to the routine focused ion beam lift-out sample preparation method without t-EBSD. Needle-shaped APT specimens readily meet the thickness criterion for electron diffraction analysis. Transmission EBSD provides an immediate feedback on grain orientation and grain boundary location within the APT specimens to help target grain boundaries in the TGO. Segregation behavior of REs is discussed in terms of the grain boundary character and relative location in TGO.

Tumors have posed a serious threat to human life and health. Researchers can determine whether or not cells are cancerous, whether the cancer cells are invasive or metastatic, and what the effects of drugs are on cancer cells by the physical properties such as hardness, adhesion, and Young's modulus. The atomic force microscope (AFM) has emerged as a key important tool for biomechanics research on tumor cells due to its ability to image and collect force spectroscopy information of biological samples with nano-level spatial resolution and under near-physiological conditions. This article reviews the existing results of the study of cancer cells with AFM. The main foci are the operating principle of AFM and research advances in mechanical property measurement, ultra-microtopography, and molecular recognition of tumor cells, which allows us to outline what we do know it in a systematic way and to summarize and to discuss future directions.

Carbon-supported nanoparticles have been used widely as efficient catalysts due to their enhanced surface-to-volume ratio. To investigate their structure–property relationships, acquiring 3D elemental distribution is required. Here, carbon-supported Pt, PtMn alloy, and ordered Pt3Mn nanoparticles are synthesized and analyzed with atom probe tomography as model systems. A significant difference of Mn distribution after the heat-treatment was found. Finally, the field evaporation behavior of the carbon support was discussed and each acquired reconstruction was compared with computational results from an evaporation simulation. This paper provides a guideline for studies using atom probe tomography on the heterogeneous carbon-supported nanoparticle system that leads to insights toward a wide variety of applications.

Obsidian is volcanic glass that results from the rapid cooling of silica-rich melt. Nanoscale crystallites precipitate out of the melt prior to solidification and remain embedded in the amorphous matrix. These crystallites provide information on the flow kinetics and composition of the melt. Due to the sparsity and size of nanolites, studies often focus on supramicron crystallites. This research takes advantage of the conchoidal fracture of obsidian by knapping samples with nanometer-thin edges for transmission electron microscopy characterization. Nanolites in the amorphous matrix are studied using energy-dispersive spectroscopy (EDS) and electron diffraction. Certain alkali and alkaline-earth cations exhibit patterns of depletion near Fe-oxide nanolites. EDS is used to identify nanolites and variations in the composition of the matrix. Parallel beam diffraction and radial distribution function analysis of nearest-neighbor distances determine average bond lengths in the matrix near nanolites, showing that nanolites influence the nearby short-range ordering and atomic character of the matrix. Analysis reveals decreased mean nearest-neighbor distances in the matrix adjacent to nanolites compared to the bulk. Our methods exhibit the required sensitivity to detect variations in the composition and structure near nanolites, and our findings indicate that obsidian nanolites contribute to quantifiable localized changes in the amorphous structure.

Atom probe tomography was employed to observe and derive the composition of carbon clusters in implanted silicon. This value, which is of interest to the microelectronic industry when considering ion implantation defects, was estimated not to exceed 2 at%. This measurement has been done by fitting the distribution of first nearest neighbor distances between monoatomic carbon ions (C+ and C2+). Carbon quantification has been considerably improved through the detection of molecular ions, using lower electric field conditions as well as equal proportions of 12C and 13C. In these conditions and using another quantification method, we have shown that the carbon content in clusters approaches 50 at%. This result very likely indicates that clusters are nuclei of the SiC phase.

The local field ion emission properties of helium and neon around a step edge atom of W(112) were examined at liquid nitrogen temperature using a micro-probe hole field ion microscope combined with a pulse-counting analysis. We have analyzed the mapped field ion densities obtained for both imaging gas atoms at their respective best local image voltages based on the formula for tunneling barrier strength and have evaluated the dipole moment of polarized adatom as well as the local field enhancement factor at the adatom site. We found that the dipole moments of helium and neon adatoms showed the same value, although the best local image field acting on the helium adatom is much higher than that on the neon adatom. We also found the same magnitude of local field enhancement factors for both noble gas field adsorptions. These results imply that the key to the best local image condition is the tunneling barrier field variations above the adatom. The vital role of the imaging gas atoms is to form an optimum dipole moment to create an ideal electric field distribution for the best local image appearance at each atom site depending on the different chemical nature of adatom species.

In this work, the technique and the pictorial materials employed by Claude Monet in Pink Water Lilies, presently housed at the National Gallery of Modern and Contemporary Art in Rome, were investigated. The painting underwent noninvasive investigations such as energy-dispersive X-ray fluorescence and visible reflectance spectroscopies. The combined use of these techniques allowed us to identify most of the inorganic pigments such as cobalt blue and violet, zinc oxide, cadmium yellow, vermilion, and mixtures. Particularly, the spectrophotometric curves allow for the detection of the anhydrous and hydrated chromium greens. Two micro-fragments of the painting were also examined with micro-Fourier transform infrared spectroscopy and the cross-sections obtained were analyzed with the optical microscope and with scanning electron microscopy (SEM) and energy-dispersive X-ray spectrometry (EDS). Fourier Transform Infrared spectroscopy analyses allowed us to recognize the animal glue used for priming the canvas, which was covered with a ground layer consisting of calcite and lead white mixed with an oil binder. A lipidic binder was also detected in the color layer. Optical microscopy and SEM-EDS were useful to retrieve information about the stratigraphy, the distribution of pigments, and a more complete palette identification of phosphate, arsenate, and magnesium arsenate cobalt violets, and the red lake was possible.

Nanocrystalline oxides are mainly responsible for Ni-base oxide dispersion strengthened (ODS) superalloys excellent thermo-mechanical properties. To establish the microstructural correlations between the metallic matrix and various oxide dispersoids, we report here the atomic-scale structure and chemistry of the complex nano-oxide dispersoids. Ultrahigh-resolution Cs-aberration-corrected scanning transmission electron microscopy (STEM) based techniques have been used to resolve nano-dispersoids in the Alloy 617 ODS. These nano-oxides, interestingly, possess a variety of high-angle annular dark-field (HAADF) contrasts, that is, bright, dark, and bi-phases. Both the light and heavy atoms have been found to be present in Y–Al–O complex-oxide nanostructures in varying quantities and forming a characteristic interface with the metallic matrix. In overcoming the limitation of conventional STEM-HAADF imaging, the integrated differential phase-contrast imaging technique was employed to investigate the oxygen atoms along with other elements in the dispersoids and its interface with the matrix. The most intriguing aspect of the study is the discovery of a few atoms thick Al2O3 interlayer (shell) around a monoclinic Y–Al–O core in the Ni-matrix. On the other hand, when the dispersoid is a hexagonal type Y–Al–O complex, the interface energy is already low, maintaining a semi-coherent interface and it was devoid of a shell.

Indium (In) and other low melting point metals are used as interconnects in a variety of hybridized circuits and a full understanding of the metallurgy of these interconnects is important to the reliability and performance of the devices. This paper shows that room temperature focused ion beam (FIB) preparation of cross-sections, using Ga+ or Xe+ can result in artifacts that obscure the true In microbump structure. The use of modified milling strategies to minimize the increased local sample temperature are shown to produce cross-sections that are representative of the In bump microstructure in some sample configurations. Furthermore, cooling of the sample to cryogenic temperatures is shown to reliably eliminate artifacts in FIB prepared cross-sections of In bumps allowing the true bump microstructure to be observed.

The effect of sample preparation on a pre-aged Al–Mg–Si–Cu alloy has been evaluated using atom probe tomography. Three methods of preparation were investigated: electropolishing (control), Ga+ focused ion beam (FIB) milling, and Xe+ plasma FIB (PFIB) milling. Ga+-based FIB preparation was shown to introduce significant amount of Ga contamination throughout the reconstructed sample (≈1.3 at%), while no Xe contamination was detected in the PFIB-prepared sample. Nevertheless, a significantly higher cluster density was observed in the Xe+ PFIB-prepared sample (≈25.0 × 1023 m−3) as compared to the traditionally produced electropolished sample (≈3.2 × 1023 m−3) and the Ga+ FIB sample (≈5.6 × 1023 m−3). Hence, the absence of the ion milling species does not necessarily mean an absence of specimen preparation defects. Specifically, the FIB and PFIB-prepared samples had more Si-rich clusters as compared to electropolished samples, which is indicative of vacancy stabilization via solute clustering.

Plasma focused ion beam microscopy (PFIB) is a recent nanofabrication technique that is suitable for site-specific atom probe sample preparation. Higher milling rates and fewer artifacts make it superior to Ga+ FIBs for the preparation of samples where large volumes of material must be removed, for example, when trying to avoid lift-out techniques. Transmission Kikuchi diffraction (TKD) is a method that has facilitated phase identification and crystallographic measurements in such electron transparent samples. We propose a procedure for preparing atom probe tomography (APT) tips from mechanically prepared ribbons by using PFIB. This is highly suitable for the preparation of atom probe tips of interfaces such as interphase boundaries from challenging materials where lift-out tips easily fracture. Our method, in combination with TKD, allows the positioning of regions of interest such as interfaces close to the apex of the tip. We showcase the efficacy of the proposed method in a case study on Alloy 718, where the interface between γ-matrix and δ-phase has not been yet extensively explored through APT due to preparation challenges. Results show depletion of γ″-precipitates near the γ/δ interface. A quantitative evaluation of the composition of phases in the bulk versus near the interface is achieved.

The nitrogen deficiency in steels measured by atom probe tomography (APT) is considered to arise from the obscurement of singly charged dimer nitrogen ions (N2+) by the iron-dominant peak (56Fe2+) at 28 Da. To verify this by quantifying the amount of N2+ ions, γ′-Fe4N consisting of the 15N isotope was prepared on iron substrates by plasma nitriding using a nitrogen isotopic gas (15N2). Although considerable amounts of 15N2+ were observed at 30 Da without overlap with any iron peak, the observed nitrogen concentrations of γ′-Fe4N were clearly lower than the stoichiometric composition (19–20 at%), using both pulsed voltage and pulsed laser atom probes. The origin of the missing nitrogen, excluding nitrogen obscured by other ion species, was predicted to be the occurrence of neutral nitrogen or nitrogen gas molecules in field evaporation. The generation rate of iron nitride ions (FeN2+) for 15N was significantly lower than that for 14N in γ′-Fe4N, which affected the amount of the missing nitrogen. The isotope effect suggests that the isotopic ratio cannot always be determined from only one ion species among the multiple species observed in the APT analysis. We discuss the mechanism of the isotope effect in FeN2+ formation by field evaporation.

The integrated differential phase contrast (IDPC) method is useful for generating the potential map of a thin sample. We evaluate theoretically the potential of IDPC imaging for thick samples by varying the focus at different sample thicknesses. Our calculations show that high defocus values result in enhanced anisotropy of the contrast transfer function (CTF) and uninterpretable images, if a quadrant detector is applied. We further show that applying a multi-sector detector can result in an almost isotropic CTF. By sector number-dependent calculations for both Cc/C3-corrected and C3-corrected scanning transmission electron microscopy (STEM), we show that the increase of detector sectors not only removes the anisotropy of the CTF, but also improves image contrast and resolution. For a proof-of-principle IDPC-STEM (uncorrected) experiment, we realize the functionality of a 12-sector detector from a physical quadrant detector and demonstrate the improvement in contrast and resolution on the example of InGaN/GaN quantum well structure.

The impact of secondary fluorescence on the material compositions measured by X-ray analysis for layered semiconductor thin films is assessed using simulations performed by the DTSA-II and CalcZAF software tools. Three technologically important examples are investigated: AlxGa1−xN layers on either GaN or AlN substrates, InxAl1−xN on GaN, and Si-doped (SnxGa1−x)2O3 on Si. Trends in the differences caused by secondary fluorescence are explained in terms of the propensity of different elements to reabsorb either characteristic or bremsstrahlung X-rays and then to re-emit the characteristic X-rays used to determine composition of the layer under investigation. Under typical beam conditions (7–12 keV), the quantification of dopants/trace elements is found to be susceptible to secondary fluorescence and care must be taken to prevent erroneous results. The overall impact on major constituents is shown to be very small with a change of approximately 0.07 molar cation percent for Al0.3Ga0.7N/AlN layers and a maximum change of 0.08 at% in the Si content of (SnxGa1−x)2O3/Si layers. This provides confidence that previously reported wavelength-dispersive X-ray compositions are not compromised by secondary fluorescence.

Electron probe microanalysis (EPMA) is based on physical relations between measured X-ray intensities of characteristic lines and their X-ray production efficiency, which depends on the specimen composition. The quality of the analysis results relies on how realistically the physical relations describe the generation and emission of X-rays. Special experiments are necessary to measure X-ray production efficiencies. A challenge in these experiments is the determination of the detection efficiency of the spectrometer as a function of the photon energy. An energy-dispersive spectrometer was used in this work, for which the efficiency was determined at metrological synchrotron beamlines with an accuracy of ±2%. X-ray production efficiencies for the L series and the Kα series of copper and zirconium and for the M and L series of tungsten were determined at energies up to 30 keV in a scanning electron microscope. These experimental values were compared with calculated X-ray production efficiencies using physical relations and material constants applied in EPMA. The objective of the comparison is the further improvement of EPMA algorithms as well as extending the available database for X-ray production efficiencies. Experimental data for the X-ray production efficiency are also useful for the assessment of spectrum simulation software.