The formation of copper-rich precipitates of 17-4 precipitate hardened stainless steel has been investigated, after tempering at 350–570°C for 4 h, by atom probe tomography (APT). The results reveal that the clusters, enriched only with Cu, were observed after tempering at 420°C. Segregation of Ni, Mn to the Cu-rich clusters took place at 450°C, contributing to the increased hardening. After tempering at 510°C, Ni and Mn were rejected from Cu-rich precipitates and accumulated at the precipitate/matrix interfaces. Al and Si were present and uniformly distributed in the precipitates that were <1.5 nm in radius, but Ni, Mn, Al, and Si were enriched at the interfaces of larger precipitates/matrix. The proxigram profiles of the Cu-rich precipitates formed at 570°C indicated that Ni, Mn, Al, and Si segregated to the precipitate/matrix interfaces to form a Ni(Fe, Mn, Si, Al) shell, which significantly reduced the interfacial energy as the precipitates grew into an elongated shape. In addition, the number density of Cu-rich precipitates was increased with the temperature elevated from 350 up to 450°C and subsequently decreased at higher temperatures. Also, the composition of the matrix and the precipitates were measured and found to vary with temperature.

Diffuse rings from amorphous materials sit on a steep background resulting in a monotonically decreasing intensity over scattering vector length, frequently with no clear local maximum that could be used to determine the center of the ring. The novelty of the method reported here is that it successful processes such weak patterns. It is based on separating the angular dependence of the positions of the maxima on the azimuthal angle in the measured two-dimensional pattern for a manually preselected peak. Both pattern center and elliptical distortion are simultaneously refined from this angular dependence. Both steps are based on nonlinear least square fitting, using the Levenberg–Marquardt method. It can be successfully applied to any amorphous patterns provided they were recorded with experimental conditions that facilitate dividing them into sectors with acceptable statistics. Patterns with the center shifted to the camera corner (recording a quadrant of a ring) can also be reliably evaluated, keeping precalibrated values of the elliptical distortion fixed during the fit. Finally, the limited number of counts in any pattern is overcome by cumulating many patterns (from equivalent areas) into a single pattern. Eliminating false effects is facilitated by masking out unwanted parts of any recorded pattern from processing.

This letter describes an innovative spin-coating system, built from off-the-shelf components, that can easily and inexpensively be integrated into any laboratory environment. Combined with a liquid suspension of conductive polymer, such a “rotary coater” enables simple coating of planar samples to create a physical protective barrier on the sample surface. This barrier aids in charge dissipation during scanning electron microscope and focused ion beam (FIB) imaging and provides wide-scale protection of the sample surface from ion bombardment during FIB imaging and gas-assisted deposition. This polymer layer replaces the localized and time-consuming electron beam deposition step typically performed during transmission electron microscopy lamella preparation. After observation, the coating can be easily removed, if desired. The described spin-coating procedure has minimal cost while providing repeatable positive results, without the need for expensive commercial coating instrumentation.

We report a systematic spectroscopical investigation of three plagioclase particles (RB-QD04-0022, RA-QD02-0025-01, and RA-QD02-0025-02) returned by the Hayabusa spacecraft from the asteroid Itokawa, by means of scanning electron microscopy, cathodoluminescence microscopy/spectroscopy, and micro-Raman spectroscopy. The cathodoluminescence properties are used to evaluate the crystallization effects and the degree of space weathering processes, especially the shock-wave history of Itokawa. They provide new insights regarding spectral changes of asteroidal bodies due to space weathering processes. The cathodoluminescence spectra of the plagioclase particles from Itokawa show a defect-related broad band centered at around 450 nm, with a shoulder peak at 425 nm in the blue region, but there are no Mn- or Fe-related emission peaks. The absence of these crystal field-related activators indicates that the plagioclase was formed during thermal metamorphism at subsolidus temperature and extreme low oxygen fugacity. Luminescence characteristics of the selected samples do not show any signatures of the shock-induced microstructures or amorphization, indicating that these plagioclase samples suffered no (or low-shock pressure regime) shock metamorphism. Cathodoluminescence can play a key role as a powerful tool to determine mineralogy of fine-grained astromaterials.

We have used field emission scanning electron microscopy (FESEM) to study the high-resolution organization of cellulose microfibrils in onion epidermal cell walls. We frequently found that conventional “rule of thumb” conditions for imaging of biological samples did not yield high-resolution images of cellulose organization and often resulted in artifacts or distortions of cell wall structure. Here we detail our method of one-step fixation and dehydration with 100% ethanol, followed by critical point drying, ultrathin iridium (Ir) sputter coating (3 s), and FESEM imaging at a moderate accelerating voltage (10 kV) with an In-lens detector. We compare results obtained with our improved protocol with images obtained with samples processed by conventional aldehyde fixation, graded dehydration, sputter coating with Au, Au/Pd, or carbon, and low-voltage FESEM imaging. The results demonstrated that our protocol is simpler, causes little artifact, and is more suitable for high-resolution imaging of cell wall cellulose microfibrils whereas such imaging is very challenging by conventional methods.

The history and iconography of Swiss stained glass dating between the 16th and 18th centuries are well studied. However, the chemical and morphological characteristics of the glass and glass paints, particularly the nature of the raw materials, the provenance of the glass, and the technology used to produce it are less well understood. In this paper, we studied two sets of samples from stained-glass panels attributed to Switzerland, which date from the 16th to 17th centuries: the first set comes from Pena National Palace collection, the second from Vitrocentre Romont. The aims were to identify the materials used in the production of the glass, to find out more about their production origin and to characterize the glass paints. Both glass and the glass paints were analysed by particle-induced X-ray emission; the paints were additionally analysed by scanning electron microscopy–electron-dispersive X-ray spectroscopy (SEM-EDS). The results show that the glass from both sets was probably produced in the same region and that wood ash was used as a fluxing agent. Different recipes have been used to make the blue enamels. However, the cobalt ore used as a coloring agent in all of the blue enamels came from the mining district in Schneeberg, Germany.

Essentially all biological processes are highly dependent on the nanoscale architecture of the cellular components where these processes take place. Statistical measures, such as the autocorrelation function (ACF) of the three-dimensional (3D) mass–density distribution, are widely used to characterize cellular nanostructure. However, conventional methods of reconstruction of the deterministic 3D mass–density distribution, from which these statistical measures can be calculated, have been inadequate for thick biological structures, such as whole cells, due to the conflict between the need for nanoscale resolution and its inverse relationship with thickness after conventional tomographic reconstruction. To tackle the problem, we have developed a robust method to calculate the ACF of the 3D mass–density distribution without tomography. Assuming the biological mass distribution is isotropic, our method allows for accurate statistical characterization of the 3D mass–density distribution by ACF with two data sets: a single projection image by scanning transmission electron microscopy and a thickness map by atomic force microscopy. Here we present validation of the ACF reconstruction algorithm, as well as its application to calculate the statistics of the 3D distribution of mass–density in a region containing the nucleus of an entire mammalian cell. This method may provide important insights into architectural changes that accompany cellular processes.

The microstructural evolution of precipitation in two model alloys, Fe–NiAl and Fe–NiAl–Cu, was investigated during aging at 500°C for different times using atom probe tomography (APT). The APT results reveal that the addition of Cu effectively increases the number density of NiAl precipitates. This is attributed to Cu promoting the nucleation of NiAl particles by increasing the chemical driving force and decreasing the interfacial energy. The NiAl precipitates of the Fe–NiAl–Cu alloy grow and coarsen at a slower rate than that of the Fe–NiAl alloy, mainly due to the slower diffusion rate of the Cu atoms. The mechanical properties of the two alloys were characterized by Vickers hardness and tension tests. It was found that the addition of Cu results in the formation of core–shell precipitates with a Cu-rich core and a NiAl shell, leading to a dramatic improvement of peak hardness and strength. The effect of Cu on precipitation strengthening is discussed in terms of chemical strength and coherency strength.

The preparation of transmission electron microscopy (TEM) samples from powders is quite difficult and challenging. For powders with particles in the 1–5 μm size range, it is especially difficult to select an adequate sample preparation technique. Epoxy is commonly used to bind powder, but drawbacks, such as differential milling originating from unequal milling rates between the epoxy and powder, remain. We propose a new, simple method for preparing TEM samples. This method is especially useful for powders with particles in the 1–5 μm size range that are vulnerable to oxidation. The method uses solder as an embedding agent together with focused ion beam (FIB) milling. The powder was embedded in low-temperature solder using a conventional hot-mounting instrument. Subsequently, FIB was used to fabricate thin TEM samples via the lift-out technique. The solder proved to be more effective than epoxy in producing thin TEM samples with large areas. The problem of differential milling was mitigated, and the solder binder was more stable than epoxy under an electron beam. This methodology can be applied for preparing TEM samples from various powders that are either vulnerable to oxidation or composed of high atomic number elements.

Cytological responses in different organs of sentinel organisms have proven to be useful tools for characterizing the health status of those organisms and assessing the impact of environmental contaminants. Our study shows that nickel (II) accumulated in both germ cells (oogonia and developing oocytes) and somatic cells (muscle cells, follicle cells) in the Astacus leptodactylus ovary. Muscle cells from ovarian wall show disorganization and the disruption of cytoplasmic microtubules and pyknosis of the cell nucleus. Follicle cells, both those that surround the developing oocytes and also those that are not associated with the oocytes contained within the cytoplasm vacuoles of different sizes, degenerated mitochondria, myelin bodies, disorganized microtubules, and pyknotic nuclei. The most evident pathological phenomenon was the alteration and disorganization of the basal matrix, which separates the ovarian interstitium from ovarian follicles compartment. Exposure to nickel induces cytoplasmic vacuolation in oogonia and developing oocytes, structural alteration of the developing yolk granules and condensation of the nucleoli. Ultrastructural autometallography has shown grains of silver-enhanced nickel inside the cytoplasm of the muscle cells with altered morphology, including the cytoplasm, nucleus, and basal matrix of the follicle cells, and in intracisternal granules and developing yolk granules of the oocytes.

In creep resistant Z-phase strengthened 12% Cr steels, MX (M=Nb, Ta, or V, and X=C and/or N) to Z-phase (CrMN, M=Ta, Nb, or V) transformation plays an important role in achieving a fine distribution of Z-phase precipitates for creep strengthening. Atom probe tomography was employed to investigate the phase transformation in a Nb-based Z-phase strengthened trial steel. Using iso-concentration surfaces with different concentration values, and subtracting the matrix contribution enabled us to reveal the core-shell structure of the transient precipitates between MX and Z-phase. It was shown that Z-phase forms by diffusion of Cr into NbN upon ageing, and Z-phase has a composition corresponding to Cr1+xNb1−xN with x=0.08.

In the development of dry self-lubricating composites, not only solid lubricant particle size and distribution are important, but also the correct selection of the solid lubricant characteristics, which should be stable, i.e. not reactive, during the whole processing. In this work, Fe+9 vol% h-BN composites were produced by uniaxial cold compaction and sintering, for which a reaction between h-BN and iron was detected after sintering at 1,150°C. The reaction phase was characterized by optical and scanning electron microscopy and identified by X-ray diffraction and energy-dispersive X-ray spectroscopy. The newly formed phase had high hardness when compared with the iron matrix. The resulting composites presented a high friction coefficient and high wear.

Irradiation of reactor pressure vessel (RPV) steels causes the formation of nanoscale microstructural features (termed radiation damage), which affect the mechanical properties of the vessel. A key tool for characterizing these nanoscale features is atom probe tomography (APT), due to its high spatial resolution and the ability to identify different chemical species in three dimensions. Microstructural observations using APT can underpin development of a mechanistic understanding of defect formation. However, with atom probe analyses there are currently multiple methods for analyzing the data. This can result in inconsistencies between results obtained from different researchers and unnecessary scatter when combining data from multiple sources. This makes interpretation of results more complex and calibration of radiation damage models challenging. In this work simulations of a range of different microstructures are used to directly compare different cluster analysis algorithms and identify their strengths and weaknesses.