The properties and the shape memory effect depend, among other things, on chemical composition, as well as the method of shape memory alloy (SMA) production. One of the manufacturing methods that leads to the amorphous/nanocrystalline SMA is high-energy ball milling combined with annealing. Using this technique, an SMA memory alloy, with the nominal chemical composition of Ni25Ti50Cu25, was produced from commercial elemental powders (purity −99.7%). The structure and morphology were characterized (at the various stages of its production) by the use of X-ray diffraction, as well as electron microscopy (both scanning and transmission). Choosing the appropriate grinding time made it possible to produce an NiTiCu alloy with a different crystallite size. Its average size changed from 6.5 nm (after 50 h) to about 2 nm (100 h). Increasing the grinding time up to 140 h resulted in the formation of areas that showed the B19 martensite and the Ti2(Ni,Cu) phase with the average crystallite size of about 6 nm (as milled). After crystallization, the average size increased to 11 nm.

The study of the fundamentals of the α → ω and β → ω phase transformations induced by high-pressure torsion (HPT) in Ti–Nb-based alloys is presented in the current work. Prior to HPT, three alloys with 5, 10, and 20 wt% of Nb were annealed in the temperature range of 700–540°C in order to obtain the (α + β)-phase state with a different amount of the β-phase. The samples were annealed for a long time in order to reach equilibrium Nb content in the α-solid solution. Scanning electron microscope (SEM), transmission electron microscopy, and X-ray diffraction techniques were used for the characterization of the microstructure evolution and phase transformations. HPT results in a strong grain refinement of the microstructure, a partial transformation of the α-phase into the ω-phase, and a complete β → ω phase transformation. Two kinds of the ω-phase with different chemical compositions were observed after HPT. The first one was formed from the β-phase, enriched in Nb, and the second one from the almost Nb-pure α-phase. It was found that the α → ω phase transformation depends on the Nb content in the initial α-Ti phase. The less the amount of Nb in the α-phase, the more the amount of the α-phase is transformed into the ω-phase.

The excitability of local surface plasmon modes in radial trimers composed of gold nanorods was mapped using hyperspectral cathodoluminescence (CL) in the scanning electron microscope. In symmetric trimers, the local plasmon resonances could be excited most effectively at the ends of individual rods. Introducing asymmetry into the structure breaks the degeneracy of the dipole modes and changes the excitability of transverse dipole modes in different directions. CL in the scanning electron microscope has great potential to interrogate individual nanophotonic structures and is a complement to electron energy loss spectroscopy and optical microscopy.

Surface-sensitive information on a bulk sample can be obtained by using a low incident electron energy (low accelerating voltage/landing voltage) in a scanning electron microscope (SEM). However, topography and composition contrast obtained at low incident electron energies may not be intuitive and should be analyzed carefully. By combining an Auger electron spectrometer (AES) with a low incident electron energy SEM (LE-SEM), we investigated the SEM contrast carefully by separating the secondary electron (SE) and back-scattered electron (BSE) components with high accuracy. For this, we modified an AES to measure the electron energy in the range of 0–0.6 keV with a sample bias voltage of 0 to −0.3 keV. We could clearly observe reversed brightness of gold and carbon (graphite) in BSE images when the energy of the incident electrons was reduced to 0.2–0.3 keV. In addition, reflected electron energy spectroscopy (REELS) is known to be a tool for chemical state analysis of the sample. We demonstrated that it is possible to study the electron states of graphite, diamond, and graphene by acquiring low incident energy REELS spectra from their surfaces with the newly modified AES. This will be a new method for analyzing the electron states of local areas of a surface.

En este trabajo se presentan los resultados del análisis de una pieza ósea que brinda información pionera sobre aspectos tecnológicos prehispánicos en el sector ribereño Paraguay-Paraná del Chaco argentino. Se analizó un elemento óseo de Rhea americana con evidencias de formatización. Con el objetivo de caracterizar la etapa de producción representada, se registraron marcas de manufactura, una de las cuales fue analizada con microscopio electrónico de barrido a fin de identificar el material con que se produjo la formatización (piedra o valva). A partir del análisis, se define el elemento como un núcleo con “extracción bosquejada”, es decir, una pieza en la cual se evidencia una forma base que aún no ha sido extraída. Se propone que la técnica de manufactura consistió en el ranurado a partir de filos de valva (Diplodon sp.). Este trabajo constituye el primer aporte con evidencias sobre el uso de filos de valvas de molusco en el proceso de confección de artefactos óseos en sitios arqueológicos de Argentina.

The structural details of chromosomes have been of interest to researchers for many years, but how the metaphase chromosome is constructed remains unsolved. Divalent cations have been suggested to be required for the organization of chromosomes. However, detailed information about the role of these cations in chromosome organization is still limited. In the current study, we investigated the effects of Ca2+ and Mg2+ depletion and the reversibility upon re-addition of one of the two ions. Human chromosomes were treated with different concentrations of Ca2+and Mg2+. Depletion of Ca2+ and both Ca2+ and Mg2+ were carried out using 1, 2-bis(2-aminophenoxy)ethane-N,N,N',N'-tetraacetic acid and ethylenediaminetetraacetic acid (EDTA), respectively. Chromosome structure was examined by fluorescence microscopy and scanning electron microscopy. The results indicated that chromosome structures after treatment with a buffer without Mg2+, after Ca2+ depletion, as well as after depletion of both Mg2+, and Ca2+, yielded fewer compact structures with fibrous chromatin than those without cation depletion. Interestingly, the chromatin of EDTA-treated chromosomes reversed to their original granular diameters after re-addition of either Mg2+ or Ca2+ only. These findings signify the importance of divalent cations on the chromosome structure and suggest the interchangeable role of Ca2+ and Mg2+.

This study aimed to examine in vivo starch digestion kinetics and to unravel the mechanisms of starch hydrolysing enzymes. Ninety pigs (23 (sd 2·1) kg body weight) were assigned to one of nine treatments in a 3×3 factorial arrangement, with starch source (barley, maize, high-amylose (HA) maize) and form (isolated, within cereal matrix, extruded) as factors. We determined starch digestion coefficients (DC), starch breakdown products and digesta retention times in four small-intestinal segments (SI1–4). Starch digestion in SI2 of pigs fed barley and maize, exceeded starch digestion of pigs fed HA maize by 0·20–0·33 DC units (P<0·01). In SI3–4, barley starch were completely digested, whereas the cereal matrix of maize hampered digestion and generated 16 % resistant starch in the small intestine (P<0·001). Extrusion increased the DC of maize and HA maize starch throughout the small intestine but not that of barley (P<0·05). Up to 25 % of starch residuals in the proximal small intestine of pigs was present as glucose and soluble α(1–4) maltodextrins. The high abundance of glucose, maltose and maltotriose in the proximal small intestine indicates activity of brush-border enzymes in the intestinal lumen, which is exceeded by α-amylase activity. Furthermore, we found that in vivo starch digestion exceeded our in vitro predictions for rapidly digested starch, which indicates that the role of the stomach on starch digestion is currently underestimated. Consequently, in vivo glucose release of slowly digestible starch is less gradual than expected, which challenges the prediction quality of the in vitro assay.

This paper presents a new method for creating and monitoring controlled localized negatively charged regions inside insulators with a scanning electron microscope (SEM). A localized buried charged region is created and observed close to the point where a high voltage primary beam (10 kV) strikes a metal–insulator–silicon specimen. The amount of buried charge within the insulator at any given moment can be dynamically monitored by detecting the appearance of a second peak in the secondary electron (SE) energy spectrum. SE energy spectral signals were obtained through the use of a compact high signal-to-noise energy analyzer attachment that was fitted on to the SEM specimen stage. An electrostatic model, together with Monte Carlo simulations, is presented to explain how the SE charge contrast effect functions. This model is then experimentally confirmed by using the SE energy spectral signal induced by a gallium ion beam inside a dual focused ion beam-SEM instrument.

Scanning electron micrographs that depict the surface and internal structure of several starch-encapsulated granular formulations of EPTC (S-ethyl dipropylthiocarbamate) and butylate (S-ethyl diisobutylthiocarbamate) relate well with herbicidal release rates previously reported. Fast-release formulations appear to have a porous surface with little distinctive internal structure. Diffusion would be expected to be more rapid as fewer diffusion barriers are present. Slow-release formulations have a smooth, hard surface with irregular surface pores and a honeycombed internal structure. The slower release characteristics are associated with stronger oxidants used for crosslinking xanthate in the entrapment of herbicides. The scanning electron microscope would be an excellent quality control technique in the preparation of starch-encapsulated herbicides.

In the present investigation, AA6351 aluminum alloy matrix composites reinforced with various percentages of AlN particles were fabricated by stir casting technique. The percentage of AlN was varied from 0 to 20% in a step of 4%. The prepared AA6351-AlN composites were characterized using scanning electron microscope (SEM) and x-ray diffraction (XRD). The mechanical properties such as micro-hardness, compression strength, flexural strength, and tensile strength of the proposed composite have been studied. X-ray diffraction patterns confirm the presence of AlN particles in the composites. SEM analysis reveals the homogeneous distribution of AlN particles in the AA6351 matrix. The mechanical properties of the composite were found to be noticeably higher than that of the plain matrix alloy due to augmented particle content. The produced composites exhibit superior mechanical properties when compared with unreinforced matrix alloy. Fracture surface analysis of tensile specimens show the ductile–brittle nature of failure in the composites.

A contactless method of probing and analyzing multifunctional oxide interfaces using an electron energy analyzer inside a scanning electron microscope is presented. High contrast experimental secondary electron analyzer signals are used to detect changes in the interface conductivity of a LaAlO3/SrTiO3 sample. Monte Carlo simulations of the primary beam/specimen interaction are carried out and correlated with the experimental results in order to help understand the role of the primary beam energy and adjust it to enhance contrast.

Electron-beam-induced soft-X-ray emission spectroscopy (SXES) that uses a grating spectrometer has been introduced to a conventional scanning electron microscope (SEM) for characterizing desired specimen areas of bulk materials. The spectrometer was designed as a grazing incidence flat-field optics by using aberration corrected (varied line spacing) gratings and a multichannel plate detector combined with a charge-coupled device camera, which has already been applied to a transmission electron microscope. The best resolution was confirmed as 0.13 eV at Mg L-emission (50 eV), which is comparable with that of recent dedicated electron energy-loss spectroscopy instruments. This SXES-SEM instrument presents density of states of simple metals of bulk Mg and Li. Apparent band-structure effects have been observed in Si L-emission of Si wafer, P L-emission of GaP wafer, and Al L-emissions of intermetallic compounds of AlCo, AlPd, Al2Pt, and Al2Au.

Elemental analysis of dental hard tissues is of importance. The aim of this study is to evaluate X-ray microanalysis (XRMA) of bovine enamel in a scanning electron microscope (SEM) with different coatings. The buccal surface of bovine incisors was polished flat, one-third was coated with carbon, one-third with gold, leaving one-third uncoated for XRMA in an SEM equipped with an energy-dispersive microanalysis system. The elements oxygen, sodium, magnesium, phosphorous, chlorine, potassium, and calcium were analyzed using their respective characteristic K X-ray series. Comparisons were made with analyses of glass produced by fusion of the bovine enamel, showing that oxygen analyses using the K X-ray series are reliable and preferable to calculating oxygen by stoichiometry for natural enamel. For the gold-coated and uncoated analyses, carbon was also measured using the K X-ray series. Small area Analyses in small areas (80 × 80 μm) in variable pressure-SEM mode with low vacuum (20 Pa), without any coating, midway between 40 μm wide gold lines 140 μm apart to avoid build-up of electrostatic charge is the preferred method, especially if carbon is included in the analysis. The analyses of bovine enamel are sufficiently reproducible to be regarded as quantitative for all elements except carbon.

A method is presented for determining the point spread function (PSF) of an electron beam in a scanning electron microscope for the examination of near planar samples. Once measured, PSFs can be used with two or more low-resolution images of a selected area to create a high-resolution reconstructed image of that area. As an example, a 4× improvement in resolution for images is demonstrated for a fine gold particle sample. Since thermionic source instruments have high beam currents associated with large probe sizes, use of this approach implies that high-resolution images can be produced rapidly if the probe diameter is less of a limiting factor. Additionally, very accurate determination of the PSFs can lead to a better understanding of instrument performance as exemplified by very accurate measurement of the beam shape and therefore the degree of astigmatism.

We have developed a fiber-based confocal optical microscope that operates inside of a commercial scanning electron microscope (SEM) instrument (JEOL 6400; JEOL Ltd., Tokyo, Japan) enabling the excitation of a sample either by a laser or by electron beam, and hence combining the complimentary techniques of photoluminescence and cathodoluminescence. The instrument uses single-mode fibers that enter the SEM by vacuum feedthroughs. The illumination and collection fibers operate as effective pinholes providing, in combination with a microscope objective (NA = 0.3), high spatial resolution (~2 μm) and excellent collection efficiency. The high spatial resolution ensures that the light collected from the sample is in a region of optimal laser beam and electron beam overlap. The capabilities of this instrument are tested by experiments involving the excitation of europium ions in situ doped in GaN thin films.

A total of twenty-seven species of marine-living coccolithophores were recorded from seawater samples that were collected during two spring cruises along the shelf regions of the Yellow Sea (YS) and the East China Sea (ECS). They were classified into ten families and four orders, with some additional species incertae sedis. Most of these species were heterococcolithophores, and no holococcolithophores were examined from the YS waters. Six species were recorded for the first time from the coastal waters of the China Seas and their morphological characteristics are described and photographically illustrated in this paper. They were Cyrtosphaera lecaliae, Syracosphaera histrica, Syracosphaera marginaporata, Pappomonas cf. sp. type 3, Calyptrolithophora papillifera and Corisphaera strigilis. Three types of Emiliania huxleyi, type A, type B/C and type C, were examined. Species of the genus Syracosphaera, in addition to E. huxleyi and Gephyrocapsa oceanica, frequently occurred at the surveyed sites. The coccolithophore assemblages in the offshore waters of the ECS were characterized by high species diversity—fourteen species in one sample. This finding indicated that the shelf waters adjacent to the Kuroshio path were ideal habitats for living coccolithophores. The variation in taxonomic composition of these algae could be associated with differences in their preferred habitats.

The amino acid, fatty acid and mineral composition of Aspongubus viduatus F. (melon bug) and Agonoscelis pubescens (Thunberg) (sorghum bug) were investigated. The approximate analyses of A. viduatus and A. pubescens adults showed 8.3 and 7.6% moisture, 27.0 and 28.2% crude protein, 54.2 and 57.3% fat and 3.5 and 2.5% ash on a dry-matter basis, respectively. The bug protein contained 16 amino acids, including all of the essential ones. Compared with the amino acid profile recommended by FAO/WHO, the protein was of medium quality. The most predominant fatty acids in melon bug oil were oleic, palmitic, linoleic and linolenic acids, viz. 45.5, 31.3, 4.9 and 0.48%, respectively, and in sorghum bug 41.15, 11.41, 35.28 and 1.28%, respectively. The mineral analysis indicated high P and K content. Scanning electron microscopy was used to study ground insect structure before and after oil extraction. Micrographs of full-fat ground insects were different from defatted ones.

Over the past decades, pollution, overfishing, and habitat degradation have driven the population size of Taiwan shoveljaw carp down markedly in Taiwan. Cryopreservation is a useful tool which could be used to maintain genetic resources to protect and preserve this endemic species. Four cryoprotectants [dimethyl sulphoxide (DMSO), dimethylacetamide (DMA), glycerol and methanol] and six freezing rates (0.5, 1, 2, 4, 8, 16 °C min-1) were tested in order to develop an optimal controlled slow-freezing protocol for Taiwan shoveljaw carp spermatozoa. Samples were subsequently examined under the scanning electron microscope to reveal whether cryopreservation had affected their ultrastructural morphology. The highest survival rate (50.1 ± 2.0%) was observed with a freezing rate of 8 °C min-1 in 1M DMSO, using SYBR-14 + PI staining. Fertility and hatching rate results using frozen-thawed spermatozoa (90.2 ± 2.2% and 22.3 ± 2.5%, respectively) were not significantly different from results with fresh spermatozoa. After cryopreservation, 21.0 ± 1.6% of frozen-thawed spermatozoa had mid-piece swelling and rupture of the head. Cryopreservation might, therefore, slightly affect Taiwan shoveljaw carp spermatozoa in terms of morphological change. However, these alterations could be compensated by using large enough numbers of normally functioning frozen-thawed spermatozoa to achieve a standard equal to fresh spermatozoa. This is the first report of successful cryopreservation of Taiwan shoveljaw carp spermatozoa using a controlled slow-cooling method.

Experimental low-loss electron (LLE) yields were measured as a function of loss energy for a range of elemental standards using a high-vacuum scanning electron microscope operating at 5 keV primary beam energy with losses from 0 to 1 keV. The resulting LLE yield curves were compared with Monte Carlo simulations of the LLE yield in the particular beam/sample/detector geometry employed in the experiment to investigate the possibility of modeling the LLE yield for a series of elements. Monte Carlo simulations were performed using both the Joy and Luo [Joy, D.C. & Luo, S., Scanning11(4), 176–180 (1989)] expression for the electron stopping power and recent tabulated values of Tanuma et al. [Tanuma, S. et al., Surf Interf Anal37(11), 978–988 (2005)] to assess the influence of the more recent stopping power data on the simulation results. Further simulations have been conducted to explore the influence of sample/detector geometry on the LLE signal in the case of layered samples consisting of a thin C overlayer on an elemental substrate. Experimental LLE data were collected from a range of elemental samples coated with a thin C overlayer, and comparisons with Monte Carlo simulations were used to establish the overlayer thickness.

Here, we describe the development of an inexpensive and versatile manipulation system for in situ experiments in a field emission scanning electron microscope based on a parallel-guiding plate-spring mechanism and low cost materials. The system has been tested for a wide range of applications, such as collecting, moving, and positioning particles, fabricating atomic force microscopy tips based on carbon nanotubes, and characterizing individual nanobjects. The nanomanipulation results demonstrate that there are many opportunities for the use of physical manipulation in the bottom-up approach to fabrication of nanodevices.