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Transmission electron backscatter diffraction (t-EBSD) was used to investigate the effect of dealloying on the microstructure of 140-nm thin gold foils. Statistical and local comparisons of the microstructure between the nonetched and nanoporous gold foils were made. Analyses of crystallographic texture, misorientation distribution, and grain structure clearly prove that during the dealloying manufacturing process of nanoporous materials the crystallographic texture is enhanced significantly with a clear decrease of internal strain, whereas maintaining the grain structure.

This paper investigates the adhesive interface in a polymer/metal (polyethylene terephthalate/steel) laminate that is subjected to uniaxial strain. Cross-sections perpendicular to such interfaces were created with a focused ion beam and imaged with scanning electron microscopy during straining in the electron microscope. During in situ straining, glide steps formed by the steel caused traction at the interface and initiated crazes in the polyethylene terephthalate (PET). These crazes readily propagated along the free surface of the PET layer. Similar crazing has not been previously encountered in laminates that were pre-strained or in numerical calculations. The impact of focused ion beam treatments on mechanical properties of the polymer/metal laminate system was therefore investigated. It was found that mechanical properties such as toughness of PET are dramatically influenced by focused ion beam etching. It was also found that this change in mechanical properties has a different effect on the pre-strained and in situ strained samples.

This paper presents a statistical method to analyze instabilities that can be introduced during imaging in scanning electron microscopy (SEM). The method is based on the correlation of digital images and it can be used at different length scales. It consists of the evaluation of three different approaches with four parameters in total. The methodology is exemplified with a specific case of internal stress measurements where ion milling and SEM imaging are combined with digital image correlation. It is concluded that before these measurements it is important to test the SEM column to ensure the minimization and randomization of the imaging instabilities. The method has been applied onto three different field emission gun SEMs (Philips XL30, Tescan Lyra, FEI Helios 650) that represent three successive generations of SEMs. Important to note that the imaging instability can be quantified and its source can be identified.

A versatile method to fabricate taper-free micro-/nanopillars of large aspect ratio was developed with focused ion beam (FIB) cutting. The key features of the fabrication are a FIB with an incident angle of 90° to the long axis of the pillar that enables milling of the pillar sideways avoiding tapering and the FIB current can be reduced step by step so as to reduce possible radiation damage of the milled surface by Ga ions. A procedure to accurately determine the cross-section of each pillar was developed.

This study explores the use of DC magnetron sputtering tungsten thin films for surface modification of TiNi shape memory alloy (SMA) targeting for biomedical applications. SEM, AFM and automatic contact angle meter instrument were used to determine the surface characteristics of the tungsten thin films. The hardness of the TiNi SMA with and without tungsten thin films was measured by nanoindentation tests. It is demonstrated that the tungsten thin films deposited at different magnetron sputtering conditions are characterized by a columnar microstructure and exhibit different surface morphology and roughness. The hardness of the TiNi SMA was improved significantly by tungsten thin films. The ion release, hemolysis rate, cell adhesion and cell proliferation have been investigated by inductively coupled plasma atomic emission spectrometry, CCK-8 assay and alkaline phosphatase activity test. The experimental findings indicate that TiNi SMA coated with tungsten thin film shows a substantial reduction in the release of nickel. Therefore, it has a better in vitro biocompatibility, in particular, reduced hemolysis rate, enhanced cell adhesion and differentiation due to the hydrophilic properties of the tungsten films.

Transmission electron microscopy characterization of two major long-period stacking ordered (LPSO) phases in Mg-Zn-Y alloy, i.e., 18R- and 14H-LPSO are reported. The space group and atomic-scale microstructures of both compounds were determined using a combination of electron diffraction, convergent beam electron diffraction, high-resolution transmission electron microscopy, and Z-contrast scanning transmission electron microscopy. The 18R-LPSO phase is demonstrated to have a point group and space group 3m and R3m (or 3 m and R 3 m), with the lattice parameter a = 1.112 nm and c = 4.689 nm in a hexagonal coordinate system. The 14H-LPSO phase has a point group 6/mmm and a space group P63 /mmc, and the lattice parameter is a = 1.112 nm and c = 3.647 nm. In addition, insertion of extra thin Mg platelets of several atomic layers, results in stacking faults in the LPSO phase. These results may shed some new light on a better understanding of the microstructure and deformation mechanisms of LPSO phases in Mg alloys.

We present the results of our study about the deposition rate of focused electron beam induced processing (FEBIP) as a function of the substrate temperature with the substrate being an electron-transparent amorphous carbon membrane. When W(CO)6 is used as a precursor it is observed that the growth rate is lower at higher substrate temperatures. From Arrhenius plots we calculated the activation energy for desorption, E des, of W(CO)6. We found an average value for E des of 20.3 kJ or 0.21 eV, which is 2.5-3.0 times lower than literature values. This difference between estimates for E des from FEBIP experiments compared to literature values is consistent with earlier findings by other authors. The discrepancy is attributed to electron-stimulated desorption, which is known to occur during electron irradiation. The data suggest that, of the W(CO)6 molecules that are affected by the electron irradiation, the majority desorbs from the surface rather than dissociates to contribute to the deposit. It is important to take this into account during FEBIP experiments, for instance when determining fundamental process parameters such as the activation energy for desorption.

During laser deposition of Ni-Cr-B-Si-C alloys with high amounts of Cr and B, various microstructures and phases can be generated from the same chemical composition that results in heterogeneous properties in the clad layer. In this study, the microstructure and phase constitution of a high-alloy Ni-Cr-B-Si-C coating deposited by laser cladding were analyzed by a combination of several microscopy characterization techniques including scanning electron microscopy in secondary and backscatter imaging modes, energy dispersive spectroscopy (EDS), electron backscatter diffraction (EBSD), and transmission electron microscopy (TEM). The combination of EDS and EBSD allowed unequivocal identification of micron-sized precipitates as polycrystalline orthorhombic CrB, single crystal tetragonal Cr5B3, and single crystal hexagonal Cr7C3. In addition, TEM characterization showed various equilibrium and metastable Ni-B, Ni-Si, and Ni-Si-B eutectic products in the alloy matrix. The findings of this study can be used to explain the phase formation reactions and to tune the microstructure of Ni-Cr-B-Si-C coatings to obtain the desired properties.

A computer-controlled procedure is outlined here that first determines the position of the amorphous-crystalline interface in an image. Subsequently, from a time series of these images, the velocity of the crystal growth front is quantified. The procedure presented here can be useful for a wide range of applications, and we apply the new approach to determine growth rates in a so-called fast-growth-type phase-change material. The growth rate (without nucleation) of this material is of interest for comparison with identical material used in phase-change random access memory cells. Crystal growth rates in the amorphous phase-change layers have been measured at various temperatures using in situ heating in a transmission electron microscope. Doped SbTe films (20 nm thick) were deposited on silicon nitride membranes, and samples with and without silicon oxide capping layer were studied. The activation energy for growth was found to be 3.0 eV. The samples without capping layer exhibit a nucleation rate that is an order of magnitude higher than the samples with a silicon oxide capping layer. This difference can be attributed to the partial oxidation of the phase-change layer in air. However, the growth rates of the samples with and without capping are quite comparable.

Background: Inward curling of the barbs of Meniscus Arrows during degradation was observed in a previous study, in which swelling, distention, and water uptake by Meniscus Arrows was evaluated. This change of configuration could have consequences with respect to anchorage capacity in bone., Material/methods: Eight non-degraded Meniscus Arrows in the original configuration were pulled out of thawed, fresh-frozen human femoral condyle, and pull-out force was measured and compared with that of 6 Meniscus Arrows after 31 days of degradation under controlled conditions., Results: No significant difference was found between the 2 groups with respect to the required pull-out force (t test), the distribution of the data, or the interaction between degradation and location, as evaluated by Mann-Whitney test, and no significant difference was found between the 2 groups with respect to the degradation state or position in the condyles, as evaluated by 2-way analysis of variance., Conclusions: Our results indicate that the decrease in barb-barb diameter during the first month of degradation of the Meniscus Arrows has no significant effect on the tensile pull-out force required for removal from human femur condyle. Further research should be undertaken to examine whether the same is true for other biodegradable devices with barbs.

As a tribute to the scientific work of Professor Gareth Thomas in the field of structure-property relationships this paper delineates a new possibility of Lorentz transmission electron microscopy (LTEM) to study the magnetic properties of soft magnetic films. We show that in contrast to the traditional point of view, not only does the direction of the magnetization vector in nano-crystalline films make a correlated small-angle wiggling, but also the magnitude of the magnetization modulus fluctuates. This fluctuation produces a rapid modulation in the LTEM image. A novel analysis of the ripple structure in nano-crystalline Fe-Zr-N film corresponds to an amplitude of the transversal component of the magnetization deltaMy of 23 mT and a longitudinal fluctuation of the magnetization of the order of deltaMx = 30 mT. The nano-crystalline (Fe99Zr1)1-xNx films have been prepared by DC magnetron reactive sputtering with a thickness between 50 and 1000 nm. The grain size decreased monotonically with N content from typically 100 nm in the case of N-free films to less than 10 nm for films containing 8 at%. The specimens were examined with a JEOL 2010F 200 kV transmission electron microscope equipped with a post column energy filter (GIF 2000 Gatan Imaging Filter). For holography, the microscope is mounted with a biprism (JEOL biprism with a 0.6 microm diameter platinum wire).