Screw implantation inevitably causes microdamage in surrounding bone. However, little is known about the detailed characteristics of microdamage in peri-screw bone. In this study, we developed a method to construct microdamage cast with methylmethacrylate (MMA) and observed the cast using scanning electron microscopy (SEM). In basic fuchsin stained bone sections observed by bright-field and fluorescence microscopy, diffuse damage, cross-hatched damage, and linear cracks were all presented in peri-screw bone. Using MMA casting/SEM method, we found numerous densely packed microcracks in the areas with diffuse damage. The osteocyte canaliculi and the microcracks consisting of diffuse damage had a similar diameter (or width), usually <0.5 μm, but their morphology was largely different. In the area with cross-hatched damage, the orientation of microcracks was similar to that in diffuse damage, but the number was significantly decreased. Many microcracks were thicker than 1 μm and associated with a rough surface. Large linear cracks (∼10 μm in diameter) occurred in different areas. Plenty of microcracks were present on the surface of some linear cracks. In conclusion, the MMA casting/SEM method can demonstrate the three-dimensional morphology of different types of microdamage, particularly the microcracks in diffuse damage, which are unable to be shown by light microscopy.

Energy-dispersive X-ray fluorescence was employed to test the hypothesis that beverage consumption or mouthwash utilization will change the chemical properties of dental materials and enamel mineral content. Bovine enamel samples (n = 45) each received two cavity preparations (n = 90), each pair filled with one of three dental materials (R: nanofilled composite resin; GIC: glass-ionomer cement; RMGIC: resin-modified GIC). Furthermore, they were treated with three different solutions (S: saliva; E: erosion/Pepsi Twist®; or EM: erosion+mouthwash/Colgate Plax®). It was found that mineral loss in enamel was greater in GICE samples than in RE > RMGICE > RMGICEM > REM > GICEM. An increased percentage of Zr was found in REM indicating organic matrix degradation. Dental materials tested (R, GIC, and RMGIC) were not able to protect adjacent enamel from acid erosion by the soft drink tested. The use of mouthwash promoted protection of enamel after erosion by the soft drink. To avoid chemical dissolution by mouthwashes, protection by resin composites with surface sealants is recommended.

A three-dimensional (3D) study of multiphase nanostructures by chemically selective electron tomography combining tomographic approach and energy-filtered imaging is reported. The implementation of this technique at the nanometer scale requires careful procedures for data acquisition, computing, and analysis. Based on the performances of modern transmission electron microscopy equipment and on developments in data processing, electron tomography in the energy-filtered imaging mode is shown to be a very appropriate analysis tool to provide 3D chemical maps at the nanoscale. Two examples highlight the usefulness of analytical electron tomography to investigate inhomogeneous 3D nanostructures, such as multiphase specimens or core-shell nanoparticles. The capability of discerning in a silica-alumina porous particle the two different components is illustrated. A quantitative analysis in the whole specimen and toward the pore surface is reported. This tool is shown to open new perspectives in catalysis by providing a way to characterize precisely 3D nanostructures from a chemical point of view.

The microstructure of Cu80Fe10Ni10 (at. %) granular ribbons was investigated by means of three-dimensional field ion microscopy (3D FIM). This ribbon is composed of magnetic precipitates embedded in a nonmagnetic matrix. The magnetic precipitates have a diameter smaller than 5 nm in the as-spun state and are coherent with the matrix. No accurate characterization of such a microstructure has been performed so far. A tomographic characterization of the microstructure of melt spun and annealed Cu80Fe10Ni10 ribbon was achieved with 3D FIM at the atomic scale. A precise determination of the size distribution, number density, and distance between the precipitates was carried out. The mean diameter for the precipitates is 4 nm in the as-spun state. After 2 h at 350°C, there is an increase of the size of the precipitates, while after 2 h at 400°C the mean diameter of the precipitates decreases. Those data were used as inputs in models that describe the magnetic and magnetoresistive properties of this alloy.

With growing interest in nanostructured thin films produced by glancing angle deposition (GLAD), it becomes increasingly important to understand their overall growth mechanics and nanocolumn structure. We present a new method of isolating the individual nanocolumns of GLAD films, facilitating automated measurement of their broadening profiles. Data collected for α = 81° TiO2 vertical nanocolumns deposited across a range of substrate rotation rates demonstrates that these rates influence growth scaling parameters. Further, individual posts were found in each case that violate predicted Kardar-Parisi-Zhang growth scaling limits. The technique's current iteration is comparable to existing techniques in speed: though data were studied from 10,756 individual objects, the majority could not be confidently used in subsequent analysis. Further refinement may allow high-throughput automated film characterization and permit close examination of subtle growth trends, potentially enhancing control over GLAD film broadening and morphology.

High-resolution monochromated electron energy loss spectroscopy (EELS) at subnanometric spatial resolution and <200 meV energy resolution has been used to assess the valence band properties of a distributed Bragg reflector multilayer heterostructure composed of InAlN lattice matched to GaN. This work thoroughly presents the collection of methods and computational tools put together for this task. Among these are zero-loss-peak subtraction and nonlinear fitting tools, and theoretical modeling of the electron scattering distribution. EELS analysis allows retrieval of a great amount of information: indium concentration in the InAlN layers is monitored through the local plasmon energy position and calculated using a bowing parameter version of Vegard Law. Also a dielectric characterization of the InAlN and GaN layers has been performed through Kramers-Kronig analysis of the Valence-EELS data, allowing band gap energy to be measured and an insight on the polytypism of the GaN layers.

In situ nanoindentation of a 30 nm Cu/20 nm Nb multilayer film in a transmission electron microscope revealed confined layer slip as the dominant deformation mechanism. Dislocations were observed to nucleate from the Cu-Nb interfaces in both layers. Dislocation glide was confined by interfaces to occur within each layer, without transmission across interfaces. Cu and Nb layers co-deformed to large plastic strains without cracking. These microscopy observations provide insights in the unit mechanisms of deformation, work hardening, and recovery in nanoscale metallic multilayers.

Laboratory water uptake tests are performed at the Belgian Nuclear Research Centre SCK•CEN to obtain insight into the hydromechanical behavior of Eurobitum bituminized radioactive waste under geological disposal conditions. Small nonradioactive and radioactive Eurobitum samples are hydrated in restricted swelling conditions (i.e., nearly constant volume conditions and constant stress conditions). Microfocus X-ray computer tomography (μCT) proves to be a very suitable technique to follow up the ingress of water in the samples. μCT analyses demonstrate that, under the studied hydration conditions, the water uptake by Eurobitum samples is a diffusion controlled process. A characterization of the partially leached samples with environmental scanning electron microscopy (ESEM) shows that the hydration of salt crystals and the subsequent dilution of the salt solution result in an increase in pore size that is limited to a few tens of μm in restricted swelling conditions. The μCT and ESEM analyses allow improvement in the understanding of water uptake by Eurobitum in restricted swelling conditions. In this article we discuss the μCT and ESEM analyses of nonradioactive Eurobitum samples that were hydrated for 2 to 4 years at a constant stress of 1, 22, 33, and 44 bar or in nearly constant volume conditions.

The conservation and durability of historical renders must be carried out through compatible techniques and materials. An important operation is the restitution of historical renders cohesion, turned friable by the loss of binder, usually due to physical and/or chemical actions. Surface consolidation is based on the use of materials with aggregating properties. This operation is reached usually through the application of organic or mineral consolidants, but inorganic consolidants are becoming preferred due to better compatibility and durability. In this article two mineral compatible consolidation products were studied: a commercial suspension of calcium hydroxide nanoparticles in propanol and a limewater dispersion of ethyl silicate. Microscopy (optical and scanning electron microscopy) and X-ray microanalyses of the consolidation products and of the consolidated mortar specimens were carried out. To assess the mechanical properties and product's efficacy, analyses of the compression, flexural strength, and superficial hardness were performed. Microscopy results show that limewater dispersion of ethyl silicate forms platelike silica gels, which can interfere in product penetration. Otherwise, nanolime particles permit homogeneous distribution and optimum penetration on the treated substrate, improving cementing action and the agglomeration process.

This article presents a detailed study of the microstructure of Iberian expanded clay lightweight aggregates (LWA). Other than more commonly used mercury porosimetry (MP) and water absorption methods, the experimental study involves optical microscopy, scanning electron microscopy (SEM), and microtomography (μ-CT). Pore connectivity and how it is deployed are shown to some degree, and the pore size spectrum is estimated. LWA are in general characterized by a dense outer shell up to 200 μm thick, encasing an inner cellular structure of 10–100 times bigger pore size. Aggregate pore sizes may span from some hundreds of nanometers up to over 1 mm, though the range of 1–25 μm is more typical. A noteworthy fraction of these pores is closed, and they are mainly up to 1 μm. It is also shown that macropore spatial arrangement is affected by the manufacturing process. A step forward is given to understanding how the outer shell and the inner pore network influence the mechanical and physical LWA properties, particularly the density and water absorption. The joint consideration of μ-CT and SEM seems to be the most appropriate methodology to study LWA microstructure. MP analysis is likely to distort LWA pore spectrum assessment.