Advanced nanoanalysis of a Hf-based high-<i>k</i> dielectric stack prior to activation

Analytical electron microscopy techniques are used to investigate elemental distributions across a high-&lt;i&gt;k&lt;/i&gt; dielectric stack with a metal gate. Electron energy-loss spectroscopy results from a Si(100)/SiO2/HfO2/TiN/a-Si gate stack confirm the presence of an oxide interfacial phase at the TiN/a-Si interface prior to activation of the stack

Nanoanalytical Electron Microscopy Reveals a Sequential Mineralization Process Involving Carbonate-Containing Amorphous Precursors

A direct observation and an in-depth characterization of the steps by which bone mineral nucleates and grows in the extracellular matrix during the earliest stages of maturation, using relevant biomineralization models as they grow into mature bone mineral, is an important research goal. To better understand the process of bone mineralization in the extracellular matrix, we used nanoanalytical electron microscopy techniques to examine an in vitro model of bone formation. This study demonstrates the presence of three dominant CaP structures in the mineralizing osteoblast cultures: <80 nm dense granules with a low calcium to phosphate ratio (Ca/P) and crystalline domains; calcium phosphate needles emanating from a focus: “needle-like globules” (100–300 nm in diameter) and mature mineral, both with statistically higher Ca/P compared to that of the dense granules. Many of the submicron granules and globules were interspersed around fibrillar structures containing nitrogen, which are most likely the signature of the organic phase. With high spatial resolution electron energy loss spectroscopy (EELS) mapping, spatially resolved maps were acquired showing the distribution of carbonate within each mineral structure. The carbonate was located in the middle of the granules, which suggested the nucleation of the younger mineral starts with a carbonate-containing precursor and that this precursor may act as seed for growth into larger, submicron-sized, needle-like globules of hydroxyapatite with a different stoichiometry. Application of analytical electron microscopy has important implications in deciphering both how normal bone forms and in understanding pathological mineralization

Micro-to nano-scale characterisation of polyamide structures of the SW30HR RO membrane using advanced electron microscopy and stain tracers

The development of new reverse osmosis (RO) membranes with enhanced performance would benefit from a detailed knowledge of the membrane structures which participate in the filtration process. Here, we examined the hierarchical structures of the polyamide (PA) active layer of the SW30HR RO membrane. Scanning electron microscopy combined with focused ion beam milling (FIB-SEM) was used to obtain the 3-D reconstructions of membrane morphology with 5 nm cross-sectional resolution (comparable with the resolution of low magnification TEM imaging in 2D) and 30 nm slice thickness. The complex folding of the PA layer was examined in 3 dimensions, enabling the quantification of key structural properties of the PA layer, including the local thickness, volume, surface area and their derivatives. The PA layer was found to exhibit a much higher and convoluted surface area than that estimated via atomic force microscopy (AFM). Cross-sectional scanning transmission electron microscopy (STEM) was used to observe the distribution of a tracer stain under various conditions. The behaviour of stain in dry and wet PA indicated that the permeation pathways have a dynamic nature and are activated by water. High resolution STEM imaging of the stained PA nano-films revealed the presence of <1 nm pore-like structures with a size compatible with free volume estimations by positron annihilation lifetime spectroscopy (PALS). This study presents a comprehensive map of the active PA layer across different length scales (from micro- to sub-nanometre) and mechanistic insight into their role in the permeation process

Evidence for Supercurrent Connectivity in Conglomerate Particles in NdFeAsO1-d

Here we use global and local magnetometry and Hall probe imaging to investigate the electromagnetic connectivity of the superconducting current path in the oxygen-deficient fluorine-free Nd-based oxypnictides. High resolution transmission electron microscopy and scanning electron microscopy show strongly-layered crystallites, evidence for a ~ 5nm amorphous oxide around individual particles, and second phase neodymium oxide which may be responsible for the large paramagnetic background at high field and at high temperatures. From global magnetometry and electrical transport measurements it is clear that there is a small supercurrent flowing on macroscopic sample dimensions (mm), with a lower bound for the average (over this length scale) critical current density of the order of 103 A/cm2. From magnetometry of powder samples and local Hall probe imaging of a single large conglomerate particle ~120 microns it is clear that on smaller scales, there is better current connectivity with a critical current density of the order of 5 x 104 A/cm2. We find enhanced flux creep around the second peak anomaly in the magnetisation curve and an irreversibility line significantly below Hc2(T) as determined by ac calorimetry.Comment: 11 pages, 4 figure