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It is, indeed, an honour and pleasure to write a guest editorial for British Actuarial Journal. The guidelines stated that my topic could be ‘education’, so, as a lifelong educator (whether any students became educated is another matter), I have chosen that topic as my focus.
Advantages of the FIB lift-out technique over traditional H-bar TEM specimen preparation have been recognized. The ability to rapidly (< 1 hour) prepare a site specific TEM specimen without destroying the entire bulk specimen has led to a wide spread reliance on this method. The main disadvantage of this technique is an inability to accomplish additional membrane thinning if required. Traditional H-bar preparation allows additional thinning. However, mechanical polishing is time consuming and the bulk sample is destroyed. A method has been developed which combines the efficient, site specific advantages of the lift-out method with the H-bar's ability to accomplish additional thinning. in this procedure a lift-out specimen is removed from the bulk sample and mounted onto a half-grid in a configuration similar to that employed by the H-bar technique.
A 1.0-micron thick lift-out specimen was prepared using a FEI Strata DB-235 FIB dual-beam workstation by sputtering away bulk material leaving a thin membrane containing a desired feature (FIG 1).
Energy Dispersive Spectrometry (EDS) is an ubiquitous method of elemental analysis for SEM, TEM, and STEM applications. The elements of interest are generally quantified without standards using theoretical calculations or by using standards that are high purity specimens of the elements measured. However, EDS is often used to determine a small percentage of an element in a matrix. The accuracy and limit of detection of these low concentration measurements has not been established. An earlier report proved the concept that a cross section high dose BF2 implanted specimen could provide a standard for EDS measurement of F. This study extends this quantification approach to transition elements of importance to the semiconductor industry.
The Fe and Co standards were created by high dose ion implantation. For ions implanted into silicon, a dose of lxl016 atoms/cm2 results in a peak concentration of approximately lxl021 atoms/cm3 or 2% atomic. The exact concentration can be determined using methods such as Rutherford Backscattering Spectrometry (RBS) and Secondary Ion Mass Spectrometry (SIMS).
Antimony-doped tin oxide (ATO) catalysts are used for the oxidation of propylene to acrolein, the ammoxidation of propylene to acrylonitrile and the oxidative dehydrogenation of butanes to 1,3- butadiene. The distribution and valence states of Sb in ATOs are key in determining their catalytic activities. While these materials have been subjects of intensive studies for more than 20 years, X-ray photoelectron spectroscopy, Mössbauer spectrometry, and X-ray absorption spectroscopy4 have so far provided only indirect data for the distribution of Sb and its valence states. in particular, while has been hypothesized that the tin (IV) oxide contains Sb (V) within the bulk lattice and Sb (III) located at surface sites, no direct experimental evidence for this has been provided.
Here we use electron energy loss spectroscopy (EELS) combined with Z-contrast imaging in a JEOL 2010F field emission STEM/TEM operating at 200 KV to analyze ATO catalysts.
Mixed conductors have been the focus of many studies in the last decade, leading to a detailed understanding of many of the macroscopic bulk properties of these materials. in particular, although the reduced low temperature phase in rare earth perovskite oxides is commonly explained in terms of ordered brownmillerite structured micro domains, its transition to the high temperature phase remains elusive. in this presentation an investigation of (La, Sr)FeO3, prepared under different reducing conditions through correlated atomic resolution annular dark field imaging and electron energy loss spectroscopy will be shown.
We investigate the (La, Sr)FeO3 material by atomic resolution Z-contrast imaging and EELS using a 200 keV STEM/TEM JEOL2010F with a post column GIF. The combination of these techniques allows us to obtain direct images from the atomic structure of the bulk sample and to correlate this with the atomically resolved EELS information. In-situ heating of the material in a heating double tilt holder in the microscope columns allows us to simulate the highly reducing operating conditions for this oxygen conducting membrane material.
The promise of advanced technological applications in optical and electronic devices has led to a significant recent research effort in the structure-property relationships of defects in GaN. in particular, the major scientific issues arise from the high density of threading dislocations induced during thin film growth by film-substrate lattice mismatch. There is still debate as to the exact effect of these dislocations on the overall properties; they may or may not be electrically active and are thought to decrease the lifetime of devices. As such, a fundamental understanding of the electronic properties of these defects will facilitate the development of new and improved devices.
The analysis of the electronic structure of dislocations in GaN is performed here by a combination of atomic resolution electron energy loss spectroscopy (EELS) in the scanning transmission electron microscope (STEM) and multiple scattering (MS) simulations. Experimentally, a Z-contrast image of the dislocation core is obtained first1 and used to position the probe for EELS.
Electron loss near edge structure (ELNES) reflects transitions of inner shell electrons to site- and symmetry-projected unoccupied electronic states, which in a solid lie above the Fermi level and may be calculated using advanced electronic structure calculations. The direction of momentum transfer, q, imparted during the inelastic scattering process is dependent on the angle over which the scattered electrons are collected. It is usual to resolve the momentum transfer, into components parallel and perpendicular to the incident beam direction (q∥and q⊥). in a specimen region which is crystallographically anisotropic, the exact direction of the momentum transfer and hence energy states available to the excited electron will depend on the specimen orientation with respect to the incident electron beam. Practically, this can present problems where quantitative comparisons and/or modelling of electronic structure between different specimen regions at different orientations, or within a polycrystalline material, or even between different samples are required.
The advancement of metal-oxide-semiconductor (MOS) technology towards sub- 100nm device dimensions presents several technical difficulties. Nanoscaling in MOS devices is specifically governed by difficulties in the formation of ultrashallow junctions for the source/drain regions with the requirement of low resistance and low leakage currents. The use of a silicide (forming Schottky contacts at the source and drain) instead of the conventional ion implanted Si for the contacts allows a reduction in the contact area to be made, due to lower serial resistance per unit area of the silicide. According to the specific contact resistance dependence on the Schottky barrier height (ΦSB) and active dopant concentration (ND),
The properties of ceramic oxides being developed for such varied applications as fuel cells, ionic transporting membranes, high-Tc superconductors, ferroelectrics and varistors are dominated by the presence of grain boundaries. Key to controlling the electronic properties of the grain boundaries in these materials is a fundamental understanding of the complex relationship between structure, composition and local electronic structure. The ability to characterize and directly correlate these parameters on the atomic scale is afforded by the combination of Z-contrast imaging and electron energy loss spectroscopy (EELS) in the scanning transmission electron microscope (STEM). Furthermore, the recent development of in-situ heating capabilities in the JEOL 201 OF STEM/TEM permits atomic resolution analysis to be performed at elevated temperatures and the interactions of grain boundaries with the oxygen vacancies determined.
Figure 1 shows an example of the type of experiment that can be performed using these methods.
CdSe/ZnSe based semiconductor quantum dot (Q D) structures are a promising candidate for optoelectronic device applications. However, key to the luminescence properties is the cation distribution and ordering on the atomic level within the CdSe QDs/agglomerates. Here the Z contrast imaging technique in the scanning transmission electron microscope (STEM) is employed to study multisheet (Cd,Zn,Mn)Se QD structures. Since Z-contrast is an incoherent imaging technique, problems associated with strain contrast in conventional TEM are avoided an accurate size and composition determinations can be made.
For this work we used a JEOL JEM 201 OF field emission STEM/TEM. The sample was grown by molecular beam epitaxy in order to achieve vertical self-ordering of Cd rich quasi-2D platelet This sample comprises 8 sequences of 10 ML (2.83 nm)Zn0.9Mn0.1Se cladding layer and 0.3 ML (0.09 nm) CdSe sheet, a further 10 ML of Zn0.9Mn0.1Se, and a 50 nm ZnSe capping layer.
The heterogeneous catalytic system Pt/SiO2 is widely used in “three-way” catalysts, because of its highly selective catalytic reduction of NO by hydrocarbons at low operating temperatures. Although used effectively for more than a decade, in recent years it has become clear that the core phenomena of heterogeneous catalysis can occur at interfaces. in the work presented here, we seek to better understand the role of the atomic and electronic structure of interfaces in making particular reactions facile and moderating the stability and selectivity of a catalytic system.
We investigate model supported platinum catalysts by atomic resolution Z-contrast imaging and EELS using a 200 kV STEM/TEM JEOL2010F with a post column GIF. The combination of these techniques allows us to obtain direct images of the metal particle and its interface with the supporting SiO2, and to correlate that with the modulation of the Si L-edge fine structure.
Z-contrast images and electron energy loss spectra (EELS) were obtained from low angle grain boundaries in SrTiO3 and YBa2Cu3O7-x (YBCO). Z-contrast images are easy to interpret and especially useful for positioning the beam to acquire EELS data from small sample areas , because both these techniques can be performed simultaneously.
In high-temperature superconductors even a single grain boundary can reduce the critical current by up to four orders of magnitude. The band-bending model can quantitatively explain this phenomenon. YBCO is a hole-doped superconductor with about one hole per unit cell for optimum doping at x close to zero. It has a structure closely related to the perovskite structure, and Z-contrast images have shown that the dislocation cores are made up of similar structural units as in SrTiO3.[2,3] Our EELS measurements show clear evidence for band bending effects around isolated dislocation cores in an undoped 8° low angle grain boundary.
Gd3+ doped Ce oxides are very promising candidates as electrolytes for solid oxide fuel cells operating at ∼ 500 °C. For their successful commercial implementation, a full understanding of the defect chemistry in the bulk and at grain boundaries is essential. in particular, the contribution of the grain boundaries to the total ionic conductivity through such effects as the segregation of impurities, dopants and vacancies is of crucial importance. Here the effect of the atomic structure on the local electronic properties, i.e. oxygen coordination and cation valence at grain boundaries of the fluorite structured Gd0.2Ce0.8O2-x ceramic electrolyte is investigated by a combination of Z-contrast imaging and electron energy loss spectroscopy (EELS) in the JEOL 201 OF STEM (operating at 200keV, and aligned for a probe size ∼ 0.2 nm).
Preliminary O K- and Ce M45-edges were acquired from points in the grains (A and B) and grain boundary shown in Figure 1.
Yttria-stabilized zirconia (YSZ) has been the subject of many experimental and theoretical studies, due to the commercial applications of zirconia-based ceramics in solid state oxide fuel cells. Since the grain boundaries usually dominate the overall macroscopic performance of the bulk material, it is essential to develop a fundamental understanding of their structure-property relationships. Previous research has been performed on the atomic structure of grain boundaries in YSZ, but no precise atomic scale compositional and chemistry characterization has been carried out. Here we report a detailed analytical study of an  symmetric 24° bicrystal tilt grain boundary in YSZ prepared with ∼10 mol % Y2O3 by Shinkosha Co., Ltd by the combination of Z-contrast imaging and electron energy loss spectroscopy (EELS).
The experimental analysis of the YSZ sample was carried out on a 200kV Schottky field emission JEOL 201 OF STEM/TEM4.
In recent years, GaN and its alloys have been the subject of an intense global research effort to develop its optoelectronic properties in the blue-green region of the spectrum. Of particular interest has been the fact that despite a high density of threading dislocations, on the order of 108 to 1010 per cm2, thin film devices retain their ability to emit light. The origin of this behavior remains unclear, and it has even been suggested that reducing the number of defects by employing different growth techniques does not necessarily increase the crystal's lasing abilities. As research is now aiming to grow GaN on silicon (silicon has a large lattice-mismatch to GaN) in order to develop an inexpensive LED technology, dislocations are likely to remain a major issue. It is therefore essential that we develop a fundamental understanding of the electronic structure of these defects, in order to determine their effect on the properties.
The Perovskite structured ceramic (Lax,Sr1-x)(Fey,Cr1-y)O3-δ being developed for applications in oxygen transporting membranes. The permeability of this material is limited by the number of free ions, point-defects (oxygen vacancies) and electrons in the bulk. As any ordering of these unbound particles will restrict their mobility one key issue for controlling the membrane efficiency is the formation of ordered oxygen vacancies. In particular it is very likely, that at elevated temperatures ordered micro-domains progressively grow and asymptotically reach a stable equilibrium concentration. This is consistent with the observations of Kruidhof that below a specific order-disorder transition temperature equilibrium times of 30-40 h are required to attain steady-state conditions, irrespective of the thermal history of the sample.
We investigate the formation of ordered vacancies in (Lax,Sr1-x)(Fey,Cr1-y)O3-δ by atomic resolution Z-contrast imaging and electron energy-loss spectroscopy (EELS) using a 200 keV STEM/TEM JEOL2010L with a post column Gatan Image Filter (GIF).
CdTe/CdS thin film solar cells are being investigated extensively these days by many workers as an option for low cost photovoltaic applications . In order to achieve high efficiency solar cell it is important that the CdS film should have minimum possible structural defects and reasonably large grain size. The CdS films for CdTe/ CdS solar cell structure are mostly grown on glass substrates by chemical bath deposition (CBD). Although adherent, transparent and conformal films with index of refraction close to single crystal CdS can be grown by CBD, impurity inclusions and micropinholes are a problem there in. Very little work has been carried out to grow CdS films by thermal evaporation in vacuum. In the present work we have grown pure and CdCl2 doped CdS films on glass substrates by thermal evaporation and carried out microstructural investigations of these films using scanning electron microscopy.
Corning 7059 glass of 25.4 x 25.4 x 1.2 mm size were used as substrates for the deposition of CdS as well as CdCl2 doped CdS films.
Perovskite-type oxides with high electronic and ionic conductivity are very promising materials for use as dense ceramic membranes for oxygen separation. For the successful implementation of practical ceramic membranes, a full understanding of the parameters controlling the degree of non-stoichiometry, i.e. the defect chemistry is essential. A combination of Z-contrast imaging and electron energy loss spectroscopy (EELS) in the scanning transmission electron microscope (STEM) can be used to directly image crystal and defect structures and the effect of the structures on the local electronic properties (i.e. oxygen coordination and cation valence). Here the defect chemistry in SrCoO3-δ before and after a reduction treatment at high temperatures is investigated in the JEOL 201 OF STEM. This material is known to exist in a wide a variety of phases with different crystal structures, compositions and valence states of cobalt, and can be highly oxygen deficient.