It all started in Berlin in 1931 where Dr. Ernst Ruska built the first TEM with 2 magnetic lenses. Three years later a third lens was added and a resolution of l00nm was demonstrated, just enough to beat the light microscope by a factor of two. His achievements and vision was acknowledged and celebrated in 1986 when he was awarded the Nobel Prize for Physics. Philips’ commitment to electron microscopy dates back to the mid-1930s, when it collaborated in EM research programs with universities in the UK and the Netherlands. in 1949, the company introduced its first EM production unit, the EM 100 transmission electron microscope, which already was a significant step forward in terms of ease of use and reliability.

In fifty years the TEM has come a long way; enumerating all the milestones would be too lengthy.

What in the “real” world does this title mean? I would argue that every paper given at this meeting in some way reflects an application in the real world, thus rendering this paper and this symposium redundant. But then again, here we are. of course, every one using an instrument will insist that his application is in some way unique and therefore not a common, mundane, “real-world” one. The “real-world” for an academically motivated scientist may be quite different from the “real-world” of the commercially motivated scientist. What happens in an asbestos testing lab is quite different from the activities of a consulting group using the microscope to solve industrial problems. Every application is “real world”.. .but they most certainly may be different.

And so, where to begin? For a start, consider the following “real world” situations: 1. a University using a microscope to support the research activities of that University,

The cotton textile fiber is a field dried, single cellular, collapsed convoluted tube. It is covered with waxes, which are connected by ester linkages to pectins enmeshed in a basket weave structure of the cellulosic primary wall. Depending upon its variety, the mature cotton fiber contains between 0.5%and 1% wax by weight, and it is practically waterproof. The normal industrial method for cleaning cotton fabric involves three steps: de-sizing with amylase enzymes to remove starch sizing or boiling in an aqueous surfactant solution to remove polyvinyl alcohol (PVA) sizing; scouring with caustic soda to remove waxes; and bleaching with hydrogen peroxide to obtain uniform whiteness. The effluent from this process is environmentally toxic, but the process is necessary to prepare fabric for dyeing, durable press finishing, etc. Current research is directed towards the investigation of environmentally friendly methods of removing cotton waxes.

Trees can act as efficient biological filters to remove significant amounts of particulate pollution from urban atmospheres (Nowak, et al. 1994 ). Recent controlled environment studies have indicated that tree's ability in intercepting and removing particle pollution varies among species. Studies by Abdollahi et al. (2000) confirmed that there were significant differences among different tree species in intercepting particle pollution. Live Oaks (Quercus virginiana), River Birch ( Betula nigra),and Sugar hackberry (Celtis occidentalis) are statistically more efficient at capturing pollutant particles of less than 2.5 microns (PM2.5) than tree species such as Red Maple (Acer Rubrum),Southern Magnolia (Magnolia grandiflora),and Sycamore (Platanus occidentalis).Other Studies also suggested that the leaf surface morphology of these trees might play an important role in interception and removal of PM2.5.

The main objectives of this study were to quantify the relative ability of selected oak species (Quercus spp.) in removing particle pollution of less than 2.5 microns (PM2.5) and to characterize oak leaf surface morphology.

In the hierarchical model of soil structure, the lowest scale of structure is the combination of clays < 0.2 um diameter to form 2 um domains. to investigate the basis for soil structure, two highly weathered soils from Brazil (Oxisols) were selected and the < 2 um size fraction extracted by sedimentation for analysis. The first soil used in this study, classified as Xanthic Hapludox, was collected in 1991 at an EMBRAPA research station outside of Manaus, Brazil from a tropical forest site collected from the 0-8 cm depth. The second soil (0-20 cm depth) was sampled from a topographically flat area inside the Brasilia National Park, Brasilia D.F. Brazil by Dr. Flavio Vasconcelos.

The samples were analyzed by NMR spectroscopy, transmission electron microscopy, atomic force microscopy, and scanning electron microscopy. NMR spectroscopy revealed the organic materials within this size fraction consisted predominantly of polysaccharides.

Metasedimentary rocks of the Archean Quetico subprovince of the Superior province in northeastern Minnesota contain monazite that has undergone low-grade hydrothermal alteration and disseminated sulfide mineralization. The area contains multiply deformed, metasedimentary rocks with abundant granitic veins that were subjected to deep burial, deformation, and syntectonic Barrovian metamorphism ranging from kyanite-staurolite grade to sillimanite-muscovite grade. Continued deformation and concomitant granitic intrusion produced rapid decompression and a well-developed high-temperature, low-pressure thermal aureole adjacent to the granitic intrusive bodies. This second metamorphic event is characterized by mineral assemblages containing cordierite or andalusite after staurolite. Subsequent reburial of the area produced prennite/pumpellyite facies regional metamorphism that is widespread but only locally recognized.

The initial aim of this study was to determine the petrographic relationships between monazite, a light rare-earth phosphate, and the surrounding minerals as a basis for absolute age dating, by electron probe microanalyzer (EPMA), of deformation and related metamorphic events.

Green glauconite-like minerals from Weipa, Australia, which were previously known as glauconite, were determined to be unusual Fe-rich vermicuhte and Fe-rich smectite. This study revealed the structural and chemical nature of these unique phyllosilicates with HRTEM, AEM, SEM and XRD analysis.

The Fe-rich phyllosilicates comprising up to about 15 wt% of the rock occur with various amounts of quartz, mica, feldspar, low-Fe smectite, kaolinite, pyrite and siderite at about 30 meters depth in unweathered marine sediments of the Rolling Downs Formation at Weipa. The proportions of Fe-rich vermiculite and smectite decrease upward and become undetectable in the upper saprolite zone at about 23 m depth.

Two major morphologies of the Fe-rich phyllosilicates were observed. One is of tabular or granular detrital-shaped form (Fig.la); the other is platy or film-like, coating grains and occurring in matrix and fissures (Fig.lb).

A precise analysis of the biological remains is presented in the paper. A single-channel waveguide carbon dioxide laser is used in a process of ablation ‘ for the exposing of biological remains of mineralised organisms found in a sea slime used as a component in some technological process.

Many important applications of the laser base on the process of ablation. These include also so precise biomedical uses like structural studies of biomolecules. Among of the wide range of the laser devices the waveguide carbon dioxide lasers can be used in a precise biological investigations. A single-channel waveguide CO2 laser emits very easy the optical wave formed in a single, so called quasi-Gaussian, mode2. The distribution of the intensity of the laser output radiation in a basic Gaussian mode is shown in Figure 1. A high quality laser output beam in a basic Gaussian mode can be easy focused permitting a precise ablation of the investigated material in a very small area of 100 μm and less.

Confocal laser scanning microscopy (CLSM) has been used to study asphaltene aggregation kinetics by employing the microscope's automated acquisition to generate time-lapsed projection maps of aggregating asphaltenes in the autofluorescent matrix of crude oil. Heavy crude oils contain asphaltene particles resulting in the production of optically observable micron-sized asphaltene aggregates. These aggregates form as a result of attractive interactions induced by mixing the heavy crude oil with a poor solvent. This technique has been employed to determine the volume fraction of aggregated asphaltenes, ϕagg, and the time evolution of this phenomenon. The measurements cover a range of various concentrations of asphaltene volume fractions of the heavy asphaltenic oil, ϕm, from ϕm =0.001 to ϕm =0.4.

At each ϕm,after the mixtures have been made, approximately 20 μl of the crude oil is placed in a 20 μm deep flat-well quartz cell and immediately placed on a microscope stage.

Alloy development can range from purely empirical, trial-and-error efforts to very theoretical, based on either fundamental first-principles calculations or computational-modeling using various kinds of data base inputs. However, “real-world” efforts to improve or optimize complex engineering alloys often cannot afford the time or cost of either extreme approach. in the past 10-15 years, an alloy development and processing optimization methodology has been developed that utilizes strategic microanalytical data (both detailed microstucture and microcompositional information) as the critical input that then enables efficient and effective design of various kinds of alloys for improved high-temperature performance [1-6]. in many cases, first time tests produce outstanding high-temperature creep or creep-rupture results, and enable improvements without trading off one property for another. This invited paper will highlight several examples of significantly improved creep resistance obtained using such microstructural design.

This microstructural design methodology for high-temperature creep-resistance was initially developed for and demonstrated in austenitic stainless steels (Fe-14Cr-16Ni) designed for improved creep-strength and rupture resistance at 700°C and above for superheater and boiler tubing in advanced fossil power plants.

Conventional microanalytical tools, particularly analytical electron microscopy (AEM), electron probe microanalysis (EPMA), and powder x-ray diffraction (XRD), have been traditionally used in the development of new engineering alloys to determine the identity of phases in new materials, their composition, phase equilibria, and the subsequent effect on properties. Recently, there has been a growing effort in industry to reduce the cycle time (and lower the cost) associated with new material development. This is particularly true for the advanced alloys needed for high-temperature components in power generation and aerospace application. This has led first to the development of more rapid screening methodologies, such as combinatorial approaches, where a large number of compositions can be evaluated in parallel, or the diffusion multiple method, where multi-component phase space is investigated in a single experiment. These new approaches require new analysis tools that can rapidly assess crystal structure and composition in automated fashion.

The microstructural development in a Type 309 stainless steel weldment associated with a post-weld heat treatment of 30 h at 580°C has been studied using analytical electron microscopy (AEM). The purpose of post-weld thermal treatments is generally to relieve stresses within the weld, thereby improving performance. Microstructural stability during these thermal treatments is important for the weld; i.e., no deleterious phases should form. in this example, detailed microstructural analyses of a weldment in the as-welded and postweld heat-treated condition have been performed. Microstructural analyses were performed using Philips CM 12 and CM300-FEG analytical electron microscopes equipped with Oxford Instruments ISIS analyzers and LZ5 energy dispersive x-ray spectrometers, and a CM200-FEG analytical electron microscope equipped with a Gatan Image Filter (GIF).

As-Welded Condition:The microstructure of the weld was characterized by the presence of dislocated austenite (γ) and a network of delta (δ) ferrite.

The high temperature application of iron-based ferritic alloys is limited by their rapid decrease of yield strength at temperatures approaching 1000°C. It has been shown that mechanical-alloying (MA) to produce oxide dispersion-strengthened (ODS) ferritic alloys improves their high temperature mechanical properties. Prior characterization of such materials has shown that in certain as-processed alloys the original yttria oxide particles are replaced by nanoscale (2-5 nm diameter) clusters containing Ti, Y and O. As a result of the high density of these fine clusters, dislocation pinning produced a ∼10-fold increase in dislocation density relative to similar ODS materials not exhibiting the nanoscale clustering. The improved creep resistance of the clustered material was attributed both to the higher dislocation density, additional dislocation pinning and resistance to recovery during creep. The current work examines clustering in a related alloy, as well as the effects of high temperature creep on the stability of such clusters.

The microscopy effort within the Saint-Gobain R&D labs involves working with a wide variety of ceramic materials. Samples vary from routine QC type work, to manufacturing plant emergencies, to failure analysis, to marketing support. A typical sample will require a variety of techniques to provide a solution within a few working days. Working in such an environment it is essential that people are aware of the different analytical tools that can be utilized in a given situation. For the microscopists in our lab this means a working knowledge of the techniques that are close to our core competencies centered around optical microscopy and SEM; these include AFM, XRD, Auger, SIMS, and FTIR, which are all used in a complimentary fashion. The examples shown here are illustrative of the kinds of problems worked on and the interactive nature of the solutions.

XRD of a siliconized silicon carbide material showed that it contained a higher fraction of the beta phase than was expected.

Electron diffraction can be a very useful technique in solving real world structure-related problems. However, electron diffraction is much less widely used in industry compared to x-ray diffraction for several reasons. So far, application of electron diffraction has been limited to large-sized companies either to characterize newly synthesized materials in a research division or to directly support business activities in an analytical laboratory. New materials produced on a commercial scale are more and more complex with micro-, even nano-meter sized structures. Development of these materials on a commercial scale, for example, high temperature superconducting compounds, fullerenes, and giant magneoresistance devices [1-7], has increased demand for electron diffraction techniques considerably. Here, I would like to review how electron microscopists in industry solve their real world problems using electron diffraction techniques [8].

Unit cell determination. Unit cell parameters and atom coordinates of a crystal can be routinely determined by single crystal x-ray technique if the crystal is large enough (about 0.1 mm in size).

CdTe is a promising photovoltaic material due to its near optimum band gap and high absorption coefficient. Polycrystalline, thin-film CdTe/CdS solar cells have demonstrated an efficiency of 15.8%. High density of extended defects is often found in polycrystalline CdTe films grown by close-spaced sublimation (CSS). So far, most investigations of defects in CdTe have focused on epitaxially grown films, and the reported extended defects are mainly lamellar twins. However, epitaxially grown films generally have a different microstructure compared to CSS grown polycrystalline CdTe thin films. in this paper, we report our study of extended defects in CSSgrown polycrystalline CdTe thin films by high-resolution transmission electron microscopy (HRTEM). We found that the extended defects are mostly lamellar twins and stacking faults. The stacking faults always propagate across the grains, without ending at a partial dislocation inside the grains.

Polycrystalline CdTe is a promising candidate for solar cells due to its nearly ideal band-gap, high absorption coefficient, and ease of film fabrication. Small-area CdTe/CdS cells with efficiencies of 16.0% have been demonstrated. The structure of a typical CdTe/CdS solar cell (Figure 1) consists of a glass superstrate, on which a thin layer of SnO2 is deposited (front contact), n-type CdS, p-type CdTe, and a back contact. Prior to applying the back contact to the CdTe, etching of the CdTe surface using a mixture of nitric and phosphoric (NP) acids is normally needed. It is known that the etching depletes a crystalline CdTe surface of Cd and creates a Te-rich layer. Two effects of the Te-rich layer has been proposed, namely, forming a Te-CdTe low-series-resistance contact and improving CdTe device stability by the gettering of Cu. Thus, the NP etching is an important process in the CdTe device fabrication. in this paper, we report on transmission electron microscopy (TEM) study of the microstructure of the surface of NP etched CdTe thin films.

A technique for very thin silicon oxide measurements using energy filtered TEM (EFTEM) is presented and applied for BiCMOS technology optimization.

In advanced VLSI circuits, thin silicon oxide layers are used as critical part of active devices such as MOS or bipolar transistors (BiCMOS). Today the 2 nm thick gate oxides of the 0.12 urn generation MOS transistors can be controlled using high resolution TEM (HRTEM). However, for the next generations these measurements will become difficult or will necessitate Cs corrected microscopes'. For the NPN bipolar transistor very thin oxides (less than 0.5 nm) are used at the base-emitter interface to control the forward base (hole) current and improve the transistor current gain. This interface presents generally some roughness and the oxide control is impossible using HRTEM. in this communication we demonstrate a new technique for very thin oxide measurement using low loss energy filtered TEM (EFTEM).

Silicon-on-insulator (SOI) is becoming a key technology for low power electronics due to substantially reduced power consumption of electronic components, and a capability of compact circuit design which are not readily achievable in bulk silicon technology [1]. Separation by IMplantation of OXygen (SIMOX) is the most promising technology for fabricating SOI material. The basic SIMOX process consists of implantation of oxygen into the single crystalline silicon wafer and the subsequent high temperature annealing. Oxygen implantation at low doses does not form a continuous buried oxide (BOX) layer but leads to an inhomogeneous distribution of the oxygen precipitates during implantation process. The formation and growth of oxygen precipitates in low-dose SIMOX depend strongly on the implantation conditions such as oxygen dose, implantation temperature, annealing temperature and ramping rate [2,3]. During the subsequent annealing, Ostwald ripening of the precipitates takes place and the larger precipitates grow at the expanse of small ones until they coalesce to the buried oxide layer.

The spontaneous formation of so-called self-assembled quantum dots (SAQDs) during heteroepitaxial growth has attracted much recent interest because of potential device applications. Much attention has been directed towards the Ge/Si(001) system, in particular to characterize the island shape and size distributions as a function of growth conditions, i.e., Ge coverage and substrate temperature. Due to the lattice mismatch, a layer-to-island transition occurs at coverages greater than about 3 monolayers, and thereafter small, coherent hut clusters and larger coherent and incoherent dome clusters are observed. Interdiffusion of Si into the Ge islands as a strain-relief mechanism also occurs. Strategies for achieving better control of island size, shape, composition and separation continue to be sought. in this paper, we report a preliminary investigation of island growth in the alternative Ge/Si(l12) system.

The Ge/Si(112) samples were grown by molecular beam epitaxy using a Riber 2300 system equipped with a Ge Knudsen effusion cell.