Upon hot strip mill of titanium Interstitial Free (IF) steels, during cooling from austenite to ferrite region, the level of interstitial elements not removed by steelmaking process is dropped down by Ti that combines with N, C and S. Some authors [1-3] have reported that the traditional precipitation sequence TiN, TiS, Ti4C2S2 and TiC occurs with freestanding particles formed by nucleation and growth processes. Other authors [4] have indicated that the transformation from TiS to Ti4C2S2 may be considered as a hybrid of shear and diffusion, i.e., faulted Ti8S9 (9R) + 10[Ti] + 9[C] → 41/2Ti4C2S2 (or H for its hexagonal crystal structure). At low temperature (≤930°C), the stabilization process continues through epitaxial growth of carbides on H phase. to study the evolution of precipitation upon hot strip mill conditions, samples of a Ti - IF steel were subjected to double straining tests [5] by means of a computerized hot torsion machine, at 1000 °C and 920 °C, with strain rate of 1 s-1 and interpass times ranging from 0.5 to 100 s.

TEM has been used for semiconductor device characterization since the 1980's, when Marcus and Cheng first demonstrated the feasibility and utility of applying TEM to semiconductors. The frequency of use of TEM has accelerated briskly due to the continual shrinkage of devices as predicted by Gordon Moore and now documented in the SIA roadmap (http://public.itrs.net/Home.htm). TEM use has also grown due to application of FIB techniques which make possible high precision cross-sections of specific structures. This relentless shrinking has resulted in difficulties in preparing suitable specimens. Many of the features and interfaces in a device may be curved rather than planar, and as the radius of curvature begins to approach the thickness of a TEM specimen, it can result in “geometrical blurring” of features, both for imaging and microanalysis. The origin of this blurring is illustrated in Figure 1, where it can be seen that a single electron may pass through two different features, and as a result, they are not resolved.

The microscopy to support process development of Si-based semiconductors has consistently required state-of-the-art instrumentation. As the industry strains to achieve 1 OOnm design rules, this requirement has never been more pronounced. This paper presents TEM, SEM and FIB examples with a focus on using the instrumentation near the performance limit.

Transmission Electron Microscopy - The high contrast and high resolution images provided by the TEM have made this “research instrument” into the mainstay of the semiconductor analysis laboratory. For the vast majority of samples, both plan view and cross sections, precious little tilt is required. For cross sections, +/- 3 degrees is usually adequate to bring the silicon into (110) orientation and plan views are commonly made from polycrystalline films, which benefit more from choosing the right thickness than from tilt. Under appreciated is the benefit of very high resolution polepieces which have superior spherical and chromatic aberration coefficients producing real improvements in image quality.

Electron beam induced current (EBIC) is the common term used in the semiconductor industry for the failure analysis and yield enhancement of semiconductor devices using SEM to electrically pinpoint leakage sites. EBIC is a useful technique for locating defects in diodes, transistors, and capacitors where the scanning electron microscope beam is used to generate a signal and the sample is the detector. Often during yield enhancement efforts the failure analyst is asked to determine the mechanism for which a PC structure (which may contain as many as a few hundred thousand structures in one device) is failing tests. Blind cross sections rarely give evidence of the failure mechanism. EBIC can be used to pinpoint the bad site which is then precision cross-sectioned using the focused ion beam (FIB).

When an electron beam impinges on a semiconductor such as silicon, electron-hole pairs are created when the incident beam transfers enough energy to promote an electron from the valance band to the conduction band.

The analytical needs in semiconductor technology have grown under the increasing demands imposed by reduced critical dimensions, increased wafer size, and complexity. Optical visualization, localization and counting of particles and defects has been extended to morphological and chemical characterization owing to the shifting balance from quality control to root-cause defect analysis. This becomes increasingly important because, via knowledge of the particle defect material plus the process/ hardware features, it leads to a direct path for the particle culprit and a methodical defect reduction procedure.

We present here specific examples from Applied Materials development, particularly related to particles formed during poly Si etch and during two different cleaning procedures (a) NF3 rf process chamber clean and (b) pre-clean (before subsequent deposition) of SiON film via Ar+ sputtering. These cases include identification of Br-based particles after poly-gate etch, and attempts to classify a variety of Al-containing particles of differing origins caused by too aggressive cleaning.

Rechargeable Lithium ion batteries are widely used as portable power source in communication and computer technology, prospective uses include medical implantable devices and electric vehicles. The safety and cycle life of Li ion batteries is improved over that of batteries containing metallic lithium anodes because the insertion of Li between the crystal layers of both electrodes was proved to be safer than the electroplating of Li onto a metallic Lithium anode. in Li-ion batteries, the charge transport is governed by the oscillation of Li ions between anode and cathode. They are sometimes called “rocking-chair“ batteries. The most common materials for these batteries are lithiated carbons for anodes, and transition metal oxides (LixCoO2) as cathodes.

LixCoO2 has an ordered rhombohedral Rm structure consisting of alternating layers of Co-O-Li-O-Co. The capacity and energy density of the batteries is limited by the amount of Li that can be stored in the anode and cathode materials.

The unique physical and chemical properties of AgX (X=C1, Br, I) emulsion microcrystals (optical, solid state, transport, chemical and spectral sensitizations and development) account for their use as basic light quanta detectors in practical photography for over 150 years. in spite of the advances made in other recording systems, especially in electronic imaging, contemporary AgX-based photographic materials are still superior in sensitivity and resolution. Although the replacement of AgX-based imaging systems by electronic imaging was already predicted 20 years ago, their current world manufacturing level is now larger than ever. However, in order to be successfully incorporated into digital and hybrid information technologies for the new Millennium, AgX-based photographic materials should further improve their quantum efficiency and image quality. in order to achieve these objectives, the key components should be intentionally modified with a focus primarily at the nanostructural level.

Transmission electron microscopes have been built along with and guided by technological opportunities since the last five decades. Even though there are some “workhorse” type of microscopes, these instruments are still more or less built from the technological viewpoint and less from the viewpoint of ease of use in a wide range of applications. On the other hand, leading edge applications are the drivers for the development and the use of leading edge technology. The result then is a “race horse” which is of very limited benefit in “Real world”.

During the last decade computers have been integrated to build microscope systems. in most cases, however, computers still have to deal with obsolete electron optical ray path designs and thus, have to be used more to overcome the problems of imperfect optics and bad design of ray paths than to provide optimized “Real world” capabilities.

In the last two decades, microscopy, in particular transmission electron microscopy, has moved from the research environment into industry. As such, the user requirements of the microscopes have changed. Previously, users required the highest performance in all aspects of microscopy e.g. imaging, analytical capabilities, with little regard to other factors. Today, additional requirements are being placed on areas such as ease of use, reliability, high throughput, expanded sample requirements, and networking capabilities. However, the “high performance” aspects of the instrumentation are still a high priority to the end user. These user requirements cause microscope manufacturers a dilemma in many instances. It is not always possible to provide the “new” requirements while still maintaining the high performance of the instruments, at a “reasonable” cost. An example is the large sample requirements in scanning electron microscopes. Large stages are inherently more prone to vibration than smaller stages, and therefore adversely affect resolution.

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.