Multivariate Statistical Approach to Electron Back Scattered Diffraction
Ultramicroscopy
Abstract not provided.
Ultramicroscopy
Abstract not provided.
Acta Materialia
Abstract not provided.
Abstract not provided.
Abstract not provided.
Abstract not provided.
Materials Science and Technology Conference and Exhibition, MS and T'07 - "Exploring Structure, Processing, and Applications Across Multiple Materials Systems"
Pre-oxidized and glass-to-metal (GtM) sealed austenitic stainless steels were found to display a ferritic layer near the metal/oxide interface, as determined by electron backscatter diffraction (EBSD). Electron probe microanalysis (EPMA) showed that this layer was depleted in alloying elements due to the oxidation and sealing process. Characterization of the morphology suggested that it formed through the martensite transformation mechanism. Moreover, this observed layer was correlated to the composition gradient through published empirical relationships for martensite-start (Ms) temperatures. Due to Cr, Mn, and Si depletion during pre-oxidation and glass sealing, Ms temperatures near room temperature are possible in this surface region. Further support for a martensitic transformation was provided by thermochemical modeling. Possible detrimental ramifications of bulk composition, surface depletion, and phase transformations on GtM sealing are discussed. Copyright © 2007 MS&T'07®.
Proceedings of the 3rd International Brazing and Soldering Conference
An oxidation treatment, often termed "pre-oxidation", is performed on austenitic stainless steel prior to glass/metal joining to produce hermetic seals. The resulting thin oxide acts as a transitional layer and a source of Cr and other elements which diffuse into the glass during the subsequent bonding process. Pre-oxidation is performed in a low pO 2 atmosphere to avoid iron oxide formation and the final oxide is composed of Cr 2O 3, MnCr 2O 4 spinel, and SiO 2. Significant heat-to-heat variations in the oxidation behavior of 304L stainless steel have been observed, which result in inconsistent glass/metal seal behavior. The objectives of this work were to characterize the oxidation kinetics, the oxide morphology and composition, and the stainless steel attributes that lead to robust glass/metal seals. The oxidation kinetics were determined by thermogravimetric (TG) analysis and the oxide layers were characterized using metallography, SEM, focused ion beam (FIB) analysis, and image analysis. The results show that poor sealing behavior is associated with slower oxidation kinetics and a more continuous layer of SiO 2 at the metal/oxide interface. In addition, the effects of 304L heat composition on oxidation behavior will be discussed. Copyright © 2006 ASM International®.
Ceramic Engineering and Science Proceedings
An oxidation treatment, often termed "pre-oxidation", is performed on austenitic stainless steel prior to joining to alkali barium silicate glass to produce hermetic seals. The resulting thin oxide acts as a transitional layer and a source of Cr and other elements which diffuse into the glass during the subsequent bonding process. Pre-oxidation is performed in a low pO2 atmosphere to avoid iron oxide formation and the final oxide is composed of Cr2O3, MnCr2O4 spinel, and SiO2. Significant heat-to-heat variations in the oxidation behavior of 304L stainless steel have been observed, which result in inconsistent glass-to-metal (GTM) seal behavior. The objectives of this work were to characterize the stainless steel pre-oxidized layer and the glass/oxide/304L interface region after glass sealing. The 304L oxidation kinetics were determined by thermogravimetric (TG) analysis and the glass/metal seals characteristics were studied using sessile drop tests, in which wetting angles were measured and glass adhesion was analyzed. The pre-oxidized layers and glass/metal interface regions were characterized using metallography, focused ion beam (FIB) sectioning, scanning and transmission electron microscopy, and electron probe microanalysis (EPMA). The results show that poor glass sealing behavior is associated with a more continuous layer of SiO 2 at the metal/oxide interface.
Frictional contact results in surface and subsurface damage that could influence the performance, aging, and reliability of moving mechanical assemblies. Changes in surface roughness, hardness, grain size and texture often occur during the initial run-in period, resulting in the evolution of subsurface layers with characteristic microstructural features that are different from those of the bulk. The objective of this LDRD funded research was to model friction-induced microstructures. In order to accomplish this objective, novel experimental techniques were developed to make friction measurements on single crystal surfaces along specific crystallographic surfaces. Focused ion beam techniques were used to prepare cross-sections of wear scars, and electron backscattered diffraction (EBSD) and TEM to understand the deformation, orientation changes, and recrystallization that are associated with sliding wear. The extent of subsurface deformation and the coefficient of friction were strongly dependent on the crystal orientation. These experimental observations and insights were used to develop and validate phenomenological models. A phenomenological model was developed to elucidate the relationships between deformation, microstructure formation, and friction during wear. The contact mechanics problem was described by well-known mathematical solutions for the stresses during sliding friction. Crystal plasticity theory was used to describe the evolution of dislocation content in the worn material, which in turn provided an estimate of the characteristic microstructural feature size as a function of the imposed strain. An analysis of grain boundary sliding in ultra-fine-grained material provided a mechanism for lubrication, and model predictions of the contribution of grain boundary sliding (relative to plastic deformation) to lubrication were in good qualitative agreement with experimental evidence. A nanomechanics-based approach has been developed for characterizing the mechanical response of wear surfaces. Coatings are often required to mitigate friction and wear. Amongst other factors, plastic deformation of the substrate determines the coating-substrate interface reliability. Finite element modeling has been applied to predict the plastic deformation for the specific case of diamond-like carbon (DLC) coated Ni alloy substrates.
Abstract not provided.
Abstract not provided.
Abstract not provided.
Abstract not provided.
Abstract not provided.
Microscopy and Microanalysis
Abstract not provided.
Abstract not provided.
Abstract not provided.
Abstract not provided.
ASM Proceedings of the International Conference: Trends in Welding Research
Tubular specimens of the nitrogen-strengthened alloy 21Cr-6Ni-9Mn were instrumented with thermocouples and inertia welded using a wide range of axial forces and kinetic energies. It was determined that a linear relationship exists between upset and kinetic energy for a given axial force. Furthermore, the peak temperatures are inversely related to the applied axial force. Microstructural characterization was performed using optical and electron microscopy techniques. Ferrite was observed locally at the weld interface, and it was determined that the width of the ferrite zone could vary widely depending on the process parameters. Electron backscattered diffraction analysis revealed that the ferrite and austenite at the weld interface exhibit the Kurdjumov-Sachs orientation relationship, and suggests that a very large amount of ferrite is present during the welding process that subsequently transforms to austenite during cooling. The fracture toughness of inertia welds thermally charged in gaseous hydrogen was also measured. It was found that the hydrogen-assisted fracture susceptibility of the inertia welds was greater than that of the base metal, but less than that of 21Cr-6Ni-9Mn gas tungsten arc welds. Copyright © 2006 ASM International®.
The film stress of Ni films deposited at near-ambient temperatures from sulfamate electrolytes was studied. The particulate filtering of the electrolyte, a routine industrial practice, becomes an important deposition parameter at lower bath temperatures. At 28 C, elevated tensile film stress develops at low current densities (<10 mA/cm{sup 2}) if the electrolyte is filtered. Filtering at higher current densities has a negligible effect on film stress. A similar though less pronounced trend is observed at 32 C. Sulfate-based Ni plating baths display similar film stress sensitivity to filtering, suggesting that this is a general effect for Ni electrodeposition. It is shown that filtering does not significantly change the current efficiency or the pH near the surface during deposition. The observed changes in film stress are thus attributed not to adsorbed hydrogen but instead to the effects of filtering on the formation and concentration of polyborate species due to the decreased solubility of boric acid at near-ambient temperatures.
Abstract not provided.
Abstract not provided.
Electron backscattered diffraction (EBSD) is a widely used technique for both identifying the crystallographic phase and for mapping the orientation of crystalline materials on the micron length scale. Often the operating conditions necessary for phase identification are not suitable for orientation mapping and vice versa. In an effort to optimize the speed involved in the mapping technique, pattern quality is sacrificed and the wealth of information present in an EBSD pattern is compressed to basically 4 values: a matched phase and three Euler angles. However, ab initio identification of phases from EBSD patterns requires high quality patterns and fairly intense computation. Spectrum imaging is an analytical approach that may offer some solutions to the aforementioned problems. Spectrum imaging consists of collecting a whole spectrum at each pixel in a mapping style measurement. This large set of data is then analyzed using multivariate statistical analysis (MSA) techniques such as principle components analysis, multivariate curve resolution, or other least squares based techniques. The result of these calculations is a set of component spectral shapes with corresponding abundances that allow the analyst to extract the greatest amount of physically relevant information from an otherwise enormous data set. Spectrum imaging has been used successfully in EDX microanalysis (both in the SEM and TEM), TOF-SIMS, WDS, and EELS. To examine the potential benefits of the spectrum imaging approach for EBSD data, a series of basic experiments and calculations were run. Test data sets (20 x 20 patterns in .jpeg format) on polycrystalline Al and on the directionally solidified eutectic oxide, CoO/ZrO{sub 2}(CaO), were collected using the HKL Channel 5 system with a Nordlys detector under normal mapping conditions. The data was collected on a FEI dual beam FIB (model DB235) and a Zeiss (Supra 55 VP) SEM at 20keV for Al and CoO/ZrO{sub 2}(CaO), respectively. The data sets were analyzed according to the schematic shown in Figure 1. Each EBSD pattern was hough transformed, unzipped into a 1-D vector of channels with intensities ranging from 0-255, and then added to an overall data matrix. A range of treatments (edge/no edge detection, spatial simplicity/spectral simplicity, etc.) were examined to determine the optimal way of treating the data. The multivariate analyses were performed using the AXSIA code developed at Sandia National Laboratories. The MSA techniques were able to correctly identify individual grains in the Al sample and individual phases in the CoO/ZrO{sub 2}(CaO) sample. For each component EBSD pattern identified from the Al data, a corresponding color map of abundance can be seen which clearly corresponds to a single grain (Figure 2). The success in the CoO/ZrO{sub 2}(CaO) sample is particularly notable due to both phases sharing the Fm-3m space group which would confuse most autoindexing routines. The range of analytical treatments identified two extremes in results: a minimal number of components (patterns) with only kikuchi line positions present or a larger number of components with full intensity information present. The further application of these results to phase mapping will be discussed.
Abstract not provided.
Abstract not provided.
Abstract not provided.
Abstract not provided.
Abstract not provided.
Proposed for publication in the Journal of Materials Research.
Boron sub-arsenide, B{sub 12}As{sub 2}, is based on twelve-atom clusters of boron atoms and two-atom As-As chains. By contrast, SiC is a tetrahedrally bonded covalent semiconductor. Despite these fundamental differences, the basal plane hexagonal lattice constant of boron sub-arsenide is twice that of SiC. This coincidence suggests the possibility of heteroepitaxial growth of boron sub-arsenide films on properly aligned SiC. However, there are a variety of incommensurate alignments by which heteroepitaxial growth of B{sub 12}As{sub 2} on (0001) 6H-SiC can occur. In this study, we first used geometrical crystallographic considerations to describe the possible arrangements of B{sub 12}As{sub 2} on (0001) 6H-SiC. We identified four translational and two rotational variants. We then analyzed electron backscattered diffraction and transmission electron microscopy images for evidence of distinct domains of such structural variants. Micron-scale regions with each of the two possible rotational alignments of B{sub 12}As{sub 2} icosahedra with the SiC surface were seen. On a finer length scale (100-300 nm) within these regions, boron-rich boundaries were found, consistent with those between pairs of the four equivalent translational variants associated with a two-to-one lattice match. Boron-carbide reaction layers were also observed at interfaces between SiC and B{sub 12}As{sub 2}.
Metallic Phases in extraterrestrial materials are composed of Fe-Ni with minor amounts of Co, P, Si, Cr, etc. Electron microscopy techniques (SEM, TEM, EPMA, AEM) have been used for almost 50 years to study micron and submicron microscopic features in the metal phases (Fig. 1) such as clear taenite, cloudy zone, plessite, etc [1,2]. However lack of instrumentation to prepare TEM thin foils in specific sample locations and to obtain micro-scale crystallographic data have limited these investigations. New techniques such as the focused ion beam (FIB) and the electron backscatter electron diffraction (EBSD) techniques have overcome these limitations. The application of the FIB instrument has allowed us to prepare {approx}10 um long by {approx} 5um deep TEM thin sections of metal phases from specific regions of metal particles, in chondrites, irons and stony iron meteorites, identified by optical and SEM observation. Using a FEI dual beam FIB we were able to study very small metal particles in samples of CH chondrites [3] and zoneless plessite (ZP) in ordinary chondrites. Fig. 2 shows a SEM photomicrograph of a {approx}40 um ZP particle in Kernouve, a H6 chondrite. Fig. 3a,b shows a TEM photograph of a section of the FIB prepared TEM foil of the ZP particle and a Ni trace through a tetrataenite/kamacite region of the particle. It has been proposed that the Widmanstatten pattern in low P iron meteorites forms by martensite decomposition, via the reaction {gamma} {yields} {alpha}{sub 2} + {gamma} {yields} {alpha} + {gamma} in which {alpha}{sub 2}, martensite, decomposes to the equilibrium {alpha} and {gamma} phases during the cooling process [4]. In order to show if this mechanism for Widmanstatten pattern formation is correct, crystallographic information is needed from the {gamma} or taenite phases throughout a given meteorite. The EBSD technique was employed in this study to obtain the orientation of the taenite surrounding the initial martensite phase and the kamacite which forms as {alpha}{sub 2} or as Widmanstatten plates in a series of IVB irons. Fig. 4a,b shows EBSD orientation maps of taenite and kamacite from the Tawallah Valley IVB iron. We observe that the orientation of the taenite in the IVB meteorites is the same throughout the sample consistent with the orientation of the high temperature single phase taenite before formation of the Widmanstatten pattern.
Microanalysis is typically performed to analyze the near surface of materials. There are many instances where chemical information about the third spatial dimension is essential to the solution of materials analyses. The majority of 3D analyses however focus on limited spectral acquisition and/or analysis. For truly comprehensive 3D chemical characterization, 4D spectral images (a complete spectrum from each volume element of a region of a specimen) are needed. Furthermore, a robust statistical method is needed to extract the maximum amount of chemical information from that extremely large amount of data. In this paper, an example of the acquisition and multivariate statistical analysis of 4D (3-spatial and 1-spectral dimension) x-ray spectral images is described. The method of utilizing a single- or dual-beam FIB (w/o or w/SEM) to get at 3D chemistry has been described by others with respect to secondary-ion mass spectrometry. The basic methodology described in those works has been modified for comprehensive x-ray microanalysis in a dual-beam FIB/SEM (FEI Co. DB-235). In brief, the FIB is used to serially section a site-specific region of a sample and then the electron beam is rastered over the exposed surfaces with x-ray spectral images being acquired at each section. All this is performed without rotating or tilting the specimen between FIB cutting and SEM imaging/x-ray spectral image acquisition. The resultant 4D spectral image is then unfolded (number of volume elements by number of channels) and subjected to the same multivariate curve resolution (MCR) approach that has proven successful for the analysis of lower-dimension x-ray spectral images. The TSI data sets can be in excess of 4Gbytes. This problem has been overcome (for now) and images up to 6Gbytes have been analyzed in this work. The method for analyzing such large spectral images will be described in this presentation. A comprehensive 3D chemical analysis was performed on several corrosion specimens of Cu electroplated with various metals. Figure 1A shows the top view of the localized corrosion region prepared for FIB sectioning. The TSI region has been coated with Pt and a trench has been milled along the bottom edge of the region, exposing it to the electron beam as seen in Figure 1B. The TSI consisted of 25 sections and was approximately 6Gbytes. Figure 1C shows several of the components rendered in 3D: Green is Cu; blue is Pb; cyan represents one of the corrosion products that contains Cu, Zn, O, S, and C; and orange represents the other corrosion product with Zn, O, S and C. Figure 1 D shows all of the component spectral shapes from the analysis. There is severe pathological overlap of the spectra from Ni, Cu and Zn as well as Pb and S. in spite of this clean spectral shapes have been extracted from the TSI. This powerful TSI technique could be applied to other sectioning methods well.
Abstract not provided.
Abstract not provided.
Abstract not provided.
Proposed for publication in Welding Journal.
Abstract not provided.
Proposed for publication in Welding Journal.
The physical and welding a metallurgy of gadolinium- (Gd-) enriched Ni-based alloys has been examined using a combination of differential thermal analysis, hot ductility testing. Varestraint testing, and various microstructural characterization techniques. Three different matrix compositions were chosen that were similar to commercial Ni-Cr-Mo base alloys (UNS N06455, N06022, and N06059). A ternary Ni-Cr-Gd alloy was also examined. The Gd level of each alloy was {approx}2 wt-%. All the alloys initiated solidification by formation of primary austenite and terminated solidification by a Liquid {gamma} + Ni{sub 5}Gd eutectic-type reaction at {approx}1270 C. The solidification temperature ranges of the alloys varied from {approx}100 to 130 C (depending on alloy composition). This is a substantial reduction compared to the solidification temperature range to Gd-enriched stainless steels (360 to 400 C) that terminate solidification by a peritectic reaction at {approx}1060 C. The higher-temperature eutectic reaction that occurs in the Ni-based alloys is accompanied by significant improvements in hot ductility and solidification cracking resistance. The results of this research demonstrate that Gd-enriched Ni-based alloys are excellent candidate materials for nuclear criticality control in spent nuclear fuel storage applications that require production and fabrication of large amounts of material through conventional ingot metallurgy and fusion welding techniques.
Proposed for publication in Journal of Microscopy.
Abstract not provided.
Abstract not provided.
Abstract not provided.
Abstract not provided.
Journal of Microscopy
Recently, an electron backscatter diffraction (EBSD) system was developed that uses a 1024 × 1024 CCD camera coupled to a thin phosphor. This camera has been shown to produce excellent EBSD patterns. In this system, crystallographic information is determined from the EBSD pattern and coupled with the elemental information from energy or wavelength dispersive X-ray spectrometry. Identification of the crystalline phase of a sample is then made through a link to a commercial diffraction database. To date, this system has been applied almost exclusively to conventional, bulk samples that have been polished to a fiat surface. In this investigation, we report on the application of the EBSD system to the phase identification analysis of individual micrometre and submicrometre particles rather than fiat surfaces.
Materials Research Society Symposium - Proceedings
Interfaces play an important role in determining the effect of electric fields on the mechanism of the formation of spinel by solid-state reaction. The reaction occurs by the movement of phase boundaries but the rate of this movement can be affected by grain boundaries in the reactants or in the reaction product. Only by understanding these relationships will it be possible to engineer their behavior. As a particular example of such a study, MgIn2O4 can be formed by the reaction between single-crystal MgO substrate and a thin film of In2O3 with or without an applied electric field. High-resolution backscattered electron (BSE) imaging and electron backscattered diffraction (EBSD) in a scanning electron microscope (SEM) has been used to obtain complementary chemical and crystallographic information.
Abstract not provided.
Materials Research Society Symposium - Proceedings
EBSD in the SEM has been developed into a tool that can provide identification of unknown crystalline phases with a spatial resolution that is better than one micrometer. This technique has been applied to a wide range of materials. Use of the HOLZ rings in the EBSD patterns has enabled the reduced unit cell to be determined from unindexed EBSD patterns. This paper introduces EBSD for phase identification and illustrates the technique with examples from metal joining and particle analysis. Reduced unit cell determination from EBSD patterns is then discussed. © 2001 Materials Research Society.
Welding Journal Research Supplement
The weld solidification and cracking behavior of sulfur bearing free machining austenitic stainless steel was investigated for both gas-tungsten arc (GTA) and pulsed laser beam weld processes. The GTA weld solidification was consistent with those predicted with existing solidification diagrams and the cracking response was controlled primarily by solidification mode. The solidification behavior of the pulsed laser welds was complex, and often contained regions of primary ferrite and primary austenite solidification, although in all cases the welds were found to be completely austenite at room temperature. Electron backscattered diffraction (EBSD) pattern analysis indicated that the nature of the base metal at the time of solidification plays a primary role in initial solidification. The solid state transformation of austenite to ferrite at the fusion zone boundary, and ferrite to austenite on cooling may both be massive in nature. A range of alloy compositions that exhibited good resistance to solidification cracking and was compatible with both welding processes was identified. The compositional range is bounded by laser weldability at lower Cr{sub eq}/Ni{sub eq} ratios and by the GTA weldability at higher ratios. It was found with both processes that the limiting ratios were somewhat dependent upon sulfur content.
Nanotechnology is based on the ability to create and utilize materials, devices and systems through control of the matter at the nanometer scale. If successful, nanotechnology is expected to lead to broad new technological developments. The efficiency of energy conversion can be increased through the use of nanostructured materials with enhanced magnetic, light emission or wear resistant properties. Energy generation using nanostructured photovoltaics or nanocluster driven photocatalysis could fundamentally change the economic viability of renewable energy sources. In addition, the ability to imitate molecular processes found in living organisms may be key to developing highly sensitive and discriminating chemical and biological sensors. Such sensors could greatly expand the range of medical home testing as well as provide new technologies to counter the spread of chemical and biological weapons. Even the production of chemicals and materials could be revolutionized through the development of molecular reactors that can promote low energy chemical pathways for materials synthesis. Although nanotechnologies hold great promise, significant scientific challenges must be addressed before they can convert that promise into a reality. A key challenge in nanoscience is to understand how nano-scale tailoring of materials can lead to novel and enhanced functions. The authors' laboratory, for example, is currently making broad contributions in this area by synthesizing and exploring nanomaterials ranging from layered structures for electronics/photonics to novel nanocrystalline catalysts. They are even adapting functions from biological molecules to synthesize new forms of nanostructured materials.
An overall trend toward smaller electronic packages and devices makes it increasingly important and difficult to obtain meaningful diffraction information from small areas. X-ray micro-diffraction, electron back-scattered diffraction (EBSD) and Kossel are micro-diffraction techniques used for crystallographic analysis including texture, phase identification and strain measurements. X-ray micro-diffraction primarily is used for phase analysis and residual strain measurements. X-ray micro-diffraction primarily is used for phase analysis and residual strain measurements of areas between 10 {micro}m to 100 {micro}m. For areas this small glass capillary optics are used for producing a usable collimated x-ray beam. These optics are designed to reflect x-rays below the critical angle therefore allowing for larger solid acceptance angle at the x-ray source resulting in brighter smaller x-ray beams. The determination of residual strain using micro-diffraction techniques is very important to the semiconductor industry. Residual stresses have caused voiding of the interconnect metal which then destroys electrical continuity. Being able to determine the residual stress helps industry to predict failures from the aging effects of interconnects due to this stress voiding. Stress measurements would be impossible using a conventional x-ray diffractometer; however, utilizing a 30{micro}m glass capillary these small areas are readily assessable for analysis. Kossel produces a wide angle diffraction pattern from fluorescent x-rays generated in the sample by an e-beam in a SEM. This technique can yield very precise lattice parameters for determining strain. Fig. 2 shows a Kossel pattern from a Ni specimen. Phase analysis on small areas is also possible using an energy dispersive spectrometer (EBSD) and x-ray micro-diffraction techniques. EBSD has the advantage of allowing the user to observe the area of interest using the excellent imaging capabilities of the SEM. An EDS detector has been used for simultaneous element identification which enhances phase identification of unknowns. The x-ray area detector also allows for rapid microstructure information including crystallite orientation and size by directly observing the diffraction rings. These techniques allow for small area analysis that in the past would have been difficult if not impossible to obtain. The future development in x-ray optics and the use of synchrotron sources will allow for the potential of nondestructive submicron x-ray diffraction analysis.
Welding Journal (Miami, Fla)
The solidification behavior and resultant solidification cracking susceptibility of autogenous gas tungsten arc fusion welds in Alloy HR-160 was investigated by Varestraint testing, differential thermal analysis and various microstructural characterization techniques. The alloy exhibited a liquidus temperature of 1387 °C and initiated solidification by a primary L→γ reaction in which Ni, Si and Ti segregated to the interdendritic liquid and cosegregated to the γ dendrite cores. Chromium exhibited no preference for segregation to the solid or liquid phase during solidification. Solidification terminated at ≈1162 °C by a eutectic-type L→[γ+ (Ni,Co)16(Ti,Cr)6Si7] reaction. The (Ni,Co)16(Ti,Cr)6Si7] phase is found to be analogous to the G phase that forms in the Ni-Ti-Si and Co-Ti-Si ternary systems, and similarities are found between the solidification behavior of this commercial multicomponent alloy and the simple Ni-Si and Ni-Ti binary systems. Reasonable agreement is obtained between the calculated and measured volume percent of the [γ+(Ni,Co)16(Ti,Cr)6Si7] eutectic-type constituent with the Scheil equation using experimentally determined k values for Si and Ti from electron microprobe data. The alloy exhibited a very high susceptibility to solidification cracking in the Varestraint test. This is attributed to a large solidification temperature range of 225 °C and the presence of 2-5 vol-% solute-rich interdendritic liquid that preferentially wets the grain boundaries and interdendritic regions.
A methodology has been established to predict the effect of atmospheric corrosion on the reliability of plastic encapsulated microelectronic (PEM) devices. New experimental techniques were developed to directly characterize the Al/Au wirebond interface where corrosion primarily occurs. A deterministic empirical model describing wirebond degradation as a function of environmental conditions was generated. To demonstrate how this model can be used to determine corrosion effects on device reliability, a numerical simulation was performed on a three-lead voltage reference device. Surface reaction rate constants, environmental variables and the defect characteristics of the encapsulant were treated as distributed parameters. A Sandia-developed analytical framework (CRAX{trademark}) was used to include uncertainty in the analysis and directly calculate reliability.
A database of mechanical properties for weldment fusion and heat-affected zones was established for AerMet{reg_sign}100 alloy, and a study of the welding metallurgy of the alloy was conducted. The properties database was developed for a matrix of weld processes (electron beam and gas-tungsten arc) welding parameters (heat inputs) and post-weld heat treatment (PWHT) conditions. In order to insure commercial utility and acceptance, the matrix was commensurate with commercial welding technology and practice. Second, the mechanical properties were correlated with fundamental understanding of microstructure and microstructural evolution in this alloy. Finally, assessments of optimal weld process/PWHT combinations for cotildent application of the alloy in probable service conditions were made. The database of weldment mechanical properties demonstrated that a wide range of properties can be obtained in welds in this alloy. In addition, it was demonstrated that acceptable welds, some with near base metal properties, could be produced from several different initial heat treatments. This capability provides a means for defining process parameters and PWHT's to achieve appropriate properties for different applications, and provides useful flexibility in design and manufacturing. The database also indicated that an important region in welds is the softened region which develops in the heat-affected zone (HAZ) and analysis within the welding metallurgy studies indicated that the development of this region is governed by a complex interaction of precipitate overaging and austenite formation. Models and experimental data were therefore developed to describe overaging and austenite formation during thermal cycling. These models and experimental data can be applied to essentially any thermal cycle, and provide a basis for predicting the evolution of microstructure and properties during thermal processing.