Application of extraction replicas and analytical electron microscopy to precipitate phase studies

Extraction replicas provide a powerful extension of AEM techniques for analysis of fine precipitates. In many cases, replicas allow more accurate analyses to be performed and, in some cases, allow unique analyses which cannot be performed in-foil. However, there are limitations to the use of extraction replicas in AEM, of which the analyst must be aware. Many can be eliminated by careful preparation. Often, combined AEM studies of precipitates in-foil and on extraction replicas provide complementary and corroborative information for the fullest analysis of precipitate phases

Effects of proton irradiation on the microstructure and microchemistry of type 304L stainless steel

A research program has been undertaken to determine the origins of irradiation-assisted stress corrosion cracking (IASCC) in austenitic alloys in light water reactors, and the effect of impurities on IASCC susceptibility. Controlled purity alloys of 304L stainless steel were irradiated with protons at 400[deg]C to a dose of 1 dpa and analyzed via Auger electron spectroscopy (AES) and scanning transmission electron microscopy (STEM). The alloys investigated were an ultra-high purity (UHP) alloy and UHP alloys containing phosphorus (UHP + P), sulfur (UHP + S), or silicon (UHP + Si). Microstructural and microchemical changes were quantified and compared with literature results for other irradiating species. Following irradiation, the alloys showed dislocation loop formation and growth, "black dot" loops, and a change in the nature of the dislocation network. AES and STEM microchemical analysis of the alloys revealed Cr depletion of up to 6 at% and Ni enrichment of up to 6.6 at% at the grain boundaries of the alloys, with more segregation observed in the alloys containing impurities than in the UHP alloy. Significant grain boundary enrichment of P and Si in the UHP + P and UHP + Si alloys, respectively, was also observed. The results of the analyses of proton-irradiated samples are shown to compare favorably with previous studies on samples irradiated with neutrons at or near LWR conditions.Peer Reviewedhttp://deepblue.lib.umich.edu/bitstream/2027.42/30554/1/0000187.pd

Beam-broadening effects in STEM/EDS measurement of radiation-induced segregation in high-purity 304L stainless steel

Radiation-induced segregation (RIS) is the spatial redistribution of elements at defect sinks such as grain boundaries and free surfaces during irradiation. This phenomenon has been studied in a wide variety of alloys and has been linked to irradiation-assisted stress corrosion cracking (IASCC) of nuclear reactor core components. Therefore, accurate determination of the grain boundary composition is important in understanding its effects on environmental cracking. Radiation-induced segregation profiles are routinely measured by scanning-transmission electron microscopy using energy-dispersive X-ray spectroscopy (STEM-EDS) and Auger electron spectroscopy (AES). Because of the narrow width of the segregation profile (typically less than 10-nm full width at half-maximum), the accuracy of grain boundary concentration measurements using STEM/EDS depends on the characteristics of the analyzing instrument, specifically, the excited volume in which x-rays are generated. This excited volume is determined by both electron beam diameter and the primary electron beam energy. Increasing the primary beam energy in STEM/EDS produces greater measured grain boundary segregation, as the reduced electron beam broadening a smaller excited volume. In this work, the effect of beam broadening is assessed on segregation measurements in a 304L stainless steel sample irradiated with 3.2 MeV protons at 400 C to doses of 3.0 and 0.1 dpa. The STEM/EDS measurements are also compared to measurements made using AES

Quantitative analysis of radiation-induced grain-boundary segregation measurements

Radiation-induced and precipitation-induced grain-boundary segregation profiles are routinely measured by scanning-transmission electron microscopy using energy-dispersive X-ray spectroscopy (STEM-EDS). However, radiation-induced grain-boundary segregation (RIS) profiles achieved at low and moderate temperatures are exceedingly narrow, typically less than 10 nm full width at half maximum. Since the instrumental spatial resolution can be a significant fraction of this value, the determination of grain boundary compositions poses a formidable challenge. STEM-EDS and Auger electron spectroscopy (AES) measurements are reported, performed on controlled-purity alloys of type 304L stainless steel irradiated with 3.4 MeV protons to 1 displacement per atom at 400[deg]C. Because of statistical noise and the practical lower limit on the step size in STEM, deconvolution of the measured data does not yield physical results. An alternative analysis of STEM data is presented. Numerical calculations of RIS profiles are convoluted with the instrumental broadening function and modified iteratively to fit the data, yielding a "best estimate" profile. This "best estimate" is convoluted with the Auger intensity profile to yield a simulated AES measurement, which is compared with the actual AES measurement to provide an independent test of the validity of the "best estimate". For impurities with a narrow segregation profile and an Auger electron escape depth of one monolayer, a combination of STEM and AES data allows a determination of the width of the segregated layer. It is found that, in an ultrahigh-purity alloy doped with P, the latter is essentially contained in a single monolayer.Peer Reviewedhttp://deepblue.lib.umich.edu/bitstream/2027.42/31453/1/0000374.pd

Delamination and damage progression in a composite laminate subjected to bending using multicontinuum theory

10.2514/6.2011-1860Collection of Technical Papers - AIAA/ASME/ASCE/AHS/ASC Structures, Structural Dynamics and Materials Conference-CPSC