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Goldstein, J. I.

Publications and source records attributed to Goldstein, J. I..

At least 19 records

Cooling History of Almahata Sitta Ureilite as Inferred from Transmission Electron Microscopy of Iron Metal

Almahata Sitta (AS) is a polymict breccia mainly composed of various ureilite lithologies with lesser chondritic lithologies [1]. In the ureilite lithologies, Fe metal is a common accessory phase present either as large grain boundary grains or small particles formed by reduction of olivine and pyroxene. In our earlier studies on grain boundary metals in one of AS fragments (#44) we found unique features never seen in other ureilites [2,3]. In order to further characterize these metal grains, we performed a detailed TEM study on a FIB section prepared from one of AS #44 grain boundary metals and here discuss its thermal history.

Mikouchi, T.

Microstructure and Thermal History of Metal Particles in CH Chondrites

Fe-Ni metal particles with smooth Ni, Co, and Cr zoning patterns, 8-13 wt.% Ni in the center of the particle to 3-5 wt% Ni at the rim, have been identified in several CR-clan (CH, Bencubbinlike, and CR) chondrites. These zoning patterns are broadly consistent with an origin by gas-solid condensation in the solar nebula at temperatures between approximately 1500 to 1300 K and fast cooling rates, 2 to 25 K/day. Apparently, this condensate metal was not melted during chondrule formation or affected significantly in the solid-state by alteration during parent body processing. Consideration of diffusional redistribution of Ni, Co, Cr and siderophile elements have further constrained the calculated condensation temperatures and cooling rates of the zoned condensates. These condensate metals have irregular shapes and vary in size from 50 to 350 m as revealed in some detail by optical and SEM techniques. In addition to zoned condensate particles, other types of metal particles have been observed. These include zoned condensates with exsolution-precipitates, unzoned homogeneous metal with no exsolution precipitates, unzoned metal exhibiting exsolution precipitates and high Ni metal grains.

Goldstein, J. I.

Metallographic Cooling Rate of IVA Irons Revisited

There is long standing problem reconciling the chemical evidence that the IVA iron meteorites formed in a core with the diverse cooling rates reported by several researchers. This large inferred range of cooling rates suggests that the IVA irons were distributed at different depths in a parent body with a complex structure when the Widmanstatten pattern formed. On the other hand, some researchers argued that the diverse cooling rates in group IVA result from inaccurate model parameters such as phase diagram, interdiffusion coefficients, and kamacite nucleation and growth mechanisms. In addition, the measured cooling rates may not apply for the same cooling temperature ranges, and the variation in the crystallographic orientations of the Widmanstatten plates on the analysis surface may result in inaccurate measurements of widths needed for the computer simulation models. We have revaluated the major parameters in computer model developed by Hopfe and Goldstein and measured cooling rates for the IVA irons. Such data are useful in evaluating whether these meteorites were part of a single core of a parent body during the formation of the Widmanstatten pattern.

Yang, J.

Nucleation of the Widmanstatten Pattern in Iron Meteorites

The Widmanstatten pattern develops at low temperatures during the evolution of the asteroids. We have studied the origin of the Widmanstatten pattern in order to obtain metallographic cooling rates in the temperature range (approx. 700 to 300 deg C). This paper summarizes our recent evaluation of the various mechanisms for the formation of the Widmanstatten pattern. All chemical groups of the iron meteorites are considered. We also propose a new mechanism for the formation of the Widmanstatten pattern in the low P metal phase of iron, stony-iron and stony meteorites. The results of this evaluation enables us to more accurately determine metallographic cooling rates particularly when incorporated with other recent advances in Fe-Ni and Fe-Ni (P saturated) phase diagrams and interdiffusion coefficients.

Yang, J.

High-Performance X-ray Detection in a New Analytical Electron Microscope

X-ray detection by energy-dispersive spectrometry in the analytical electron microscope (AEM) is often limited by low collected X-ray intensity (P), modest peak-to-background (P/B) ratios, and limitations on total counting time (tau) due to specimen drift and contamination. A new AFM has been designed with maximization of P. P/B, and tau as the primary considerations. Maximization of P has been accomplished by employing a field-emission electron gun, X-ray detectors with high collection angles, high-speed beam blanking to allow only one photon into the detector at a time, and simultaneous collection from two detectors. P/B has been maximized by reducing extraneous background signals generated at the specimen holder, the polepieces and the detector collimator. The maximum practical tau has been increased by reducing specimen contamination and employing electronic drift correction. Performance improvments have been measured using the NIST standard Cr thin film. The 0-3 steradian solid angle of X-ray collection is the highest value available. The beam blanking scheme for X-ray detection provides 3-4 times greater throughput of X-rays at high count rates into a recorded spectrum than normal systems employing pulse-pileup rejection circuits. Simultaneous X-ray collection from two detectors allows the highest X-ray intensity yet recorded to be collected from the NIST Cr thin film. The measured P/B of 6300 is the highest level recorded for an AEM. In addition to collected X-ray intensity (cps/nA) and P/B measured on the standard Cr film, the product of these can be used as a figure-of-merit to evaluate instruments. Estimated minimum mass fraction (MMF) for Cr measured on the standard NIST Cr thin film is also proposed as a figure-of-merit for comparing X-ray detection in AEMs. Determinations here of the MMF of Cr detectable show at least a threefold improvement over previous instruments.

Lyman, C. E.

A Comparison of Metallographic Cooling Rate Methods Used in Meteorites

The primary objective of this study was to test the postulate that cooling rates acquired from metal grains in chondrites are consistent with those from iron meteorites. Both types of metal occur in some Group IAB meteorites, which are mixtures of massive metal with well-developed Widmanstatten structures and chondritic inclusions with dispersed metal grains. The grains have textures and compositions similar to chondritic metal, including negligible P. The meteorites studied show little or no sign of shock reheating and textural evidence indicates that silicates and metal were mixed before Widmanstatten patterns formed during cooling. Cooling rates were obtained by comparing measured to modeled taenite grain or lamellae dimensions and central Ni contents. Modeling entails solving diffusion equations using experimental diffusion coefficients, phase relations, and bulk or local Ni and P contents, taking into account geometry, undercooling, and impingement. There is one set of parameters for grains and another, quite different set for Widmanstatten lamellae, including a factor of 30 difference in diffusion coefficients. Yet cooling rates obtained from Widmanstatten structures and metal grains in chondritic inclusions of the same meteorite are consistent; uncertainties in the best data are +/- 10 K/Ma, equivalent to a factor of 1 +/- 0.25. This agreement implies that the data and models are correct or contain fortuitously offsetting errors, which is quite unlikely. Cooling rates range from 40 K/Ma to 70 K/Ma in IAB meteorites that contain both grains and Widmanstatten structures. Rates based on grains in Ni-poor and Ni-rich meteorites lacking Widmansatten patterns expand the range from 30 K/Ma to perhaps 200 K/Ma. Cooling rates correlate with Ni content; Ni-poor meteorites have slower rates than Ni-rich ones. Evidently, IAB meteorites were radially distributed over greater than 30km in a body with a radius less than 50km. A comparison of the available Ar ages with cooling times inferred from the cooling rates suggests that the parent body cooled more slowly after the metallographic cooling rates were established.

Herpfer, Marc A.

The microstructure and formation of duplex and black plessite in iron meteorites

Two of the most common plessite structures, duplex and black plessite, in the taenite region of the Windmanstatten pattern of two iron meteorites (Grant and Carlton) are characterized using high-resolution electron microscopy and microanalysis techniques. Two types of gamma precipitates, found in the duplex plessite and black plessite regions, respectively, are identified, and their morphologies are described. The formation of the plessite structure is discussed using the information obtained in this study and results of a parallel investigation of decomposed martensitic Fe-Ni laboratory alloys.

Zhang, J.

Preliminary AEM study of the microstructure and composition of metal particles in ordinary chondrites

The purpose of this study is to examine the microstructure and composition of the metal particles in ordinary chondrites using analytical electron microscopy (AEM) techniques. Since the phases produced within the metal particles are very fine, the application of various AEM techniques for structural and chemical characterization is critical. However, thin specimen preparation for AEM study has proven very difficult because of the matrix silicate which is present. This is the first AEM study of the metal particles in chondrites. A type 6 chondrite, Saint Severin (LL6), was selected for examination because the metal phases have been reheated into the single phase taenite region (greater than 700 C), and cooled slowly to lower temperatures. A combination of electron optical instruments was employed including a field emission gun (FEG) JEOL 840F high resolution scanning electron microscope (HRSEM), a JEOL 6300F FEG-HRSEM, a Philips 400T AEM, and a JEOL 733 electron probe microanalyzer (EPMA).

Yang, C. W.

Applications of the Analytical Electron Microscope to Materials Science

In the last 20 years, the analytical electron microscope (AEM) as allowed investigators to obtain chemical and structural information from less than 50 nanometer diameter regions in thin samples of materials and to explore problems where reactions occur at boundaries and interfaces or within small particles or phases in bulk samples. Examples of the application of the AEM to materials science problems are presented in this paper and demonstrate the usefulness and the future potential of this instrument.

Goldstein, J. I.

X-Ray Microanalysis and Electron Energy Loss Spectrometry in the Analytical Electron Microscope: Review and Future Directions

This paper reviews and discusses future directions in analytical electron microscopy for microchemical analysis using X-ray and Electron Energy Loss Spectroscopy (EELS). The technique of X-ray microanalysis, using the ratio method and k(sub AB) factors, is outlined. The X-ray absorption correction is the major barrier to the objective of obtaining I% accuracy and precision in analysis. Spatial resolution and Minimum Detectability Limits (MDL) are considered with present limitations of spatial resolution in the 2 to 3 microns range and of MDL in the 0.1 to 0.2 wt. % range when a Field Emission Gun (FEG) system is used. Future directions of X-ray analysis include improvement in X-ray spatial resolution to the I to 2 microns range and MDL as low as 0.01 wt. %. With these improvements the detection of single atoms in the analysis volume will be possible. Other future improvements include the use of clean room techniques for thin specimen preparation, quantification available at the I% accuracy and precision level with light element analysis quantification available at better than the 10% accuracy and precision level, the incorporation of a compact wavelength dispersive spectrometer to improve X-ray spectral resolution, light element analysis and MDL, and instrument improvements including source stability, on-line probe current measurements, stage stability, and computerized stage control. The paper reviews the EELS technique, recognizing that it has been slow to develop and still remains firmly in research laboratories rather than in applications laboratories. Consideration of microanalysis with core-loss edges is given along with a discussion of the limitations such as specimen thickness. Spatial resolution and MDL are considered, recognizing that single atom detection is already possible. Plasmon loss analysis is discussed as well as fine structure analysis. New techniques for energy-loss imaging are also summarized. Future directions in the EELS technique will be the development of new spectrometers and improvements in thin specimen preparation. The microanalysis technique needs to be simplified and software developed so that the EELS technique approaches the relative simplicity of the X-ray technique. Finally, one can expect major improvements in EELS imaging as data storage and processing improvements occur.

Goldstein, J. I.

Definition of the Spatial Resolution of X-Ray Microanalysis in Thin Foils

The spatial resolution of X-ray microanalysis in thin foils is defined in terms of the incident electron beam diameter and the average beam broadening. The beam diameter is defined as the full width tenth maximum of a Gaussian intensity distribution. The spatial resolution is calculated by a convolution of the beam diameter and the average beam broadening. This definition of the spatial resolution can be related simply to experimental measurements of composition profiles across interphase interfaces. Monte Carlo calculations using a high-speed parallel supercomputer show good agreement with this definition of the spatial resolution and calculations based on this definition. The agreement is good over a range of specimen thicknesses and atomic number, but is poor when excessive beam tailing distorts the assumed Gaussian electron intensity distributions. Beam tailing occurs in low-Z materials because of fast secondary electrons and in high-Z materials because of plural scattering.

Williams, D. B.

An APFIM/AEM Study of Phase Decompositions in Fe-Ni Alloys at Low Temperatures

A combined atom probe field ion microscopy and analytical electron microscopy characterization has been performed on laboratory aged martensitic and austenitic specimens of FeNi and FeNiP alloys. These techniques revealed that the martensitic 24.1 and 28.6 at.% Ni alloys decomposed during aging for 1 year at 300 C to form face centered cubic precipitates of approx. 56 at.% Ni in a body centered cubic matrix containing approx. 20 at.% Ni. Some thin platelets were observed in the field ion micrographs of the austenitic Fe-42.9 at. % Ni alloy and the Fe-43.2 at.% Ni-0.44 at.% P alloy after aging at 400 and 350 C. Atom probe analysis revealed phosphorus clustering in the ternary alloy aged at 300 C.

Zhang, J.

The structure and composition of metal particles in two type 6 ordinary chondrites

The microstructure and composition of taenite particles were examined in two type-6 ordinary chondrites, Kernouve (H6) and Saint Severin (LL6), using reflected light microscopy and a combination of electron optical instruments. It was found that, in both meteorites, the taenite particles consisted of a narrow rim of high-Ni taenite and a central region of cloudy zone similar to those present in iron meteorites. The microstructure of the cloudy zone in Saint Severin was coarser than that in Kernouve , due to the higher Ni content and slower cooling rate of the former. Three microstructural zones were observed in the outer taenite rim of both meteorites, the origin of which is considered likely to be due to the presence of ordered domain boundaries or to the presence of two phases FeNi and FeNi3 in the high-Ni region of the outer taenite rim.

Holland-Duffield, C. E.

Electron microscopy study of the iron meteorite Santa Catharina

A characterization of the microstructural features of Santa Catharina (SC) from the millimeter to submicron scale is presented. The same specimen was examined using an optical microscope, a scanning electron microscope, an electron probe microanalyzer, and an analytical electron microscope. Findings include the fact that SC metal nodules may have different bulk Ni values, leading to different microstructures upon cooling; that SC USNM 6293 is the less corroded sample, as tetrataenite exists as less than 10 nm ordered domains throughout the entire fcc matrix (it is noted that this structure is the same as that of the Twin City meteorite and identical to clear taenite II in the retained taenite regions of the octahedrites); that SC USNM 3043 has a more complicated microstructure due to corrosion; and that the low Ni phase of the cloudy zone was selectively corroded in some areas and formed the dark regions, indicating that the SC meteorite corrosion process was electrochemical in nature and may involve Cl-containing akaganeite.

Zhang, J.

Spatial Resolution and Detectability Limits in Thin-Film X-Ray Microanalysis

The major advantages of performing x-ray microanalysis in the analytical electron microscope (AEM) are the high compositional spatial resolution and the elemental analysis sensitivity. Unfortunately, there is usually a trade-off between these two advantages. This paper discusses the factors involved in the optimization of both spatial resolution and sensitivity during x-ray microanalysis and shows the results of such optimization experiments for several AEM instruments.

Goldstein, J. I.

Ordering in the Fe-Ni system under electron irradiation

The disorder-order transformation was generated in a range of Fe-Ni alloys using 1 MeV electrons in a high voltage electron microscope. The experimental factors that influence the occurrence of the transformation were determined, and the critical disordering temperature, Tc, was determined as a function of composition. It was demonstrated that the irradiation enhanced the ordering reaction kinetics. A metastable, ordered phase transformation was not induced. From the results, it is possible to deduce new information about the Fe-Ni phase diagram below 350 C.

Reuter, K. B.

Determination of the Fe-Ni phase diagram below 400 C

Analytical EM techniques have been used to obtain a phase diagram for the Fe-Ni system below 400 C in the composition range from 0-52 wt pct Ni. The present diagram is consistent with all the phases observed in the Fe-Ni regions of meteorites. An asymmetric spinodal decomposition results in the expected two-phase isotropic microstructure. The present experimentally-determined miscibility gap below 400 C, located between 11.7 and 51.9 wt pct Ni at 200 C, is shown to be wider than the calculated miscibility gap.

Reuter, K. B.