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Structural and mineralogical significance of meteoritic craters, including mineral paragenesis, high pressure polymorphs, microfractures, and quartz lamellae
Bivariant eutectic alloys, located on a liquidus surface within the Ni-Cb-Cr-Al quaternary, were identified which permitted the production of aligned delta Ni3Cb lamellae within a nichrome matrix containing the fcc precipitate gamma prime Ni3Al. The volume fraction of delta and gamma prime could be varied significantly by compositional changes. After directional solidification certain alloys possessed improved ductility and corrosion resistance with respect to the Ni3Al-Ni3Cb eutectic, while their values of tensile and creep strength approached or exceeded those for the Ni3Al-Ni3Cb pseudobinary system. The mechanical properties of the directionally solidified alloy, Ni-19.7 wt % Cb-6.0 wt % Cr-2.5 wt % Al, were evaluated. Its longitudinal strength in tension and creep was found to be superior to all advanced nickel base superalloys. It is thus demonstrated that useful properties for gas turbine airfoil applications can be achieved by reinforcing a strong and tough gamma nichrome matrix containing precipitated gamma prime by a strong lamellar intermetallic compound having greater strength at elevated temperature.
Monovariant eutectic alloys, located on the liquidus trough between the binary eutectic gamma, Ni - delta, Ni3Cb and the ternary eutectic gamma, Ni - gamma-prime, Ni3Al - delta, Ni3Cb, were identified which permitted the production of aligned lamellae within a nickel solid solution matrix containing the precipitate gamma-prime. These alloys exhibited great insensitivity in their composite microstructures to solidification parameters such as growth rate temperature gradient, and were found to be remarkably uniform in composition along their length.
By means of a screening and solidification optimization study of certain alloys located on the gamma-sigma liquidus surface within the Ni-Cb-Cr-Al system, alloys with high temperature properties superior to those of all known superalloys were defined. One alloy, Ni - 19.7w/o Cb - 6.0w/o Cr - 2.5w/o Al, directionally solidified at 3 cm/hr met or exceeded each program goal. A second alloy, Ni-21.75 w/o Cb-2.55 w/o Al, although deficient in its inherent oxidation resistance, met the other program goals and combined a remarkable insensitivity of composite microstructure to solidification parameters with excellent low temperature toughness. This investigation demonstrated that useful properties for gas turbine airfoil application have been achieved by reinforcing a strong and tough gamma solid solution matrix containing precipitated gamma prime by a lamellar intermetallic compound Ni3 Cb having greater strength at elevated temperature.
By means of a compositional and heat treatment optimization program based on the quaternary gamma/gamma prime-delta, a tantalum modified gamma/gamma prime-delta alloy with improved shear and creep strength combined with better cyclic oxidation resistance was identified. Quinary additions, quaternary adjustments, and heat treatment were investigated. The tantalum modified gamma/gamma prime-delta alloy possessed a slightly higher liquidus temperature and exhibited rupture strength exceeding NASA VIA by approximately three and one-half Larson-Miller parameters (C = 20) above 1000 C. Although improvements in longitudinal mechanical properties were achieved, the shear and transverse strength property goals of the program were not met and present a continuing challenge to the alloy metallurgist.
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Introduction: Presolar grains preserve isotopic, chemical and microstructural records of physical and chemical processing, and formation mechanisms within a vast range of evolved stellar systems, the interstellar medium, solar nebula and their parent bodies. These evolutionary records are preserved at the micrometric to atomic scale, requiring coordinated studies to expand our understanding of evolutionary processes occurringthroughout ours and external stellar systems [1]. NanoSIMS enabled rapid in situ identification and isotopic characterisation of presolar grains and their stellar origins using 17O/16O and 18O/16O, and 13C/12C isotopic ratios [1]. Coordination with transmission electron microscopy (TEM) revealed crystallographic and localised contextual relationships and quantitively constrained their major and minor compositions [1]. However, trace elements cannot be quantified, the most sensitive geochemical tracers of environmental conditions, essential to unravelling the chemical record of their evolutionary pathway and parent stellar systems [2-3] . Furthermore, owing to the combination of technical limitations (only 5 – 7 isotopes can be measured per NanoSIMS run) and their small grain sizes of 100 nm < 3 μm (with rare exceptions in nanodiamonds (2 nm ≤) and SiC (< 40 μm)), the number of measurable isotopes per grain volume is limited [1,3] . Through more comprehensive isotopic studies of presolar grains, NanoSIMS studies have shown the importance of the latter, identifying Fe and Mg as important indicators of nuclear synthetic processing and their stellar origins, respectively [4- 5]. Coordination of NanoSIMS and Atom Probe Tomography (APT) revealed morphological signatures, and isotopic and chemical signatures at major to trace levels without requirements for preselection of elements [6]. However, crystallographic signatures in localized contextual relationships cannot be measured. Consequently, coordination of NanoSIMS, TEM and APT is essential to gain access to almost all contextual, structural and geochemical signatures within each presolar grain.Transmission electron microscopy requires a 100 nm thin lamella which is unstable in APT and would not produce any viable data. Atom probe tomography requires a needle-shaped specimen which when measured in TEM removes the local context, impacts the quality of the TEM diffraction images due to the shank angle of the needle, and can alter the chemistry of beam sensitive materials from the higher degree of surface exposure at the tip. To address these issues, we developed METIS-Fa (Multi-technical measurements of Electron Transparent materials using an Indium Sandwich - a FIB approach). A novel method which enables coordination of NanoSIMS, TEM and APT for generalized and targeted studies of individual grains, including beam sensitive materials, without compromising sample preparation requirements for TEM and APT. This method requires only indium and a Focus Ion Beam (FIB), minimizing the movement of fragile materials while still enabling preparation of TEM lamella into APT needles. Samples: Initial experimental development and testing of the method occurred at Astromaterials Research and Exploration Science (ARES), Johnson Space Centre (JSC), NASA and APT measurements and needle preparation occurred at JdLC, Curtin University. Synthetic silicate samples were used as analogs for presolar silicates when performing a trial run of the method. Samples were extracted from a polished thin section created at JSC, NASA, comprised of 38 wt.% Si, 17 wt.% FeO, 13 wt.% MgO, 12 wt.% Al, 11 wt.% Ca based on electron microprobe analysis (EMPA) [8] . Experimental details, pressure and temperature conditions were presented in [8] and references therein. Testing of the capability to target individual grains in mineral matrices using this method for acquisition in APT, measured matrix regions in meteoritic thin sections of primitive meteorites. These meteorites and their identified presolar grains for future targeted studies are detailed in [9]. Techniques: The TEM-FIB lamella were prepared using a FIB. An e-beam assisted pt deposition was used as a protective coating for the synthetic and meteoritic samples. When targeting individual grains, a secondary e-beam assisted pt deposition button is placed over the desired grain before the protective coating to denote its location. A JEOL 2500SE field-emission TEM was used for high-resolution imaging, energy-dispersive X-ray (EDX) and electron diffraction data.TheMETIS-Fa method was experimentally designed, tested and executed using a FIB at ARES, JSCNASA. Needles for APT were prepared using the Tescan Lyra3 GM Dual Beam Focus Ion Beam (FIB) Field Emission SEM (FE-SEM) at the JdLC, Curtin University. Atom probe tomography measurements were conducted using a CAMECA Local Electrode Atom Probe, LEAP 4000X HR. Two pure indium needles were analyzed initially to constraining acquisition parameters and stability under the beam. Manual acquisition was required to maintain evaporation of specimen’s at the apex and monitor interactions with measurement parameters. Experimental Design: Indium foil is pressed onto an Al stub with a pneumatic press and mounted into the FIB adjacent to the TEM-FIB lamella of interest. Using a FIB, two indium slices (5 μm x ~300 nm x 3 μm) are extracted from indium foil and aligned with the TEM-FIB lamella before touching the TEM-FIB lamella. Each slice is then attached through cold welding to the FIB-TEM lamella. This approach eliminates the need for chemical treatments and proved effective for aligning the Indium within the region of interest for APT, holding it in place for up to 4 days during testing.Once both indium slices are attached within their pre-determined region per grain targeting requirements, they are gradually melted onto the FIB-TEM lamella.When targeting a specific grain, measurements should be taken of the pt button and its distance from edge to edge of the lamella before and after sandwiching. A secondary button should be placed over the same region after the Indium slices have been attached to improve precision when preparing APT needles. Results: Figure 1 shows two indium slices melted onto a FIB-TEM lamella, adding additional bulk for preparation into APT needles as shown in Figure 2 [7] . The latter was essential so samples could be measured in TEM and APT without compromising sample preparation requirements and consequently data quality and acquisition stability. METIS-Fa proved effective forimproving geometry. Figure 3 shows a successful APTrun of the synthetic silicate. EMPA, TEM and APTshowed no chemical alterations. During targetingtesting, a solar silicate grain was successfully identifiedand measured in TEM, and prepared into an APTneedle. However, the indium was melted too long during sample preparation, causing expansion andformation of internal porosity leading to sample loss.Conclusion: METIS-Fa greatly expands the number of isotopic and chemical signatures measured per grain volume, and enables measurements of contextual, structural, crystallographic, isotopic and geochemical signatures within individual grains. Gaining access to such a vast range of evolutionary signatures required for expanding our understanding of external stellar and planetary systems and the evolution of our solar system. This method was designed for application to a vast range of phases including being sensitive materials and thus provides a way for coordination of NanoSIMS, TEM and APT not just for the study of presolar grains and by extension primitive astromaterials, but studies in a vast range of other fields including the geosciences and material sciences.Acknowledgments: Thankyou to ARES, JSC, NASA; JdLC Curtin University and Space Science Technology Centre for the use of laboratory facilities and funding [confirm].
Presolar grains are remnants of evolved stellar systems preserved within primitive extraterrestrial materials. They are important for studying physical and chemical processing, and formation mechanisms occurring within the interstellar medium, Solar Nebula and their parent stellar environments [1]. Our recent work has shown coordinated nano-scale Secondary Ion Mass Spectrometry (NanoSIMS) and Atom Probe Tomography (APT) can show isotopic and chemical signatures at major to trace levels, morphological signatures, and regional contextual relationships [2,3]. Previous studies have shown Transmission Electron Microscopy (TEM) of Focus Ion Beam (FIB) TEM lamella, can provide localized contextual relationships, crystallographic information and chemical information [1]. Coordinating NanoSIMS, TEM, and APT could gain access to almost all contextual, structural and geochemical signatures within each presolar grain. However, this has proved challenging owing to the preparation requirements for TEM and APT. For example, studying specimen prepared as APT needles in TEM removes the local context, the higher degree of surface exposure can alter the chemistry of beam sensitive materials, and the shank angle of the needle can impact the quality of TEM diffraction images. We designed a new FIB method which takes a 100 nm thick FIB-TEM lamella and sandwiches it between two indium slices (5 μm x ~300 nm x 3 μm). The indium is melted onto the lamella surface using the electron beam (Fig 1). This process adds bulk to the lamella, making it more amenable to APT needle formation (Fig 2). Consequently, samples can be prepared per the optimal requirements for each technique improving data quality, acquisition stability, and access to the signatures and relationships summarised earlier. This technique can be used for measuring multiple phases across a TEM lamella and targeting an individual phase. For example, a presolar grain identified in NanoSIMS could be targeted, studied in TEM and then indium sandwiched with its precise location in the TEM lamella marked using a Pt button for preparation of an APT needle and atomic scale acquisition. [1] A. M. Davis (2014) Meteorites and cosmochemical processes, 1. [2] Nevill N. et al. (2023) LPSC, 54, #1707. [3] Nevill N. et al. (2023) LPSC, 54, #1714.
The results of intensive studies indicate that shock-metamorphic effects, characteristic of meteorite impact and virtually identical to those observed in Apollo samples, are common in fragments of the Luna-16 soil sample from Mare Fecunditatis. Two types of shock effects are present: (1) deformation and partial melting features in rock and mineral fragments (1-2 percent of fragments); and (2) heterogeneous glasses and glassy breccias produced by shock melting (70-80 percent of fragments). Shock effects were observed in pyroxene (deformation twin lamellae, multiple planar shock lamellae, extreme mosaicism, partial isotropization); in plagioclase (planar shock lamellae, complete isotropization to form maskelynite); and in basalt fragments (plagioclase isotropization, selective partial melting). The glasses exhibit several characteristics of shock melting, especially: (1) diversity in chemical composition; (2) association with shock mineral fragments and Ni-Fe spherules; and (3) heterogeneous schlieren and incipient fusion of mineral inclusions. Two types of source rocks are present in the Luna-16 sample; basaltic (85-90 percent) and feldspathic (10-15 percent). The basaltic rocks are predominant and generally occur as unshocked fragments, indicating that they form the bedrock underlying Mare Fecunditatis.
Thin sections prepared from Apollo sample 14310 have been examined with 100-kV transmission electron microscopy. The sample is composed principally of anorthite and pyroxene. The anorthites fall into two categories. The transitional anorthites that show the characteristic 'c' type diffraction maxima are characterized by very fine antiphase domain structures and some fine twinning. The body-centered anorthites that show no 'c' reflections are characterized by an absence of fine twinning and a less well-defined antiphase domain structure. Although both orthopyroxene and clinopyroxenes are reported in sample 14310, only clinopyroxenes were observed in this study and all show exsolution structures. The augite exsolved in pigeonite commonly is along lamellae parallel to (100), although (001) lamellae are also present. This unusual orientation was verified by diffraction patterns. The pigeonite commonly shows antiphase domains, attributed to stacking errors when the sample inverted from its high-temperature disordered form. In augite as the host phase, the pigeonite lamellae contain very complex structures including antiphase domains.
Quartz grains displaying multiple sets of planar features are described from numerous Cretaceous-Tertiary (K-T) boundary clays and claystones at both marine and nonmarine depositional sites around the world. All these sites also show anomalously high amounts of iridium and enrichments of other siderophile elements in cosmic ratios within these boundary units. This combination of mineralogical and geochemical features are used in support of an impact hypothesis for the end-Cretaceous event. Recently, it was suggested that some combination of explosive and nonexplosive volcanism associated with the formation of the Deccan traps in India could be responsible for the mineralogy and geochemistry seen in the K-T boundary units. Besides the obvious contradition of simultaneous explosive and nonexplosive volcanism from one locality during an instant of geologic time, there remains the difficulty of spreading both iridium (and trace elements in cosmic proportions) and quartz grains around the world by volcanic (atmospheric) transport. In addition, the ability of volcanism to produce the type of shock metamorphism seen in minerals at the K-T boundary was not demonstrated. Multiple sets of shock lamellae in quartz are considered characteristic of shock metamorphism in rocks at the sites of known impact craters and are the type of deformation seen in quartz from K-T boundary clays and claystones. Single sets of poorly defined lamellae described from rare quartz grains in certain volcanic deposits are characteristic of tectonic deformation and do not correspond to the shock lamellae in quartz from K-T sediments and impact structures. So-called shock mosaicism in quartz and feldspar grains described from volcanic deposits can result from many processes other than shock metamorphism, and therefore is not considered to be an effect characteristic solely of shock. The mineralogy of shock-metamorphosed grains at the K-T boundary also argues against a volcanic origin.
The effect produced by shock loading (to peak pressures of 12 and 24) on deformed synthetic quartz containing a dislocation and abundant bubbles and small inclusions was investigated, and the relationships between preexisting dislocation density shock lamellae in the target material were examined. The resultant material was found to be inhomogeneously deformed and extremely fractured. Results of TEM examinations indicate that no change in dislocation density was caused by shock loading except in regions containing shock lamellae, where the dislocation density was lowered. The shock-induced defects tend to nucleate on and be controlled by preexisting stress concentrators; shock lamellae, glassy veins, and most curviplanar defects form in tension, presumably during release. An extremely mobile silica fluid is formed and injected into fractures during release, which forcibly removes crystalline fragments from vein walls. It is concluded that shock deformation in quartz is dominated by fracture and melting.
Two alloys, NASAIR 100 and a modified NASAIR 100 called Alloy 3, were run as turbine blades in an experimental ground-based Garrett TFE731 engine for up to 200 hours. The stress induced directional coarsening of gamma-prime (rafting) that developed during engine testing was analyzed and compared to previous research from laboratory tests. The blades were found to have formed a lamellar structure, the lamellae being normal to the centrifugal stress axis over much of the span. However, near the surfaces, the blades were found to have formed lamellae parallel to the centrifugal stress axis for certain cycles. Representative photomicrographs of the blades and the effects of stress and temperature on lamellae formation are shown.
Thus far, detailed petrologic studies of shock metamorphism have been performed on samples recovered from laboratory experiments and on a few natural impactites. The loading history of these samples is quite different: In particular, laboratory experiments spend only a short time (less than 1 microsec) at peak pressure, whereas natural impactites may have stress pulses from 0.1 - 1 ms. On the other hand, laboratory experiments have known stress histories; natural impactites do not. Natural samples are also subjected to thousands or millions of years of postshock annealing and/or weathering. A useful intermediate case is that of nuclear detonation. Stress pulses for these events can reach 0.1 ms or higher, and samples are obtained in pristine condition. All three types of loading produce stresses of hundreds of kilobars. Samples studied were taken from the Sedan nulcear test site, and consist of a coarse-grained granodiorite containing quartz, K-feldspar, cordierite, and hornblende. Samples were studied optically in this section, then were thinned with an ion mill and studied by transmission electron microscopy (TEM). Optically, quartz and K-feldspar displayed numerous sets of planar deformation features (PDF's) identical to the nondecorated PDF's seen in laboratory samples and many natural impactites. TEM study showed that the PDF's in quartz and feldspar corresponded to densely packed wide transformation lamellae identical to those described in laboratory studies. The transformation lamellae in both minerals were amorphous, with no sign of high-pressure phases. In the case of K-feldspar only, narrow sublamellae extended outward from some wide lamellae. Quartz, which was more abundant and studied more extensively, contained no shock-induced dislocations. Some planar features were also seen in cordierite, but could not be identified due to rapid beam damage. No shock defects were seen in hornblende in TEM. The shock-induced defects present at the Sedan site are very similar to those seen in shock recovery experiments, and also to those present at certain natural events (e.g., Meteor Crater). This suggests that shock deformation in quartz is not strongly dependent on shock pulse duration, and that laboratory recovery experiments are useful simulations of natural impact events.
Mineralogy of kirschsteinite exsolution in olivine from Antarctic meteorite LEW86010 has been studied by single crustal X-ray diffraction technique. The LEW86010 olivine crystals have exsolution lamellae of kirschteinite about 15 microns wide. Determination of crystallographic orientation of exsolved kirschsteinite in an olivine grain has been made. Weak reflections of exsolved kirschsteinite share common crystallographic orientation with the host olivine. The cell dimensions of the exsolved phase (a - 4.87 plus or minus 0.05A, b - 11.14 plus or minus 0.10A, c - 6.36 plus or minus 0.05A) and intensities were in well accord with those of kirschsteinite previously reported. Oriented section perpendicular to the a axis shows exsolution lamellae in two directions parallel to (031) and (031). The lamellae are up to 10 microns in width and spacings between them are usually 50-100 microns.
The Zaoyang ordinary chondrite fell as a single 14.15-kg mass in Hubey province (China) in October 1984 and was classified as a non-brecciated H5 chondrite, shock facies b. Cooling rate in pyroxenes can be calculated down to about 1000 C by using fine textures and at still lower temperatures (700 to 200 C) by intracrystalline ordering processes. The crystal chemistry of clinopyroxene and orthopyroxene from the matrix of the H5 Zaoyang chondrite has been investigated by X-ray structure refinement and detailed microprobe analysis. By comparison with terrestrial pyroxenes cell and polyhedral volumes in clino- and orthopyroxenes show a low crystallization pressure. Fe(2+) and Mg are rather disordered in M1 and M2 sites of clino- and orthopyroxenes; the closure temperatures of the exchange reaction are 600 and 512 C respectively, which is consistent with a quite fast cooling rate, estimated of the order of one degree per day. The closure temperature for the intercrystalline Ca-Mg exchange reaction for clino- and orthopyroxene showing clinopyroxene lamellae about 10 microns thick. Kinetic evaluations based on the thickness of exolved lamellae give a cooling rate of not more than a few degrees per 10(exp 4) years. The different cooling rates obtained from Fe(2+)-Mg intracrystalline partitioning and exolution lamellae suggest an initial episode of slow cooling at 900 C, followed by faster cooling at temperatures of 600-500 C at low pressure conditions. The most probable scenario of the meteorite history seems that the exolved orthopyroxene entered the parental chondrite body after exolution had taken place at high temperature. Subsequent fast cooling occurred at low temperature after the formation of the body.
Sampling cores requires the controlled breakoff of the core at a known location with respect to the drill end. An additional problem is designing a mechanism that can be implemented at a small scale, yet is robust and versatile enough to be used for a variety of core samples. The new design consists of a set of tubes (a drill tube, an outer tube, and an inner tube) and means of sliding the inner and outer tubes axially relative to each other. Additionally, a sample tube can be housed inside the inner tube for storing the sample. The inner tube fits inside the outer tube, which fits inside the drill tube. The inner and outer tubes can move axially relative to each other. The inner tube presents two lamellae with two opposing grabbing teeth and one pushing tooth. The pushing tooth is offset axially from the grabbing teeth. The teeth can move radially and their motion is controlled by the outer tube. The outer tube presents two lamellae with radial extrusions to control the inner tube lamellae motion. In breaking the core, the mechanism creates two support points (the grabbing teeth and the bit tip) and one push point. The core is broken in bending. The grabbing teeth can also act as a core retention mechanism. The praying mantis that is disclosed herein is an active core breaking/retention mechanism that requires only one additional actuator other than the drilling actuator. It can break cores that are attached to the borehole bottom as
MIL 03346 is one of the most mesostasis-rich nakhlites [1] and thought to have equilibrated at oxygen fugacities near the fayalite-magnetite-quartz oxygen (FMQ) buffer ([2,3]). Studies of FeTi oxides in nakhlites have led to additional constraints on their equilibration temperatures and fO2s [4,5,6,7]. Comparison of these results to fO2s calculated for shergottites indicates that nakhlites are among the most oxidized samples from the martian meteorite suite [2]. The mesostasis of MIL 03346 contains skeletal titanomagnetite. Several scientists noticed several years ago (e.g. [8]) that this titanomagnetite contains very fine oxidation-driven exsolution lamellae (Figure 1). However, the lamellae are so small that they cannot be characterized by electron microprobe analysis (EMPA). Here we select several areas for focused ion beam (FIB) extraction, prepare transmission electron microscopy (TEM) foils, and identify and analyze the lamellae using TEM at the Johnson Space Center (JSC). The resulting analyses are combined with previous work on nakhlites to interpret the thermal and oxidation history of this meteorite group.