We report the first combined atom‐probe tomography (APT) and transmission electron microscopy (TEM) study of a kamacite–tetrataenite (K–T) interface region within an iron meteorite, Bristol (IVA). Ten APT nanotips were prepared from the K–T interface with focused ion beam scanning electron microscopy (FIB‐SEM) and then studied using TEM followed by APT. Near the K‐T interface, we found 3.8 ± 0.5 wt% Ni in kamacite and 53.4 ± 0.5 wt% Ni in tetrataenite. High‐Ni precipitate regions of the cloudy zone (CZ) have 50.4 ± 0.8 wt% Ni. A region near the CZ and martensite interface has <10 nm sized Ni‐rich precipitates with 38.4 ± 0.7 wt% Ni present within a low‐Ni matrix having 25.5 ± 0.6 wt% Ni. We found that Cu is predominantly concentrated in tetrataenite, whereas Co, P, and Cr are concentrated in kamacite. Phosphorus is preferentially concentrated along the K‐T interface. This study is the first precise measurement of the phase composition at high spatial resolution and in 3‐D of the K‐T interface region in a IVA iron meteorite and furthers our knowledge of the phase composition changes in a fast‐cooled iron meteorite below 400 °C. We demonstrate that APT in conjunction with TEM is a useful approach to study the major, minor, and trace elemental composition of nanoscale features within fast‐cooled iron meteorites.

We present a specimen preparation procedure for atom-probe tomography using SemGlu from Kleindiek Nanotechnik, an adhesive that hardens under electron beam irradiation. The SemGlu adhesive is used in place of focused-ion-beam-induced deposition of organo-metallic Pt, W, or C to form a bond between the sample and the substrate during the specimen preparation procedure. We demonstrate the utility of this adhesive-based specimen preparation technique with a correlated atom-probe tomography-scanning transmission electron microscopy study of the iron-nickel alloy kamacite (ferrite, ɑ-iron) in the Bristol iron meteorite and two steel specimens.

Extraterrestrial chrome spinel and chromite extracted from the sedimentary rock record are relicts from coarse micrometeorites and rarely meteorites. They are studied to reconstruct the paleoflux of meteorites to the Earth and the collisional history of the asteroid belt. Minor element concentrations of Ti and V, and oxygen isotopic compositions of these relict minerals were used to classify the meteorite type they stem from, and thus to determine the relative meteorite group abundances through time. While coarse sediment‐dispersed extraterrestrial chrome‐spinel (SEC) grains from ordinary chondrites dominate through the studied time windows in the Phanerozoic, there are exceptions: We have shown that ~467 Ma ago, 1 Ma before the breakup of the L chondrite parent body (LCPB), more than half of the largest (>63 μm diameter) grains were achondritic and originated from differentiated asteroids in contrast to ordinary chondrites which dominated the meteorite flux throughout most of the past 500 Ma. Here, we present a new data set of oxygen isotopic compositions and elemental compositions of 136 grains of a smaller size fraction (32–63 μm) in ~467 Ma old pre‐LCPB limestone from the Lynna River section in western Russia, that was previously studied by elemental analysis. Our study constitutes the most comprehensive oxygen isotopic data set of sediment‐dispersed extraterrestrial chrome spinel to date. We also introduce a Raman spectroscopy‐based method to identify SEC grains and distinguish them from terrestrial chrome spinel with ~97% reliability. We calibrated the Raman method with the established approach using titanium and vanadium concentrations and oxygen isotopic compositions. We find that ordinary chondrites are approximately three times more abundant in the 32–63 μm fraction than achondrites. While abundances of achondrites compared to ordinary chondrites are lower in the 32–63 μm size fraction than in the >63 μm one, achondrites are approximately three times more abundant in the 32–62 μm fraction than they are in the present flux. We find that the sources of SEC grains vary for different grain sizes, mainly as a result of parent body thermal metamorphism. We conclude that the meteorite flux composition ~467 Ma ago ~1 Ma before the breakup of the LCPB was fundamentally different from today and from other time windows studied in the Phanerozoic, but that in contrast to the large size fraction ordinary chondrites dominated the flux in the small size fraction. The high abundance of ordinary chondrites in the studied samples is consistent with the findings based on coarse extraterrestrial chrome‐spinel from other time windows.