scholarly journals Anaerobic Microscopic Analysis of Ferrous Saponite and Its Sensitivity to Oxidation by Earth’s Air: Lessons Learned for Analysis of Returned Samples from Mars and Carbonaceous Asteroids

Minerals ◽  
2021 ◽  
Vol 11 (11) ◽  
pp. 1244
Author(s):  
Natsumi Noda ◽  
Shohei Yamashita ◽  
Yoshio Takahashi ◽  
Megumi Matsumoto ◽  
Yuma Enokido ◽  
...  
Keyword(s):  
Microscopic Analysis ◽  
Structural Rearrangement ◽  
Lessons Learned ◽  
Air Exposure ◽  
X Ray ◽  
Dwarf Planets ◽  
Submicron Scale ◽  
Scanning Transmission ◽  
Before And After ◽  
Short Time

Ferrous saponite is a secondary mineral that can be used to reveal the redox state of past aqueous environments on Mars. In mineralogical analyses for ferrous saponite formed in laboratory simulations or contained in future returned samples from Mars, its oxidation by the Earth’s air could be problematic due to the high redox sensitivity. Here, we performed micro X-ray diffraction and scanning transmission X-ray microscopy analyses for a single particle of synthesized ferrous saponite without any exposure to air. The sample was reanalyzed after air exposure for 10–18 h to assess the adequacy of our anoxic preparation/measurement methods and the impacts of air on the sample. We found that the crystal structures agreed with ferrous saponite, both before and after air exposure; however, ferrous iron in saponite was partially oxidized, at least until 0.1–1 μm from the surface, after air exposure at the submicron scale, forming micro-vein-like Fe(III)-rich features. Together with our results of infrared spectroscopy of ferrous saponite, we showed that oxidation of octahedral iron occurred rapidly and heterogeneously, even in a short time of air exposure without any structural rearrangement. Since ferrous saponite is expected to exist on carbonaceous asteroids and icy dwarf planets, our methodology is also applicable to mineralogical studies of samples returned from these bodies.

Advances in Scanning Transmission X-Ray Microscopy for Elucidating Soil Biogeochemical Processes at the Submicron Scale

2017 ◽  
Vol 46 (6) ◽  
pp. 1166-1174 ◽  
Author(s):  
Jason W. Stuckey ◽  
Jianjun Yang ◽  
Jian Wang ◽  
Donald L. Sparks
Keyword(s):  
Biogeochemical Processes ◽  
X Ray ◽  
Submicron Scale ◽  
Scanning Transmission

Analytical Microscopic Analysis of Precipitates in Hastelloy Alloy C-276

1981 ◽  
Vol 39 ◽  
pp. 280-281
Author(s):  
M. Raghavan ◽  
B. J. Berkowitz ◽  
J. C. Scanlon
Keyword(s):  
Microscopic Analysis ◽  
Scanning Transmission Electron Microscope ◽  
Second Phase ◽  
Precipitation Reaction ◽  
X Ray Diffraction ◽  
Corrosion Properties ◽  
X Ray ◽  
Transmission Electron ◽  
Second Phase Particles ◽  
Scanning Transmission

The present investigation was conducted to characterize the second phase particles in Hastelloy C-276 using an analytical Scanning Transmission Electron Microscope in order to understand their effect on the mechanical and Stress Corrosion properties of the alloy. Investigation in our 1aboratoryO) and previous published reports(2-4) have identified two types of precipitation reactions in this alloy. At temperatures in the range of 300-650°C, the alloy precipitates an ordered phase of the type Ni2(Cr, Mo)(1,2). This precipitation reaction is homogeneous with no preferential precipitation at the grain boundaries or twin boundaries. At temperatures above 650°C, several precipitate phases were observed to nucleate heterogeneously at boundaries and using X-ray diffraction techniques, the precipitates were previously identified as the μ, M6C and P phases(3-4). The present investigation was carried out to determine the composition of these second phase particles and this article describes the characterization of these precipitates using X-ray microanalysis and microdiffraction techniques.

Scanning transmission X-ray microscopic analysis of purified melanosomes of the mouse iris

Micron ◽  
2006 ◽  
Vol 37 (8) ◽  
pp. 689-698 ◽  
Author(s):  
Michael G. Anderson ◽  
Tamás Haraszti ◽  
Greg E. Petersen ◽  
Sue Wirick ◽  
Chris Jacobsen ◽  
...  
Keyword(s):  
Microscopic Analysis ◽  
X Ray ◽  
Scanning Transmission

scholarly journals Redox-Chemistry of Environmental Biofilms Probed on the Submicron Scale by in-situ Electrochemistry Scanning Transmission (soft) X-ray Microscopy

2018 ◽  
Vol 24 (S2) ◽  
pp. 502-505
Author(s):  
Martin Obst ◽  
Pablo Ingino ◽  
Adam Hitchcock ◽  
Vinod Prabu ◽  
Aude Picard
Keyword(s):  
Redox Chemistry ◽  
X Ray ◽  
Submicron Scale ◽  
Scanning Transmission

Evaluation of Freezing Methods by Low Temperature X-Ray Diffraction

1977 ◽  
Vol 35 ◽  
pp. 330-333
Author(s):  
T. Gulik-Krzywicki ◽  
M.J. Costello
Keyword(s):  
Biological Materials ◽  
Molecular Organization ◽  
X Ray Diffraction ◽  
Glass Capillary ◽  
X Ray ◽  
Rate Dependent ◽  
Before And After ◽  
Freeze Etching ◽  
Diffraction Patterns ◽  
Set Up

Freeze-etching electron microscopy is currently one of the best methods for studying molecular organization of biological materials. Its application, however, is still limited by our imprecise knowledge about the perturbations of the original organization which may occur during quenching and fracturing of the samples and during the replication of fractured surfaces. Although it is well known that the preservation of the molecular organization of biological materials is critically dependent on the rate of freezing of the samples, little information is presently available concerning the nature and the extent of freezing-rate dependent perturbations of the original organizations. In order to obtain this information, we have developed a method based on the comparison of x-ray diffraction patterns of samples before and after freezing, prior to fracturing and replication.Our experimental set-up is shown in Fig. 1. The sample to be quenched is placed on its holder which is then mounted on a small metal holder (O) fixed on a glass capillary (p), whose position is controlled by a micromanipulator.

The Precipitation of Si in AlCuSi Thin Films

1973 ◽  
Vol 31 ◽  
pp. 34-35 ◽  
Author(s):  
R. M. Anderson
Keyword(s):  
Electron Microscopy ◽  
Thin Films ◽  
Heat Treatment ◽  
Solid Solution ◽  
Integrated Circuit ◽  
Copper Film ◽  
Solution Concentration ◽  
X Ray ◽  
Silicon Thin Films ◽  
Before And After

Aluminum-copper-silicon thin films have been considered as an interconnection metallurgy for integrated circuit applications. Various schemes have been proposed to incorporate small percent-ages of silicon into films that typically contain two to five percent copper. We undertook a study of the total effect of silicon on the aluminum copper film as revealed by transmission electron microscopy, scanning electron microscopy, x-ray diffraction and ion microprobe techniques as a function of the various deposition methods.X-ray investigations noted a change in solid solution concentration as a function of Si content before and after heat-treatment. The amount of solid solution in the Al increased with heat-treatment for films with ≥2% silicon and decreased for films <2% silicon.

Microanalysis of precipitates in a ferritic steel

1978 ◽  
Vol 36 (1) ◽  
pp. 618-619
Author(s):  
J.M. Titchmarsh
Keyword(s):  
Ferritic Steel ◽  
Particle Identification ◽  
Energy Dispersive ◽  
Objective Lens ◽  
Ferritic Steels ◽  
Replica Technique ◽  
X Ray ◽  
Large Numbers ◽  
Scanning Transmission ◽  
Made In

The advances in recent years in the microanalytical capabilities of conventional TEM's fitted with probe forming lenses allow much more detailed investigations to be made of the microstructures of complex alloys, such as ferritic steels, than have been possible previously. In particular, the identification of individual precipitate particles with dimensions of a few tens of nanometers in alloys containing high densities of several chemically and crystallographically different precipitate types is feasible. The aim of the investigation described in this paper was to establish a method which allowed individual particle identification to be made in a few seconds so that large numbers of particles could be examined in a few hours.A Philips EM400 microscope, fitted with the scanning transmission (STEM) objective lens pole-pieces and an EDAX energy dispersive X-ray analyser, was used at 120 kV with a thermal W hairpin filament. The precipitates examined were extracted using a standard C replica technique from specimens of a 2¼Cr-lMo ferritic steel in a quenched and tempered condition.

High-resolution x-ray imaging of small copper-rich precipitates in steels

1988 ◽  
Vol 46 ◽  
pp. 528-529
Author(s):  
J. R. Michael ◽  
K. A. Taylor
Keyword(s):  
Electron Microscopy ◽  
Thermomechanical Processing ◽  
Atom Probe ◽  
Ferrite Matrix ◽  
Scanning Transmission Electron Microscope ◽  
Probe Field ◽  
X Ray ◽  
Subsequent Transformation ◽  
Transmission Electron ◽  
Scanning Transmission

Although copper is considered an incidental or trace element in many commercial steels, some grades contain up to 1-2 wt.% Cu for precipitation strengthening. Previous electron microscopy and atom-probe/field-ion microscopy (AP/FIM) studies indicate that the precipitation of copper from ferrite proceeds with the formation of Cu-rich bcc zones and the subsequent transformation of these zones to fcc copper particles. However, the similarity between the atomic scattering amplitudes for iron and copper and the small misfit between between Cu-rich particles and the ferrite matrix preclude the detection of small (<5 nm) Cu-rich particles by conventional transmission electron microscopy; such particles have been imaged directly only by FIM. Here results are presented whereby the Cu Kα x-ray signal was used in a dedicated scanning transmission electron microscope (STEM) to image small Cu-rich particles in a steel. The capability to detect these small particles is expected to be helpful in understanding the behavior of copper in steels during thermomechanical processing and heat treatment.

Energy Dispersive X-Ray Measurements of thin Metal Foils

1976 ◽  
Vol 34 ◽  
pp. 426-427
Author(s):  
J. Bentley ◽  
E. A. Kenik
Keyword(s):  
Materials Science ◽  
Energy Dispersive Spectrometer ◽  
Thin Foil ◽  
Thin Metal ◽  
Energy Dispersive ◽  
Thin Specimen ◽  
X Ray ◽  
Metal Foils ◽  
Small Probe ◽  
Scanning Transmission

Instruments combining a 100 kV transmission electron microscope (TEM) with scanning transmission (STEM), secondary electron (SEM) and x-ray energy dispersive spectrometer (EDS) attachments to give analytical capabilities are becoming increasingly available and useful. Some typical applications in the field of materials science which make use of the small probe size and thin specimen geometry are the chemical analysis of small precipitates contained within a thin foil and the measurement of chemical concentration profiles near microstructural features such as grain boundaries, point defect clusters, dislocations, or precipitates. Quantitative x-ray analysis of bulk samples using EDS on a conventional SEM is reasonably well established, but much less work has been performed on thin metal foils using the higher accelerating voltages available in TEM based instruments.

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