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Advances in the Applications of Mössbauer Spectroscopy for Studies of...
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Advances in the Applications of Mössbauer Spectroscopy for Studies of Iron-Bearing Minerals

A special issue of Minerals (ISSN 2075-163X). This special issue belongs to the section "Crystallography and Physical Chemistry of Minerals & Nanominerals".

Deadline for manuscript submissions: closed (31 August 2023) | Viewed by 5089

Special Issue Editor

Dr. Michael Oshtrakh

E-Mail Website
Guest Editor
Department of Experimental Physics, Institute of Physics and Technology, Ural Federal University, 620002 Ekaterinburg, Russia
Interests: Mössbauer spectroscopy; iron-containing biomolecules and pharmaceuticals; biomedical applications; iron-bearing minerals in meteorites; iron-containing nanoparticles and nanostructured materials
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Various minerals contain iron cations which can occupy one or more crystallographic sites in these crystals. The iron chemical and physical states are some of the important characteristics of iron-bearing minerals which can influence the mineral structure and physical features. Metals, including iron, occupations of different crystallographic sites, and their redistributions with temperature are also very important in order to analyze the thermal history of minerals. Various extreme factors affecting terrestrial and extraterrestrial iron-bearing minerals, namely, high pressure, heating and reheating, cooling rate, impacts, etc., lead to some variations in the iron local microenvironments. 57Fe Mössbauer spectroscopy is one of the most sensitive physical techniques for the study of various iron-containing materials, including minerals. This technique permits analyzing the 57Fe hyperfine parameters (isomer shift, quadrupole splitting/quadrupole shift, magnetic hyperfine field), the iron valence/spin states, dynamics of 57Fe, relative iron contents in different sites, including iron partitioning variations, and in the minerals’ mixture, the 57Fe local microenvironments and their transformations, etc. More than 60 years of experience demonstrate high potential and advances in the applications of Mössbauer spectroscopy in the studies of various minerals. This Special Issue aims to present reviews and original research papers in the field of Mössbauer spectroscopy of various iron-bearing terrestrial and extraterrestrial minerals to demonstrate advances in this technique.

Dr. Michael Oshtrakh
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Minerals is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2400 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • Mössbauer spectroscopy
  • iron-bearing terrestrial and extraterrestrial minerals
  • 57Fe hyperfine interactions
  • iron-bearing phase composition
  • iron oxidation states
  • Fe2+ occupations and partitioning variations in non-equivalent sites
  • effect of extreme factors on the iron state in minerals

Published Papers (5 papers)

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Research

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24 pages, 6178 KiB  
Article
Iron-Bearing Minerals in the Boda Claystone Formation: Correspondences with Stages of Evolution Revealed by Mössbauer Spectroscopy
by Károly Lázár, Zoltán Máthé, Tibor Németh, Viktória Kovács-Kis, Sándor Stichleutner and Ivett Kovács
Minerals 2024, 14(2), 196; https://doi.org/10.3390/min14020196 - 14 Feb 2024
Viewed by 672
Abstract
The Boda Claystone Formation (BCF) is an extended sedimentary sequence formed in a shallow-water salt lake under semi-arid to arid climatic conditions during the middle Permian period. The rock was formed predominantly from denuded and altered products of three primary felsic sources, the [...] Read more.
The Boda Claystone Formation (BCF) is an extended sedimentary sequence formed in a shallow-water salt lake under semi-arid to arid climatic conditions during the middle Permian period. The rock was formed predominantly from denuded and altered products of three primary felsic sources, the Mórágy Metagranite Complex, the Baksa Metamorphic Complex and the rhyolitic Gyűrűfű Formation, resulting in the recent dominant sheet silicate components, illite and chlorite. BCF has been considered a potential host rock for high-level nuclear waste, too. Thus, it has been characterized by several powerful methods so far (X-ray diffraction (XRD), transmission electron microscopy (TEM), etc.). 57Fe Mössbauer spectroscopy may provide a unique additional tool to study iron-bearing minerals. Iron is dominantly present in a ferrous form in minerals of the fresh parent rocks (in the biotite group and amphibole), and in a ferric oxide, hematite, in altered Gyűrűfű Formation. During transformations of biotite group minerals and amphibole, the partial release of ferrous iron or its conversion to ferric form takes place with the stabilization of recent illite and chlorite, while the original layered structure is still preserved. Mössbauer spectroscopy revealed the dominant presence of ferrous iron located in cis-M2 octahedral sites both in parent biotite group minerals and in the final illite, as well as chlorite in both stages. The proportion of ferrous iron in biotite group minerals was halved during the stages of evolution by conversion to ferric iron still in sheet silicate illite or by segregation into separate hematite inclusions. The transformation process of biotite group minerals and amphibole of the source rocks is connected only to the iron-bearing smaller fraction of sheet silicates in the BCF clay mineral assemblage. Determination of Fe2+/Fe3+ ratios in sheet silicates was also pertinent in two sections of BCF. Namely, in samples from the Gorica region, Fe3+ was dominant, siting in illite, whereas Fe2+ was also present in significant portions in chlorite in samples from the Western Mecsek Anticline. The interpretation is deduced in correspondence with results of extended XRD, and high-resolution TEM studies. Full article
(This article belongs to the Special Issue Advances in the Applications of Mössbauer Spectroscopy for Studies of Iron-Bearing Minerals)
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17 pages, 7279 KiB  
Article
An Intensity Tensor and Electric Field Gradient Tensor for Fe3+ at M1 Sites of Aegirine–Augite Using Single-Crystal Mössbauer Spectroscopy
by Keiji Shinoda and Yasuhiro Kobayashi
Minerals 2023, 13(11), 1452; https://doi.org/10.3390/min13111452 - 18 Nov 2023
Cited by 1 | Viewed by 670
Abstract
An intensity tensor of quadrupole doublets and an electric field gradient tensor for Fe3+ at M1 sites in aegirine–augite ((Ca0.16Na0.86)∑1.02(Mg0.13Fe2+0.04Fe3+0.72 Al0.07)∑0.96Si2.01O6 [...] Read more.
An intensity tensor of quadrupole doublets and an electric field gradient tensor for Fe3+ at M1 sites in aegirine–augite ((Ca0.16Na0.86)∑1.02(Mg0.13Fe2+0.04Fe3+0.72 Al0.07)∑0.96Si2.01O6) are determined using single-crystal Mössbauer spectroscopy. The components of the intensity tensor are IXX = 0.670 (19), IYY = 0.353 (14), IXY = −0.113 (37) and IZZ = 0.477 (33). The components of the electric field gradient tensor (VXX, VYY and VZZ) for Fe3+ at M1 sites in aegirine–augite are −5.96 × 109, −4.65 × 1010 and 5.23 × 1010 C/m3, respectively. Comparisons of the intensity tensor of aegirine–augite with those of aegirine and augite (Wo40En45Fs16) that have already been reported and the IXX, IYY, IXY and IZZ intensity tensor components of aegirine–augite in this study are almost the same as those of aegirine, but different from those of augite. While the M2 sites of aegirine–augite and aegirine are fully occupied with Na+ and Ca2+ ions, the M2 sites of augite are not fully occupied with Ca2+. The compositional dependency of the intensity tensor components suggests that the intensity tensor components for Fe3+ at the M1 site of a solid solution between aegirine and augite are dependent on the occupancy of large cations such as Ca2+ and Na+ at M2 sites. Full article
(This article belongs to the Special Issue Advances in the Applications of Mössbauer Spectroscopy for Studies of Iron-Bearing Minerals)
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13 pages, 4149 KiB  
Article
57Fe Mössbauer Spectroscopy and X-ray Diffraction of Annealed Highly Metamict Perrierite: Activation Energy and Recrystallization Processes
by Dariusz Malczewski, Agnieszka Grabias, Maria Dziurowicz and Tomasz Krzykawski
Minerals 2023, 13(11), 1395; https://doi.org/10.3390/min13111395 - 30 Oct 2023
Viewed by 691
Abstract
This paper presents the results of 57Fe Mössbauer spectroscopy and X-ray diffraction analysis of highly metamict perrierite (REE,Ca,Th)4(Fe2+,Mg)2(Ti,Fe3+)3Si4O22 after annealing in argon from 673 to 1273 K for one [...] Read more.
This paper presents the results of 57Fe Mössbauer spectroscopy and X-ray diffraction analysis of highly metamict perrierite (REE,Ca,Th)4(Fe2+,Mg)2(Ti,Fe3+)3Si4O22 after annealing in argon from 673 to 1273 K for one hour. Radioactive elements in metamict minerals damage crystal structure on geologic time scales primarily due to recoil nuclei from α-decay of 238U, 232Th, 235U, and their daughter products. Metamict minerals are widely used in geochronology and can serve as natural analogs for the study of radiation effects in high-level nuclear waste. Analyses were performed on fragments of a perrierite sample collected from granitoids near Amherst, Virginia (USA). Electron microprobe and gamma-ray spectrometry recorded Fe concentrations of 4.7 wt.% and Th and U concentrations of 0.64 and 0.06 wt.%, respectively. The calculated total absorbed α-dose was 7.8 × 1015 α-decay mg−1. The Mössbauer spectrum of the untreated sample can be fitted to two Fe2+ and two Fe3+ doublets in octahedral coordination with a relative ΣFe2+/ΣFe of 0.63. For samples annealed at 1173 K and 1273 K, spectra show a decrease in the total contribution of Fe2+ to 0.58 due to dehydroxylation associated with the simultaneous oxidation of post-metamict Fe2+ to Fe3+. In the examined perrierite, Fe2+ occurs in structural positions B and C(1). The broad, predominant Fe3+ doublet observed in the spectrum of the unannealed sample splits into two components at 973 K interpreted to represented positions C(1) and C(2) in the perrierite structure. The Mössbauer spectra show a prominent decrease in the width of the high-energy absorption peak representing Fe2+ components with increasing temperature. The variation in the width of this peak versus the annealing temperature seems to be an indicator of thermally induced recrystallization. Based on the exponential dependence of the derivative function of the parameter with the inverse temperature and using an Arrhenius plot, an activation energy (EA) of 0.73 eV was determined for thermally-induced recrystallization. Corresponding XRD data show progressive recrystallization with increasing annealing temperature. The XRD pattern of the fragment annealed at 1273 K indicates that highly metamict perrierite recrystallized to the pre-metamict state that can be indexed to the C2/m space group. Full article
(This article belongs to the Special Issue Advances in the Applications of Mössbauer Spectroscopy for Studies of Iron-Bearing Minerals)
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20 pages, 8589 KiB  
Article
Thermal Decomposition of Siderite and Characterization of the Decomposition Products under O2 and CO2 Atmospheres
by Mariola Kądziołka-Gaweł, Jacek Nowak, Magdalena Szubka, Joanna Klimontko and Marcin Wojtyniak
Minerals 2023, 13(8), 1066; https://doi.org/10.3390/min13081066 - 11 Aug 2023
Cited by 2 | Viewed by 1739
Abstract
Siderite (FeCO3) is an iron-bearing carbonate mineral that is the most abundant sedimentary iron formation on Earth. Mineralogical alteration of four siderite samples annealed at temperatures 200 °C, 300 °C, 400 °C, 500 °C, 750 °C, and 1000 °C in an [...] Read more.
Siderite (FeCO3) is an iron-bearing carbonate mineral that is the most abundant sedimentary iron formation on Earth. Mineralogical alteration of four siderite samples annealed at temperatures 200 °C, 300 °C, 400 °C, 500 °C, 750 °C, and 1000 °C in an O2 and a CO2 atmosphere were investigated using such tools as X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), the X-ray fluorescence (XRF) method, differential scanning calorimetry and thermogravimetric analysis (DSC/TGA), and Mössbauer spectroscopy measurements. The decomposition of three siderite samples with similar iron content in the oxygen atmosphere took place in the temperature range of 340–607 °C. This process begins at approximately ~100 °C higher under a reducing atmosphere, but it is completed just above 600 °C, which is a temperature comparable to decomposition in an oxidizing atmosphere. These processes are shifted toward higher temperatures for the fourth sample with the lowest iron but the highest magnesium content. Magnetite, hematite, and maghemite are products of siderite decomposition after annealing in the oxygen atmosphere in the temperature range 300–500 °C, whereas hematite is the main component of the sample detected after annealing at 750 °C and 1000 °C. Magnetite is the main product of siderite decomposition under the CO2 atmosphere. However, hematite, maghemite, wüstite, and olivine were also present in the samples after annealing above 500 °C in this atmosphere. Full article
(This article belongs to the Special Issue Advances in the Applications of Mössbauer Spectroscopy for Studies of Iron-Bearing Minerals)
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Review

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46 pages, 25299 KiB  
Review
Advances in Analysis of the Fe-Ni-Co Alloy and Iron-Bearing Minerals in Meteorites by Mössbauer Spectroscopy with a High Velocity Resolution
by Michael V. Goryunov, Alevtina A. Maksimova and Michael I. Oshtrakh
Minerals 2023, 13(9), 1126; https://doi.org/10.3390/min13091126 - 25 Aug 2023
Cited by 2 | Viewed by 866
Abstract
Meteorites are the space messengers bringing us the unique information about the Solar System formation and evolution as well as about the effects of various extreme space conditions on meteorites and their parent bodies. The main iron-bearing compounds in meteorites are Fe-Ni-Co alloy, [...] Read more.
Meteorites are the space messengers bringing us the unique information about the Solar System formation and evolution as well as about the effects of various extreme space conditions on meteorites and their parent bodies. The main iron-bearing compounds in meteorites are Fe-Ni-Co alloy, olivine (Fe, Mg)2SiO4, orthopyroxene (Fe, Mg)SiO3, clinopyroxene (Ca, Fe, Mg)SiO3, troilite FeS, chromite FeCr2O4, hercynite FeAl2O4, ilmenite FeTiO3, daubréelite FeCr2S4, schreibersite (Fe, Ni)3P and some other compounds. Therefore, 57Fe Mössbauer spectroscopy was successfully applied for the analyses of various meteorites for about 60 years of experience. The development of Mössbauer spectrometers with a high velocity resolution, i.e., with a high discretization of the velocity reference signal up to 212, provides much better adjustment to resonance and significantly increases the spectra quality and analytical possibilities of Mössbauer spectroscopy. In fact, this permits us to decompose the complex Mössbauer spectra of meteorites using the larger number of spectral components related to reliable compounds in comparison with the results obtained using conventional Mössbauer spectrometers with discretization of the velocity reference signal up to 29. In the present review we consider the results and advances of various meteorites analyses by means of Mössbauer spectroscopy with a high velocity resolution. Full article
(This article belongs to the Special Issue Advances in the Applications of Mössbauer Spectroscopy for Studies of Iron-Bearing Minerals)
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