A simple method for quantification of nonstoichiometric magnetite nanoparticles using conventional X-ray diffraction technique

Bondarenko, Lyubov; Pankratov, D. А.; Dzeranov, Artur; Джардималиева, Г. И.; Streltsova, Alla N.; Zarrelli, Mauro; Kydralieva, Kamila

doi:10.1016/j.mencom.2022.09.025

Cited by 9 publications

(10 citation statements)

References 12 publications

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“…The remaining three sextets correspond to iron atoms in different crystallographic positions for nonstoichiometric magnetite of the composition Fe 3-δ O 4 ≡ (Fe 3+ ) A (Fe 2+ 1-3δ Fe 3+ 1+2δ # δ ) B O 4 [ 49 , 50 ]. By analyzing the areas and isomeric shifts of the subspectra related to iron atoms in different crystallographic sites of magnetite, it is possible to estimate the value of the magnetite nonstoichiometric parameter (δ) using Equation (16) [ 51 ]: δ = {Σ(δ 2 − 3δ i + 2δ 3 ) × S i + (δ 2 − δ 3 )ΣS j }/{Σ(3δ 2 − δ i − 2δ 3 ) × S i + 3(δ 2 −δ 3 )ΣS j }, where S i is the relative area of the subspectrum with isomeric shift δ i related to iron atoms at the B site, S j is the relative area of the remaining subspectra, and δ 2 and δ 3 are isomeric shifts of iron atoms (+2) and (+3), respectively, in an octahedral oxygen environment for a given temperature (here, δ 2 = 1.16 ± 0.06 and 1.33 ± 0.09 mm/s for 296 and 78 K, respectively, and δ 3 = 0.37 ± 0.04 and 0.49 ± 0.04 mm/s for 296 and 78 K, respectively [ 41 ]). The results obtained for different temperatures are in agreement with each other, enabling the description of the composition of the samples as Fe 2.75 O 4 and Fe 2.85 O 4 for BR residue and sands residue, respectively; the first sample is more oxidized.…”

Section: Resultsmentioning

confidence: 99%

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High-Iron Bauxite Residue (Red Mud) Valorization Using Hydrochemical Conversion of Goethite to Magnetite

et al. 2022

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Bauxite residue (BR), also known as red mud, is a byproduct of the alumina production using the Bayer process. This material is not used to make iron or other iron-containing products worldwide, owing to its high content of sodium oxide and other impurities. In this study, we investigated the hydrochemical conversion of goethite (FeOOH) to magnetite (Fe3O4) in high-iron BR from the Friguia alumina refinery (Guinea) by Fe2+ ions in highly concentrated alkaline media. The simultaneous extraction of Al and Na made it possible to obtain a product containing more than 96% Fe3O4. The results show that the magnetization of Al-goethite and Al-hematite accelerates the dissolution of the Al from the iron mineral solid matrix and from the desilication product (DSP). After ferrous sulfate (FeSO4·7H2O) was added directly at an FeO:Fe2O3 molar ratio of 1:1 at 120 °C for 150 min in solution with the 360 g L−1 Na2O concentration, the alumina extraction ratio reached 96.27% for the coarse bauxite residue size fraction (Sands) and 87.06% for fine BR obtained from red mud. The grade of iron (total iron in the form of iron elements) in the residue can be increased to 69.55% for sands and 58.31% for BR. The solid residues obtained after leaching were studied by XRD, XRF, TG-DTA, VSM, Mössbauer spectroscopy, and SEM to evaluate the conversion and leaching mechanisms, as well as the recovery ratio of Al from various minerals. The iron-rich residues can be used in the steel industry or as a pigment.

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Section: Resultsmentioning

confidence: 99%

“… δ—isomer shift; ε (Δ)—quadrupole shift (splitting); Γ exp —line width; H eff —hyperfine magnetic field; S—relative area of a subspectrum №; “δ in Fe 3-δ O 4 ”—magnetite nonstoichiometric parameter [ 51 ]. …”

Section: Resultsmentioning

confidence: 99%

High-Iron Bauxite Residue (Red Mud) Valorization Using Hydrochemical Conversion of Goethite to Magnetite

et al. 2022

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“…Indeed, the sizes of magnetic domains can be estimated in the range from 12.6 (for Fe 3 O 4 -HA) to 15.7 (for Fe 3 O 4 -APTES) nm as reported in Table 1. Moreover, by analyzing the areas of the subspectra related to iron atoms in different crystallographic sites of magnetite, the value of the non-stoichiometric parameter-δ for nano-magnetite-Fe 3−δ O 4 ≡ (Fe 3+ ) A (Fe 2+ 1−3δ Fe 3+ 1+2δ # δ ) B O 4 [15,83], can be estimated by using the following expression:…”

Section: Local Environment Of Fe Atom/ionsmentioning

confidence: 99%

Functionalized Magnetite Nanoparticles: Characterization, Bioeffects, and Role of Reactive Oxygen Species in Unicellular and Enzymatic Systems

Kicheeva

Sushko

Bondarenko

et al. 2023

IJMS

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The current study evaluates the role of reactive oxygen species (ROS) in bioeffects of magnetite nanoparticles (MNPs), such as bare (Fe3O4), humic acids (Fe3O4-HA), and 3-aminopropyltriethoxysilane (Fe3O4-APTES) modified MNPs. Mössbauer spectroscopy was used to identify the local surrounding for Fe atom/ions and the depth of modification for MNPs. It was found that the Fe3O4-HA MNPs contain the smallest, whereas the Fe3O4-APTES MNPs contain the largest amount of Fe2+ ions. Bioluminescent cellular and enzymatic assays were applied to monitor the toxicity and anti-(pro-)oxidant activity of MNPs. The contents of ROS were determined by a chemiluminescence luminol assay evaluating the correlations with toxicity/anti-(pro-)oxidant coefficients. Toxic effects of modified MNPs were found at higher concentrations (>10−2 g/L); they were related to ROS storage in bacterial suspensions. MNPs stimulated ROS production by the bacteria in a wide concentration range (10−15–1 g/L). Under the conditions of model oxidative stress and higher concentrations of MNPs (>10−4 g/L), the bacterial bioassay revealed prooxidant activity of all three MNP types, with corresponding decay of ROS content. Bioluminescence enzymatic assay did not show any sensitivity to MNPs, with negligible change in ROS content. The results clearly indicate that cell-membrane processes are responsible for the bioeffects and bacterial ROS generation, confirming the ferroptosis phenomenon based on iron-initiated cell-membrane lipid peroxidation.

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Section: Mössbauer Analysismentioning

confidence: 99%

“…The hyperfine parameters of the minor doublet observed only at room temperature correspond to Fe 3+ ions in an octahedral oxygen environment [41]. δ − Isomer shift; ε (Δ) -Quadrupole shift (splitting); Γexp -Line width; Heff -Hyperfine magnetic field; S -Relative area of a subspectrum №, "δ in Fe3-δO4" -magnetite nonstoichiometric parameter [51].…”

Section: Mössbauer Analysismentioning

confidence: 99%

High-Iron Bauxite Residue (Red Mud) Valorisation Using Hydrochemical Conversion of Goethite to Magnetite

Shoppert¹,

Valeev²,

Diallo³

et al. 2022

Preprint

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Bauxite residue (BR), also known as red mud, is a by-product of the production of alumina via the Bayer process. Because of the high sodium oxide and other impurities content, this material is not used to obtain iron or other iron-containing products. In this paper, the hydro-chemical conversion of goethite (FeOOH) to magnetite (Fe3O4) in high-iron BR from the Friguia alumina refinery (Guinea) by Fe2+ ions in highly concentrated alkaline media was studied. The simultaneous extraction of Al and Na made it possible to obtain a product containing more than 96% Fe3O4. The results show that the magnetization of Al-goethite and Al-hemetite accelerates the dissolution of the Al from the iron mineral solid matrix and from the desilication product (DSP). After ferrous sulfate (FeSO4·7H2O) was added directly at the FeO:Fe2O3 molar ratio of 1:1 at 120 °C for 150 min in the solution with the 360 g L-1 Na2O concentration, the alumina extraction ratio reached 96.27% for the coarse bauxite residue size fraction (Sands) and 87.06% for fine BR obtained from red mud. The grade of iron (total iron in the form of iron element) in the residue can be increased to 69.55% for Sands and 58.31% for BR. The solid residues obtained after leaching were studied by XRD, XRF, TG-DTA, VSM, Mössbauer spectroscopy and SEM to evaluate the conversion and leaching mechanisms and the recovery ratio of Al from different minerals. The iron-rich residues can be used in the steel industry or as a pigment.

show abstract

A simple method for quantification of nonstoichiometric magnetite nanoparticles using conventional X-ray diffraction technique

Cited by 9 publications

References 12 publications

High-Iron Bauxite Residue (Red Mud) Valorization Using Hydrochemical Conversion of Goethite to Magnetite

High-Iron Bauxite Residue (Red Mud) Valorization Using Hydrochemical Conversion of Goethite to Magnetite

Functionalized Magnetite Nanoparticles: Characterization, Bioeffects, and Role of Reactive Oxygen Species in Unicellular and Enzymatic Systems

High-Iron Bauxite Residue (Red Mud) Valorisation Using Hydrochemical Conversion of Goethite to Magnetite

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