“…A 57 Fe Mössbauer spectrum of the as‐prepared Fe(0) nanoparticles (6 K data) shows a comparably weak intensity, which can be ascribed to the very small particle size (Figure e). The observed structure nevertheless can be clearly adapted to a sextet, which is in good agreement with 57 Fe Mössbauer spectra of small‐sized Fe(0) nanoparticles (<5 nm) reported in the literature . This also holds true for the observed isomer shift of 0 mm s −1 and the shape of the signal splitting.…”
Section: Magnetism and Mössbauer Spectroscopysupporting
The synthesis of zero‐valent iron (Fe(0)) nanoparticles in pyridine using lithium bipyridinyl ([LiBipy]) or lithium pyridinyl ([LiPy]) is presented. FeCl3 is used as the most simple starting material and reduced either in a [LiBipy]‐driven two‐step approach or in a [LiPy]‐driven one‐pot synthesis. High‐quality nanoparticles are obtained with uniform, spherical shape, and mean diameters of 2.9 ± 0.5 nm ([LiBipy]) or 4.1 ± 0.7 nm ([LiPy]). The as‐prepared, high purity Fe(0) nanoparticles are monocrystalline. In addition to particle characterization (high‐resolution transmission electron microscopy, scanning transmission electron microscopy, dynamic light scattering), composition and purity are examined in detail based on electron diffraction, X‐ray powder diffraction, elemental analysis, infrared spectroscopy, 57Fe Mössbauer spectroscopy, and magnetic measurements. Due to their small size and high purity, the Fe(0) nanoparticles are highly reactive. They can be used in follow‐up reactions to obtain a variety of iron compounds, which is exemplarily shown for the transformation to iron carbide (Fe3C) nanoparticles, the reaction with sulfur to obtain FeS nanoparticles, or the direct reaction with pentamethylcyclopentadiene to FeCp*2 (Cp*: pentamethylcyclopentadienyl).
“…A 57 Fe Mössbauer spectrum of the as‐prepared Fe(0) nanoparticles (6 K data) shows a comparably weak intensity, which can be ascribed to the very small particle size (Figure e). The observed structure nevertheless can be clearly adapted to a sextet, which is in good agreement with 57 Fe Mössbauer spectra of small‐sized Fe(0) nanoparticles (<5 nm) reported in the literature . This also holds true for the observed isomer shift of 0 mm s −1 and the shape of the signal splitting.…”
Section: Magnetism and Mössbauer Spectroscopysupporting
The synthesis of zero‐valent iron (Fe(0)) nanoparticles in pyridine using lithium bipyridinyl ([LiBipy]) or lithium pyridinyl ([LiPy]) is presented. FeCl3 is used as the most simple starting material and reduced either in a [LiBipy]‐driven two‐step approach or in a [LiPy]‐driven one‐pot synthesis. High‐quality nanoparticles are obtained with uniform, spherical shape, and mean diameters of 2.9 ± 0.5 nm ([LiBipy]) or 4.1 ± 0.7 nm ([LiPy]). The as‐prepared, high purity Fe(0) nanoparticles are monocrystalline. In addition to particle characterization (high‐resolution transmission electron microscopy, scanning transmission electron microscopy, dynamic light scattering), composition and purity are examined in detail based on electron diffraction, X‐ray powder diffraction, elemental analysis, infrared spectroscopy, 57Fe Mössbauer spectroscopy, and magnetic measurements. Due to their small size and high purity, the Fe(0) nanoparticles are highly reactive. They can be used in follow‐up reactions to obtain a variety of iron compounds, which is exemplarily shown for the transformation to iron carbide (Fe3C) nanoparticles, the reaction with sulfur to obtain FeS nanoparticles, or the direct reaction with pentamethylcyclopentadiene to FeCp*2 (Cp*: pentamethylcyclopentadienyl).
“…In relation to the developments of visible-light-activated photocatalysts and secondary battery electrodes of iron oxide NPs, we confirmed the methylene blue (MB) degradation effect of a mixture of Fe NPs and γ-Fe 2 O 3 NPs [12]. In this study, a 10-day MB aq degradation test using a 1:3 molar ratio of Fe NPs to γ-Fe 2 O 3 NPs mixed powder showed a significant decrease in MB concentration from 20.0 to 0.85 µM with a maximum k value of 2.84 day −1 , indicating that iron oxide NPs effectively degrade organic compounds [13]. This result proves that the nano size of Fe and γ-Fe 2 O 3 showed larger reactivity because of their high surface area.…”
The present study investigates the relationship between the local structure, photocatalytic ability, and cathode performances in sodium-ion batteries (SIBs) and lithium-ion batteries (LIBs) using Ni-substituted goethite nanoparticles (NixFe1-xOOH NPs) with a range of 'x' values from 0 to 0.5. The structural characterization was performed applying various techniques, including X-ray diffractometry (XRD), Thermogravimetry differential thermal analysis (TG-DTA), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray absorption spectroscopy (XANES/EXAFS), both measured at room temperature (RT), and 57Fe Mössbauer spectroscopy recorded at RT and at low temperatures (LT) from 20 K to 300 K, Brunauer-Emmett-Teller surface area measurement (BET), and diffuse reflectance spectroscopy (DRS). In addition, the electrical properties of NixFe1-xOOH NPs were evaluated by impedance spectroscopy. XRD showed the presence of goethite as the only crystalline phase in prepared samples with x ≤ 0.20, and goethite and α-Ni(OH)2 in the samples with x > 0.20. Sample with x = 0.10 (Ni10) showed the highest photo-Fenton ability with a first-order rate constant value (k) of 15.8×10-3 min-1. The 57Fe Mössbauer spectrum of Ni0, measured at RT, displayed a sextet corresponding to goethite, with an isomer shift (δ) of 0.36 mm s-1 and a hyperfine magnetic distribution (Bhf) of 32.95 T. Moreover, the DC conductivity decreased from 5.52×10-10 to 5.30×10-12 (Ω.cm)–1 with 'x' increasing from 0.10 to 0.50. Ni20 showed the highest initial discharge capacity of 223 mAh g-1, attributed to its largest specific surface area of 174.0 m2 g-1. In conclusion, NixFe1-xOOH NPs can be effectively utilized as visible-light-activated catalysts and active cathode materials in secondary batteries.
“…The initial nano-Fe 3 O 4 sample was prepared according to work [51]. Mohr's salt (2.627 g) was added to (NH 4 ) 3 Fe(C 2 O 4 ) 3 • 3H 2 O (5.693 g) and dissolved in 250 mL of deionized water.…”
The effect of swift heavy ion irradiation on sol–gel-prepared maghemite nanoparticles was studied by 57Fe transmission Mössbauer spectroscopy and X-ray diffractometry (XRD). The room temperature Mössbauer spectra of the non-irradiated nano-maghemite showed poorly resolved magnetically split, typical relaxation spectra due to the superparamagnetic state of the nanoparticles. Significant changes in the line shape, indicating changes in the superparamagnetic state, were found in the Mössbauer spectra upon irradiation by 160 MeV and 155 MeV 132Xe26+ ions with fluences of 5 × 1013 ion cm−2 and 1 × 1014 ion cm−2. XRD of the irradiated maghemite nanoparticles showed a significant broadening of the corresponding lines, indicating a decrease in the crystallite size, compared to those of the non-irradiated ones. The results are discussed in terms of the defects induced by irradiation and the corresponding changes related to the change in particle size and consequently in the superparamagnetic state caused by irradiation.
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