Search results for: Mössbauer

Authors: Justice Zakhele Msomi

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Nanoparticles of CdFe2O4 with particle size of about 10 nm have been synthesized by high energy ball milling and co-precipitation processes. The synthesis route appears to have some effects on the properties. The compounds have been characterized by X-ray diffraction, Fourier Transform Infrared (FTIR), transmission electron microscopy (TEM), Mössbauer and magnetization measurements. The XRD pattern of CdFe2O4 provides information about single-phase formation of spinel structure with cubic symmetry. The FTIR measurements between 400 and 4000 cm-1 indicate intrinsic cation vibration of the spinel structure. The Mössbauer spectra were recorded at 4 K and 300 K. The hyperfine fields appear to be highly sensitive on particle size. The evolution of the properties as a function of particle size is also presented.

Keywords: ferrite, nanoparticles, magnetization, Mössbauer

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Authors: Mohammad Beyki, Justus Pawlak, Robert Patzke, Franz Renz

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In the context of planetary exploration, the MIMOS II (miniaturized Mössbauer spectrometer) serves as a proven and reliable measuring instrument. The transmission behaviour of the electronics in the Mössbauer spectroscopy is newly developed and optimized. For this purpose, the overall electronics is split into three parts. This elaboration deals exclusively with the first part of the signal chain for the evaluation of photons in experiments with gamma radiation. Parallel to the analysis of the electronics, a new method for the stability consideration of linear and non-linear systems is presented: The extended method of Lyapunov’s stability criteria. The design helps to weigh advantages and disadvantages against other simulated circuits in order to optimize the MIMOS II for the terestric and extraterestric measurment. Finally, after stability analysis, the controller design according to Ackermann is performed, achieving the best possible optimization of the output variable through a skillful pole assignment.

Keywords: Mössbauer spectroscopy, electronic signal amplifier, light processing technology, photocurrent, trans-impedance amplifier, extended Lyapunov method

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Authors: Hakan Gungunes, Ismail A. Auwal, Abdulhadi Baykal, Sagar E. Shirsath

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Barium hexaferrite, BaFe₁₂O₁₉, substituted by Bi³⁺ and La³⁺ (BaBiₓLaₓFe₁₂₋₂ₓO₁₉ where 0.0 ≤ x ≤ 0.5) were prepared by solid state synthesis route. The effect of substituted Bi³⁺ and La³⁺ ions on the structure, morphology, magnetic and cation distributions of barium hexaferrite were investigated by X-ray powder diffractometry (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FT-IR) and Mössbauer spectroscopy. XRD powder patterns were refined by the Rietveld analysis method which confirmed the formation of single phase magneto-plumbite structure and the substitution of La³⁺ and Bi³⁺ ions into the lattice of barium ferrite. These results show that both La³⁺ and Bi³⁺ ions completely enter into barium hexaferrite lattice without disturbing the hexagonal ferrite structure. The EDX spectra confirmed the presence of all the constituents in expected elemental percentage. From 57Fe Mössbauer spectroscopy data, the variation in line width, isomer shift, quadrupole splitting and hyperfine magnetic field values on Bi and La substitutions have been determined. Cation distribution in the presently investigated hexaferrite system was estimated using the relative area of Mössbauer spectroscopy.

Keywords: hexaferrite, mössbauer, cation distribution, solid state synthesis

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Authors: N. Boudinar, A. Djekoun, A. Otmani, B. Bouzabata, J. M. Greneche

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High-energy ball milling is a solid-state powder processing technique that allows synthesizing a variety of equilibrium and non-equilibrium alloy phases starting from elemental powders. The advantage of this process technology is that the powder can be produced in large quantities and the processing parameters can be easily controlled, thus it is a suitable method for commercial applications. It can also be used to produce amorphous and nanocrystalline materials in commercially relevant amounts and is also amenable to the production of a variety of alloy compositions. Mechanical alloying (high-energy ball milling) provides an inter-dispersion of elements through a repeated cold welding and fracture of free powder particles; the grain size decreases to nano metric scale and the element mix together. Progressively, the concentration gradients disappear and eventually the elements are mixed at the atomic scale. The end products depend on many parameters such as the milling conditions and the thermodynamic properties of the milled system. Here, the mechanical alloying technique has been used to prepare nano crystalline Fe_50 and Fe_64 wt.% Ni alloys from powder mixtures. Scanning electron microscopy (SEM) with energy-dispersive, X-ray analyses and Mössbauer spectroscopy were used to study the mixing at nanometric scale. The Mössbauer Spectroscopy confirmed the ferromagnetic ordering and was use to calculate the distribution of hyperfin field. The Mössbauer spectrum for both alloys shows the existence of a ferromagnetic phase attributed to γ-Fe-Ni solid solution.

Keywords: nanocrystalline, mechanical alloying, X-ray diffraction, Mössbauer spectroscopy, phase transformations

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Authors: Z. Ž. Lazarević, Č. Jovalekić, V. N. Ivanovski, N. Ž. Romčević

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Nickel-zinc ferrite, Ni0.5Zn0.5Fe2O4 was prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2, Zn(OH)2 and Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 5 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase Ni0.5Zn0.5Fe2O4 samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra alows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrite, X-ray diffraction, infrared spectroscopy, Raman spectroscopy, Mössbauer spectroscopy

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Authors: Z. Ž. Lazarević, D. L. Sekulić, V. N. Ivanovski, N. Ž. Romčević

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NiFe2O4 (nickel ferrite), ZnFe2O4 (zinc ferrite) and Ni0.5Zn0.5Fe2O4 (nickel-zinc ferrite) were prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2/Fe(OH)3, Zn(OH)2/Fe(OH)3 and Ni(OH)2/Zn(OH)2/Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 25 h, 18 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase ferrite samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrites, Raman spectroscopy, IR spectroscopy, Mössbauer measurements

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Authors: B. S. Boyanov, A. B. Peltekov, K. I. Ivanov

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The ferrites of Zn, Cd, Cu, and mixed ferrites with NiO, MnO, MgO, CoO, ZnO, BaO combine the properties of dielectrics, semiconductors, ferro-magnets, catalysts, etc. The ferrites are used in an impressive range of applications due to their remarkable properties. A specific disadvantage of ferrites is that they are undesirably obtained in a lot of processes connected with metal production. They are very stable and poorly soluble compounds. The obtained ZnFe2O4 in zinc production connecting about 15% of the total zinc remains practically insoluble in dilute solutions of sulfuric acid. This decreases the degree of recovery of zinc and necessitates to further process the zinc-containing cake. In this context, the ferrites; ZnFe2O4, CdFe2O4, and CuFe2O4 are synthesized in laboratory conditions using ceramic technology. Their homogeneity and structure are proven by X-Ray diffraction analysis and Mössbauer spectroscopy. The synthesized ferrites are subjected to strong acid and high temperature leaching with solutions of H2SO4, HCl, and HNO3 (7, 10 and 15 %). The results indicate that the highest degree of leaching of Zn, Cd, and Cu from the ferrites is achieved by use of HCl. The resulting values for the degree of leaching of metals using H2SO4 are lower, but still remain significantly higher for all of the experimental conditions compared to the values obtained using HNO3. Five zinc sulfide concentrates are characterized for iron content by chemical analysis, Web-based Information System, and iron phases by Mössbauer spectroscopy. The charging was optimized using the criterion of minimal amount of zinc ferrite produced when roasting the concentrates in a fluidized bed. The results obtained are interpreted in terms of the hydrometallurgical zinc production and maximum recovery of zinc, copper and cadmium from initial zinc sulfide concentrates after their roasting.

Keywords: hydrometallurgy, inorganic acids, solubility, zinc ferrite

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Authors: J. A. Sawicki, C. Ebrahimi

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The first geochemical, petrological, X-ray diffraction, Raman, Mössbauer, and oxygen isotopic analyses of very intriguing 13-kg Sooke #1 stone covered in 70% of its surface with black fusion crust, found in and recovered from Sooke Basin, near Juan de Fuca Strait, in British Columbia, were reported as poster #2775 at LPSC52 in March. Our further analyses reported in poster #6305 at 84AMMS in August and comparisons with the Mössbauer spectra of Martian meteorite MIL03346 and Martian rocks in Gusev Crater reported by Morris et al. suggest that Sooke #1 find could be a stony achondrite of Martian polymict breccia type ejected from early watery Mars. Here, the Raman spectra of a carbon-rich ~1-mm² fossil-like white area identified in this rock on a surface of polished cut have been examined in more detail. The low-intensity 532 nm and 633 nm beams of the InviaRenishaw microscope were used to avoid any destructive effects. The beam was focused through the microscope objective to a 2 m spot on a sample, and backscattered light collected through this objective was recorded with CCD detector. Raman spectra of dark areas outside fossil have shown bands of clinopyroxene at 320, 660, and 1020 cm-1 and small peaks of forsteritic olivine at 820-840 cm-1, in agreement with results of X-ray diffraction and Mössbauer analyses. Raman spectra of the white area showed the broad band D at ~1310 cm-1 consisting of main mode A1g at 1305 cm⁻¹, E2g mode at 1245 cm⁻¹, and E1g mode at 1355 cm⁻¹ due to stretching diamond-like sp3 bonds in diamond polytype lonsdaleite, as in Ovsyuk et al. study. The band near 1600 cm-1 mostly consists of D2 band at 1620 cm-1 and not of the narrower G band at 1583 cm⁻¹ due to E2g stretching in planar sp2 bonds that are fundamental building blocks of carbon allotropes graphite and graphene. In addition, the broad second-order Raman bands were observed with 532 nm beam at 2150, ~2340, ~2500, 2650, 2800, 2970, 3140, and ~3300 cm⁻¹ shifts. Second-order bands in diamond and other carbon structures are ascribed to the combinations of bands observed in the first-order region: here 2650 cm⁻¹ as 2D, 2970 cm⁻¹ as D+G, and 3140 cm⁻¹ as 2G ones. Nanodiamonds are abundant in the Universe, found in meteorites, interplanetary dust particles, comets, and carbon-rich stars. The diamonds in meteorites are presently intensely investigated using Raman spectroscopy. Such particles can be formed by CVD process and during major impact shocks at ~1000-2300 K and ~30-40 GPa. It cannot be excluded that the fossil discovered in Sooke #1 could be a remnant of an alien carbon organism that transformed under shock impact to nanodiamonds. We trust that for the benefit of research in astro-bio-geology of meteorites, asteroids, Martian rocks, and soil, this find deserves further, more thorough investigations. If possible, the Raman SHERLOCK spectrometer operating on the Perseverance Rover should also search for such objects in the Martian rocks.

Keywords: achondrite, nanodiamonds, lonsdaleite, raman spectra

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Authors: Mohamed Nasraoui

Abstract:

Spatial ore distribution, ore heterogeneity and their links with geological processes involved in Niobium concentration are all factors for consideration when bridging field observations to extraction scheme. Indeed, mineralogy changes of Nb-hosting phases, their textural relationships with hydrothermal or secondary minerals, play a key control over mineral processing. This study based both on filed work and ore characterization presents data from several Nb-deposits related to carbonatite complexes. The results obtained by a wide range of analytical techniques, including, XRD, XRF, ICP-MS, SEM, Microprobe, Spectro-CL, FTIR-DTA and Mössbauer spectroscopy, demonstrate how geometallurgical assessment, at all stage of mine development, can greatly assist in the design of a suitable extraction flowsheet and data reconciliation.

Keywords: carbonatites, Nb-geometallurgy, Nb-mineralogy, mineral processing.

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Authors: S. S. Pati, L. Herojit Singh, A. C. Oliveira, V. K. Garg

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Chitosan functionalized Fe3O4-Au core shell nanoparticles have been prepared using a two step wet chemical approach using NaBH4 as reducing agent for formation of Au inethylene glycol. X-ray diffraction studies shows individual phases of Fe3O4 and Au in the as prepared samples with crystallite size of 5.9 and 11.4 nm respectively. The functionalization of the core-shell nanostructure with Chitosan has been confirmed using Fourier transform infrared spectroscopy along with signatures of octahedral and tetrahedral sites of Fe3O4 below 600cm-1. Mössbauer spectroscopy shows decrease in particle-particle interaction in presence of Au shell (72% sextet) than pure oleic coated Fe3O4 nanoparticles (88% sextet) at room temperature. At 80K, oleic acid coated Fe3O4 shows only sextets whereas the Chitosan functionalized Fe3O4 and Chitosan functionalized Fe3O4@Au core shell show presence of 5 and 11% doublet, respectively.

Keywords: core shell, drug delivery, gold nanoparticles, magnetic nanoparticles

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