scholarly journals Cristallochemical characterization of synthetic Zn-substituted maghemites (g-Fe2-xZn xO3)

2008 ◽  
Vol 32 (2) ◽  
pp. 561-568 ◽  
Author(s):  
Marcelo Augusto Batista ◽  
Antonio Carlos Saraiva da Costa ◽  
Ivan Granemann de Souza Junior ◽  
Jerry Marshal Bigham

Maghemite (g-Fe2O3) is the most usually found ferrimagnetic oxide in red basalt-derived soils. The variable degrees of ionic substitution of Fe3+ for different metals (e.g. Ti4+, Al3+, Mg2+, Zn2+, and Mn2+) and non-metals in the maghemite structure influence some cristallochemical features of this iron oxide. In this study, synthetic Zn-substituted maghemites were prepared by co-precipitation in alkaline aqueous media of FeSO4.7H2O with increasing amounts of ZnSO4.7H2O to obtain the following sequence of Fe3+ for Zn2+ substitutions: 0.0, 0.025, 0.05, 0.10, 0.15, 0.20, and 0.30 mol mol-1. The objective of this work was to evaluate the cristallochemical alterations of synthetic Zn-substituted maghemites. The dark black synthetic precipitated material was heated to 250 °C during 4 h forming a brownish maghemite that was characterized by chemical analysis as well as X ray diffraction (XRD), specific surface area and mass-specific magnetic susceptibility. The isomorphic substitution levels observed were of 0.0013, 0.0297, 0.0590, 0.1145, 0.1764, 0.2292 and 0.3404 mol mol-1, with the formation of a series of maghemites from Fe2Zn0O3 to Fe(1.49)Zn(0.770)O3 . The increase in Fe3+ for Zn2+ substitution, [Zn mol mol-1] increased the dimension a0 of the cubic unit cells of the studied maghemites according to the regression equation: a0 = 0.8343 + 0.02591Zn (R² = 0.98). On the other hand, the mean crystallite dimension and mass-specific magnetic susceptibility of the studied maghemites decreased with increasing isomorphic substitution.

2016 ◽  
Vol 98 ◽  
pp. 70-74
Author(s):  
Andrius Laurikėnas ◽  
Jurgis Barkauskas ◽  
Aivaras Kareiva

In this study, lanthanide elements (Ln3+) and 2,3,5,6-tetrafluoro-1,4-benzenedicarboxylic acid (TFBDC) based metal-organic frameworks (MOFs) were synthesized by precipitation and diffusion-controlled precipitation methods. Powders insoluble in aqueous media and polar solvents were obtained. The microstructure and properties of Ln3+ MOFs were evaluated and discussed. X-ray diffraction (XRD) analysis, infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) and fluorescence spectroscopy (FLS) were carried out to characterize Ln3+ MOF's crystallinity, the microstructure, chemical composition and optical properties.


MRS Advances ◽  
2017 ◽  
Vol 2 (64) ◽  
pp. 4025-4030 ◽  
Author(s):  
T. Kryshtab ◽  
H. A. Calderon ◽  
A. Kryvko

ABSTRACTThe microstructure of Ni-Mg-Al mixed oxides obtained by thermal decomposition of hydrotalcite-like compounds synthesized by a co-precipitation method has been studied by using X-ray diffraction (XRD) and atomic resolution transmission electron microscopy (TEM). XRD patterns revealed the formation of NixMg1-xO (x=0÷1), α-Al2O3 and traces of MgAl2O4 and NiAl2O4 phases. The peaks profile analysis indicated a small grain size, microdeformations and partial overlapping of peaks due to phases with different, but similar interplanar spacings. The microdeformations point out the presence of dislocations and the peaks shift associated with the presence of excess vacancies. The use of atomic resolution TEM made it possible to identify the phases, directly observe dislocations and demonstrate the vacancies excess. Atomic resolution TEM is achieved by applying an Exit Wave Reconstruction procedure with 40 low dose images taken at different defocus. The current results suggest that vacancies of metals are predominant in MgO (NiO) crystals and that vacancies of Oxygen are predominant in Al2O3 crystals.


DYNA ◽  
2019 ◽  
Vol 86 (211) ◽  
pp. 278-287
Author(s):  
Javier Alberto Olarte Torres ◽  
María Cristina Cifuentes Arcila ◽  
Harvey Andrés Suárez Moreno

This paper presents the results obtained from the synthesis and morphological characterization of different magnetite samples:  La0.67-x Prx Ca0.33 MnO3.LaMn1-x Cox O3 and LaMn1-x Nix O3 at 0.13 ≤ 𝑥𝑥 ≤ 0.67 produced by a solid-state reaction mechanism and 𝐿𝐿𝐿𝐿𝑀𝑀𝑀𝑀1−𝑥𝑥(𝐶𝐶𝐶𝐶/𝑁𝑁𝑁𝑁)𝑥𝑥𝑂𝑂3 at 0.0 ≤ 𝑥𝑥 ≤ 0.5 produced by the sol-gel method. These samples were characterized using X-ray diffraction spectroscopy and by measuring electric resistivity and magnetic susceptibility which were carried out as a function of temperature. Notably, the effects of strain and compressive strength on the lattices of magnetite samples were highly dependent on the concentration of 𝑃𝑃𝑟𝑟, 𝐶𝐶𝐶𝐶, and 𝑁𝑁𝑁𝑁. Moreover, the transition temperatures of metal-insulator and ferromagnetic-paramagnetic phases also largely depend on these strength effects, e.g., at higher concentrations of 𝑃𝑃𝑟𝑟, effects of increased strain strength were observed, relocating the shifts of ferromagnetic-paramagnetic transitions to lower temperatures. On the other hand, effects of increased compressive strength were observed at higher concentrations of 𝑁𝑁𝑁𝑁 and 𝐶𝐶𝐶𝐶, relocating the shifts of ferromagnetic-paramagnetic and metal-insulator transitions to higher temperatures.


2010 ◽  
Vol 24 (01n02) ◽  
pp. 128-135 ◽  
Author(s):  
YING LI ◽  
CHI MUN CHEAH ◽  
HENGKY CHANG ◽  
LEONARD LOH ◽  
ADELINE KUM

A variety of bioactive composites have been invested over the last two decades as substitute materials for diseased or damaged tissues in the human body. In this paper, bioactive composites were prepared using polycaprolactone ( PCL ) and hydroxyapatite ( HA ). The influence of micro-sized and nano-sized HA on composite properties was investigated. The nano- HA was prepared by wet chemical co-precipitation reaction method. Studies of biocomposite specimen morphology were performed by Field-emission scanning electron microscopy (SEM). XRD (X-Ray Diffraction) and DSC (Differential scanning calorimetry) were used to assess the crystal structure of HA and thermal properties of the composites, respectively. The synthesized nano- HA is found to be of high purity HA structure. The relationship between composition, structure and properties was studied. Different methods to prepare uniform composites were tried, and the outcome of this work suggests that by proper manipulation of biodegradable polymers and bioactive ceramics through material design, bioactive composites with controlled properties might be achievable.


2014 ◽  
Vol 70 (6) ◽  
pp. 1004-1010 ◽  
Author(s):  
Th. I. Shalaby ◽  
N. M. Fikrt ◽  
M. M. Mohamed ◽  
M. F. El Kady

This study investigated the applicability of magnetite Fe3O4 nanoparticles coated with chitosan (CMNs) for the removal of some toxic heavy metals from simulated wastewater. Magnetic nanomaterials were synthesized using the co-precipitation method and characterized by transmission electron microscope, scanning electron microscope, X-ray diffraction, and Fourier transformer infrared spectroscopy. The magnetic properties of the prepared magnetic nanoparticles were determined by a vibrating-sample magnetometer. Batch experiments were carried out to determine the adsorption kinetics of Cr(VI) and Cd(II) by magnetic nanoparticles. It is noteworthy that CMNs show a highly efficient adsorption capacity for low concentration Cr(VI) and Cd(II) ions solution, which can reach 98% within 10 min.


2012 ◽  
Vol 581-582 ◽  
pp. 525-528
Author(s):  
Jia Feng Zhang ◽  
Bao Zhang ◽  
Xue Yi Guo ◽  
He Zhang Chen ◽  
Jian Long Wang ◽  
...  

The LiFe0.98Mn0.02PO4/C was synthesized by spray-drying and low temperature reduction route using FePO4•2H2O as precursor, which was prepared by a simple co-precipitation method. The LiFe0.98Mn0.02PO4/C sample was characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and electrochemical measurements. The XRD analysis and SEM images show that sample has the good ordered structure and spherical particle. The charge-discharge tests demonstrate that the powder has the better electrochemical properties, with an initial discharge capacity of 162.1 mAh•g−1 and 155.8 mAh•g−1 at current density of 0.1 C and 1C, respectively. The capacity retention reaches 99.4% after 100 cycles at 1C.


Nukleonika ◽  
2017 ◽  
Vol 62 (2) ◽  
pp. 187-195 ◽  
Author(s):  
Tadeusz Szumiata ◽  
Marzena Rachwał ◽  
Tadeusz Magiera ◽  
Katarzyna Brzózka ◽  
Małgorzata Gzik-Szumiata ◽  
...  

Abstract Several samples of dusts from steel and coke plants (collected mostly with electro filters) were subjected to the investigation of content of mineral phases in their particles. Additionally, sample of bog iron ore and metallurgical slurry was studied. Next, the magnetic susceptibility of all the samples was determined, and investigations of iron-containing phases were performed using transmission Mössbauer spectrometry. The values of mass-specific magnetic susceptibility χ varied in a wide range: from 59 to above 7000 × 10−8 m-3·kg−1. The low values are determined for bog iron ore, metallurgical slurry, and coke dusts. The extremely high χ was obtained for metallurgical dusts. The Mössbauer spectra and X-ray diffraction patterns point to the presence of the following phases containing iron: hematite and oxidized magnetite (in coke and metallurgical dusts as well as metallurgical slurry), traces of magnetite fine grains fraction (in metallurgical dusts), amorphous glassy silicates with paramagnetic Fe3+ and Fe2+ ions, traces of pyrrhotite (in coke dusts), α-Fe and nonstoichiometric wüstite (in metallurgical slurry), as well as ferrihydrite nanoparticles (in bog iron ore). For individual samples of metallurgical dusts, the relative contributions of Fe2+/3+ ions in octahedral B sites and Fe2+ ions in tetrahedral A sites in magnetite spinel structure differs considerably.


2000 ◽  
Vol 55 (9) ◽  
pp. 882-886 ◽  
Author(s):  
Martin Jansen ◽  
Sascha Vensky

The silver(I,II,III) oxide clathrate Ag7O8HCO3 was synthesized by anodic oxidation of silver(I) in a suspension of Ag2CO3 in an aqueous AgF solution. The title compound was characterized by single crystal X-ray diffraction (cubic, Fm3̄m, a = 9.8085(3) Å, Z = 4), scanning electron microscopy, thermal analysis, IR spectroscopy, 1H-solid state-NMR and measurement of the magnetic susceptibility


Materials ◽  
2021 ◽  
Vol 14 (16) ◽  
pp. 4689
Author(s):  
Melissa E. Henderson ◽  
James Beare ◽  
Sudarshan Sharma ◽  
Markus Bleuel ◽  
Pat Clancy ◽  
...  

Topologically nontrivial spin textures host great promise for future spintronic applications. Skyrmions in particular are of burgeoning interest owing to their nanometric size, topological protection, and high mobility via ultra-low current densities. It has been previously reported through magnetic susceptibility, microscopy, and scattering techniques that Co8Zn8Mn4 forms an above room temperature triangular skyrmion lattice. Here, we report the synthesis procedure and characterization of a polycrystalline Co8Zn8Mn4 disordered bulk sample. We employ powder X-ray diffraction and backscatter Laue diffraction as characterization tools of the crystallinity of the samples, while magnetic susceptibility and Small Angle Neutron Scattering (SANS) measurements are performed to study the skyrmion phase. Magnetic susceptibility measurements show a dip anomaly in the magnetization curves, which persists over a range of approximately 305 K–315 K. SANS measurements reveal a rotationally disordered polydomain skyrmion lattice. Applying a symmetry-breaking magnetic field sequence, we were able to orient and order the previously jammed state to yield the prototypical hexagonal diffraction patterns with secondary diffraction rings. This emergence of the skyrmion order serves as a unique demonstration of the fundamental interplay of structural disorder and anisotropy in stabilizing the thermal equilibrium phase.


Author(s):  
Pelin Aktaş

BaTi5O11 has been widely researched due to its unique microwave properties. Conventionally it is challenging to obtain this compound as a single phase. The BaTi5O11 was synthesized via co-precipitation technique using an aqueous solution of titanium(IV)(triethanolaminato) isopropoxide, barium nitrate and ammonia as precursors which are stable in an aqueous media. The phase evolution, purity, and structure were identified by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive X-ray (EDX) spectroscopy analysis. The desired BaTi5O11 structure was obtained by calcination at 900?C. Furthermore, the structure is characterized by TGA, FT-IR and Raman studies. The study showed that the particles were between 80 and 120 nm in size and the average crystallite size was determined from the Scherrer formula as 68.1 nm at 900?C.


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