Search results for: spinel.

Authors: Ashish R. Tanna, Hiren H. Joshi

Abstract:

The mineral having chemical compositional formula MgAl2O4 is called “spinel". The ferrites crystallize in spinel structure are known as spinel-ferrites or ferro-spinels. The spinel structure has a fcc cage of oxygen ions and the metallic cations are distributed among tetrahedral (A) and octahedral (B) interstitial voids (sites). The X-ray diffraction (XRD) intensity of each Bragg plane is sensitive to the distribution of cations in the interstitial voids of the spinel lattice. This leads to the method of determination of distribution of cations in the spinel oxides through XRD intensity analysis. The computer program for XRD intensity analysis has been developed in C language and also tested for the real experimental situation by synthesizing the spinel ferrite materials Mg0.6Zn0.4AlxFe2- xO4 and characterized them by X-ray diffractometry. The compositions of Mg0.6Zn0.4AlxFe2-xO4(x = 0.0 to 0.6) ferrites have been prepared by ceramic method and powder X-ray diffraction patterns were recorded. Thus, the authenticity of the program is checked by comparing the theoretically calculated data using computer simulation with the experimental ones. Further, the deduced cation distributions were used to fit the magnetization data using Localized canting of spins approach to explain the “recovery" of collinear spin structure due to Al3+ - substitution in Mg-Zn ferrites which is the case if A-site magnetic dilution and non-collinear spin structure. Since the distribution of cations in the spinel ferrites plays a very important role with regard to their electrical and magnetic properties, it is essential to determine the cation distribution in spinel lattice.

Keywords: Spinel ferrites, Localized canting of spins, X-ray diffraction, Programming in Borland C.

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Authors: S. N. Hosseini, M. H. Enayati, F. Karimzadeh, N. M. Sammes

Abstract:

The synthesis of CuFe2O4 spinel powders by an optimized combustion-like process followed by calcination is described herein. The samples were characterized using X-ray diffraction (XRD), differential thermal analysis (TG/DTA), scanning electron microscopy (SEM), dilatometry and 4-probe DC methods. Different glycine to nitrate (G/N) ratios of 1 (fuel-deficient), 1.48 (stoichiometric) and 2 (fuel-rich) were employed. Calcining the asprepared powders at 800 and 1000°C for 5 hours showed that the G/N ratio of 2 results in the formation of the desired copper spinel single phase at both calcination temperatures. For G/N=1, formation of CuFe2O4 takes place in three steps. First, iron and copper nitrates decompose to iron oxide and pure copper. Then, copper transforms to copper oxide and finally, copper and iron oxides react with each other to form a copper ferrite spinel phase. The electrical conductivity and the coefficient of thermal expansion of the sintered pelletized samples were 2 S.cm-1 (800°C) and 11×10-6 °C-1 (25-800°C), respectively.

Keywords: SOFC interconnect coatings, Copper ferrite, Spinels, Electrical conductivity, Glycine–nitrate process.

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Authors: Jiri Plocek, Petr Holec, Simona Kubickova, Barbara Pacakova, Irena Matulkova, Alice Mantlikova, Ivan Nemec, Daniel Niznansky, Jana Vejpravova

Abstract:

This article presents summary on preparation and characterization of zinc, copper, cadmium and cobalt chromite nanocrystals, embedded in an amorphous silica matrix. The ZnCr2O4/SiO2, CuCr2O4/SiO2, CdCr2O4/SiO2 and CoCr2O4/SiO2 nanocomposites were prepared by a conventional sol-gel method under acid catalysis. Final heat treatment of the samples was carried out at temperatures in the range of 900−1200 ◦C to adjust the phase composition and the crystallite size, respectively. The resulting samples were characterized by Powder X-ray diffraction (PXRD), High Resolution Transmission Electron Microscopy (HRTEM), Raman/FTIR spectroscopy and magnetic measurements. Formation of the spinel phase was confirmed in all samples. The average size of the nanocrystals was determined from the PXRD data and by direct particle size observation on HRTEM; both results were correlated. The mean particle size (reviewed by HRTEM) was in the range from ∼4 to 46 nm. The results showed that the sol-gel method can be effectively used for preparation of the spinel chromite nanoparticles embedded in the silica matrix and the particle size is driven by the type of the cation A2+ in the spinel structure and the temperature of the final heat treatment. Magnetic properties of the nanocrystals were found to be just moderately modified in comparison to the bulk phases.

Keywords: Chromite, Fourier transform infrared spectroscopy, agnetic properties, nanocomposites, Raman spectroscopy, Rietveld refinement, sol-gel method, spinel.

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Authors: Javier Sánchez, Laura Elena De León Prado, Dora Alicia Cortés Hernández

Abstract:

Magnetic spinel ferrites are materials that possess size, magnetic properties and heating ability adequate for their potential use in biomedical applications. The Mn_0.5Ga_0.5Fe₂O₄ magnetic nanoparticles (MNPs) were synthesized by sol-gel method using citric acid as chelating agent of metallic precursors. The synthesized samples were identified by X-Ray Diffraction (XRD) as an inverse spinel structure with no secondary phases. Saturation magnetization (Ms) of crystalline powders was 45.9 emu/g, which was higher than those corresponding to GaFe₂O₄ (14.2 emu/g) and MnFe₂O₄ (40.2 emu/g) synthesized under similar conditions, while the coercivity field (Hc) was 27.9 Oe. The average particle size was 18 ± 7 nm. The heating ability of the MNPs was enough to increase the surrounding temperature up to 43.5 °C in 7 min when a quantity of 4.5 mg of MNPs per mL of liquid medium was tested. Cytotoxic effect (hemolysis assay) of MNPs was determined and the results showed hemolytic values below 1% in all tested cases. According to the results obtained, these synthesized nanoparticles can be potentially used as thermoseeds for hyperthermia therapy.

Keywords: Cytotoxicity, heating ability, manganese-gallium ferrite, magnetic hyperthermia.

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Authors: Amit Kumar Bhandary, Prithviraj Gupta, Siddhartha Mukherjee, Mahua Ghosh Chaudhuri, Rajib Dey

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Chromite ores are primarily used for extraction of chromium, which is an expensive metal. For low grade chromite ores (containing less than 40% Cr₂O₃), the chromium extraction is not usually economically viable. India possesses huge quantities of low grade chromite reserves. This deposit can be utilized after proper physical beneficiation. Magnetic separation techniques may be useful after reduction for the beneficiation of low grade chromite ore. The sample collected from the sukinda mines is characterized by XRD which shows predominant phases like maghemite, chromite, silica, magnesia and alumina. The raw ore is crushed and ground to below 75 micrometer size. The microstructure of the ore shows that the chromite grains surrounded by a silicate matrix and porosity observed the exposed side of the chromite ore. However, this ore may be utilized in refractory applications. Chromite ores contain Cr₂O₃, FeO, Al₂O₃ and other oxides like Fe-Cr, Mg-Cr have a high tendency to form spinel compounds, which usually show high refractoriness. Initially, the low grade chromite ore (containing 34.8% Cr₂O₃) was reduced at 1200 ⁰C for 80 minutes with 30% coke fines by weight, before being subjected to magnetic separation. The reduction by coke leads to conversion of higher state of iron oxides converted to lower state of iron oxides. The pre-reduced samples are then characterized by XRD. The magnetically inert mass was then reacted with 20% MgO by weight at 1450 ⁰C for 2 hours. The resultant product was then tested for various refractoriness parameters like apparent porosity, slag resistance etc. The results were satisfactory, indicating that the resultant spinel compounds are suitable for refractory applications for elevated temperature processes.

Keywords: Apparent porosity, beneficiation, low grade chromite, refractory, spinel compounds, slag resistance.

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Authors: Maryam Kiani, Abdul Basit Kiani

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To develop construction and infrastructure industry, sensors are highly desired to control building ventilation. Zinc doped magnesium ferrite nanoparticles (Z@MFO) (Zn = 0.0, 0.2, 0.3, 0.4) were prepared in this paper. Structural analyses confirmed the formation of spinel cubic nanostructures. X-Ray diffraction (XRD) data represent high reactive surface area due to small average particle size about 15 nm, which efficiently influences the gas sensing mechanism. The gas sensing property of Z@MFO for several gases was obtained by measuring the resistance as a function of different factors, such as composition and response time in air and in presence of gas. The sensitivity of spinel ferrite to CO2 at room temperature has been compared. The Z@MFO nano-structure exhibited high sensitivity represented good response time of (~1 min) to CO2, demonstrated that the material can be used in the field of gas sensors with high sensitivity and good selectivity at room temperature to control building ventilation. CO2 gas sensors play a vital role in ensuring the safety, comfort, and sustainability of modern building environments.

Keywords: MgFe2O4 nanoparticles, synthesis, gas sensing properties, X ray differentiation.

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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: V. S. Bushkova

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It is well known that in recent years magnetic materials have received increased attention due to their properties. For this reason a significant number of patents that were published during the last decade are oriented towards synthesis and study of such materials. The aim of this work is to create and study ferrite nanocrystalline materials with spinel structure, using sol-gel technology with participation of auto-combustion. This method is perspective in that it is a cheap and low-temperature technique that allows for the fine control on the product’s chemical composition.

Keywords: Magnetic materials, ferrites, sol–gel technology, nanocrystalline powders.

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Authors: M. Anis-ur- Rehman, A. Abdullah, Mariam Ansari , Zeb-un-Nisa, M. S. Awan

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Samples of CoFe2-xCrxO4 where x varies from 0.0 to 0.5 were prepared by co-precipitation route. These samples were sintered at 750°C for 2 hours. These particles were characterized by X-ray diffraction (XRD) at room temperature. The FCC spinel structure was confirmed by XRD patterns of the samples. The crystallite sizes of these particles were calculated from the most intense peak by Scherrer formula. The crystallite sizes lie in the range of 37-60 nm. The lattice parameter was found decreasing upon substitution of Cr. DC electrical resistivity was measured as a function of temperature. The room temperature thermoelectric power was measured for the prepared samples. The magnitude of Seebeck coefficient depends on the composition and resistivity of the samples.

Keywords: Ferrites, crystallite size, drift mobility, seebeck coefficient, thermopower.

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Authors: Krasimir Ivanov, Dimitar Dimitrov, Boyan Boyanov

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The paper relates to a catalyst, comprising copperchromium spinel, coated on carrier γ-Al2O3. The effect of preparation conditions on the active component composition and activity behavior of the catalysts is discussed. It was found that the activity of carbon monoxide, DME, formaldehyde and methanol oxidation reaches a maximum at an active component content of 20 – 30 wt. %. Temperature calcination at 500oC seems to be optimal for the γ– alumina supported CuO-Cr2O3 catalysts for CO, DME, formaldehyde and methanol oxidation. A three months industrial experiment was carried out to elucidate the changes in the catalyst composition during industrial exploitation of the catalyst and the main reasons for catalyst deactivation. It was concluded that the CuO–Cr2O3/γ–alumina supported catalysts have enhanced activity toward CO, DME, formaldehyde and methanol oxidation and that these catalysts are suitable for industrial application. The main reason for catalyst deactivation seems to be the deposition of iron and molybdenum, coming from the main reactor, on the active component surface.

Keywords: catalyst deactivation, CuO-Cr2O3 catalysts, deep oxidation.

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Authors: V. Sivakumar, R. Neelakantan

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Mineral mapping on the Moon surface provides the clue to understand the origin, evolution, stratigraphy and geological history of the Moon. Recently, reflectance imaging spectroscopy plays a significant role in identifying minerals on the planetary surface in the Visible to NIR region of the electromagnetic spectrum. The Moon Mineralogy Mapper (M³) onboard Chandrayaan-1 provides unprecedented spectral data of lunar surface to study about the Moon surface. Here we used the M³ sensor data (hyperspectral imaging spectroscopy) for analysing mineralogy of Orientale basin region on the Moon surface. Reflectance spectrums were sampled from different locations of the basin and continuum was removed using ENvironment for Visualizing Images (ENVI) software. Reflectance spectra of unknown mineral composition were compared with known Reflectance Experiment Laboratory (RELAB) spectra for discriminating mineralogy. Minerals like olivine, Low-Ca Pyroxene (LCP), High-Ca Pyroxene (HCP) and plagioclase were identified. In addition to these minerals, an unusual type of spectral signature was identified, which indicates the probable Fe-Mg-spinel lithology in the basin region.

Keywords: Chandrayaan-1, moon mineralogy mapper, orientale basin, moon, spectroscopy, hyperspectral.

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Authors: Krasimir I. Ivanov, Elitsa N. Kolentsova, Dimitar Y. Dimitrov, Georgi V. Avdeev, Tatyana T. Tabakova

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In recent research copper and manganese systems were found to be the most active in CO and organic compounds oxidation among the base catalysts. The mixed copper manganese oxide has been widely studied in oxidation reactions because of their higher activity at low temperatures in comparison with single oxide catalysts. The results showed that the formation of spinel CuxMn3−xO4 in the oxidized catalyst is responsible for the activity even at room temperature. That is why the most of the investigations are focused on the hopcalite catalyst (CuMn2O4) as the best coppermanganese catalyst. Now it’s known that this is true only for CO oxidation, but not for mixture of CO and VOCs. The purpose of this study is to investigate the alumina supported copper-manganese catalysts with different Cu/Mn molar ratio in terms of oxidation of CO, methanol and dimethyl ether. The catalysts were prepared by impregnation of γ-Al2O3 with copper and manganese nitrates and the catalytic activity measurements were carried out in two stage continuous flow equipment with an adiabatic reactor for simultaneous oxidation of all compounds under the conditions closest possible to the industrial. Gas mixtures on the input and output of the reactor were analyzed with a gas chromatograph, equipped with FID and TCD detectors. The texture characteristics were determined by low-temperature (- 196oС) nitrogen adsorption in a Quantachrome Instruments NOVA 1200e (USA) specific surface area & pore analyzer. Thermal, XRD and TPR analyses were performed. It was established that the active component of the mixed Cu- Mn/γ–alumina catalysts strongly depends on the Cu/Mn molar ratio. Highly active alumina supported Cu-Mn catalysts for CO, methanol and DME oxidation were synthesized. While the hopcalite is the best catalyst for CO oxidation, the best compromise for simultaneous oxidation of all components is the catalyst with Cu/Mn molar ratio 1:5.

Keywords: Supported copper-manganese catalysts, CO and VOCs oxidation.

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Authors: Laura Elena De León Prado, Dora Alicia Cortés Hernández, Javier Sánchez

Abstract:

Among the different cancer treatments that are currently used, hyperthermia has a promising potential due to the multiple benefits that are obtained by this technique. In general terms, hyperthermia is a method that takes advantage of the sensitivity of cancer cells to heat, in order to damage or destroy them. Within the different ways of supplying heat to cancer cells and achieve their destruction or damage, the use of magnetic nanoparticles has attracted attention due to the capability of these particles to generate heat under the influence of an external magnetic field. In addition, these nanoparticles have a high surface area and sizes similar or even lower than biological entities, which allow their approaching and interaction with a specific region of interest. The most used magnetic nanoparticles for hyperthermia treatment are those based on iron oxides, mainly magnetite and maghemite, due to their biocompatibility, good magnetic properties and chemical stability. However, in order to fulfill more efficiently the requirements that demand the treatment of magnetic hyperthermia, there have been investigations using ferrites that incorporate different metallic ions, such as Mg, Mn, Co, Ca, Ni, Cu, Li, Gd, etc., in their structure. This paper reports the synthesis of nanosized Mg_xMn_1-xFe₂O₄ (x = 0.3 and 0.4) ferrites by sol-gel method and their evaluation in terms of heating capability and in vitro hemolysis to determine the potential use of these nanoparticles as thermoseeds for the treatment of cancer by magnetic hyperthermia. It was possible to obtain ferrites with nanometric sizes, a single crystalline phase with an inverse spinel structure and a behavior near to that of superparamagnetic materials. Additionally, at concentrations of 10 mg of magnetic material per mL of water, it was possible to reach a temperature of approximately 45°C, which is within the range of temperatures used for the treatment of hyperthermia. The results of the in vitro hemolysis assay showed that, at the concentrations tested, these nanoparticles are non-hemolytic, as their percentage of hemolysis is close to zero. Therefore, these materials can be used as thermoseeds for the treatment of cancer by magnetic hyperthermia.

Keywords: Ferrites, heating capability, hemolysis, nanoparticles, sol-gel.

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Authors: Md. Maksudur Rahman Khan, M. Rahim Uddin, Hamidah Abdullah, Kaykobad Md. Rezaul Karim, Abu Yousuf, Chin Kui Cheng, Huei Ruey Ong

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A systematic study was conducted to explore the photocatalytic reduction of carbon dioxide (CO₂) into methanol on TiO₂ loaded copper ferrite (CuFe₂O₄) photocatalyst under visible light irradiation. The phases and crystallite size of the photocatalysts were characterized by X-ray diffraction (XRD) and it indicates CuFe₂O₄ as tetragonal phase incorporation with anatase TiO₂ in CuFe₂O₄/TiO₂ hetero-structure. The XRD results confirmed the formation of spinel type tetragonal CuFe₂O₄ phases along with predominantly anatase phase of TiO₂ in the CuFe₂O₄/TiO₂ hetero-structure. UV-Vis absorption spectrum suggested the formation of the hetero-junction with relatively lower band gap than that of TiO₂. Photoluminescence (PL) technique was used to study the electron–hole (e⁻/h⁺) recombination process. PL spectra analysis confirmed the slow-down of the recombination of electron–hole (e⁻/h⁺) pairs in the CuFe₂O₄/TiO₂ hetero-structure. The photocatalytic performance of CuFe₂O₄/TiO₂ was evaluated based on the methanol yield with varying amount of TiO₂ over CuFe₂O₄ (0.5:1, 1:1, and 2:1) and changing light intensity. The mechanism of the photocatalysis was proposed based on the fact that the predominant species of CO₂ in aqueous phase were dissolved CO₂ and HCO₃^- at pH ~5.9. It was evident that the CuFe₂O₄ could harvest the electrons under visible light irradiation, which could further be injected to the conduction band of TiO₂ to increase the life time of the electron and facilitating the reactions of CO₂ to methanol. The developed catalyst showed good recycle ability up to four cycles where the loss of activity was ~25%. Methanol was observed as the main product over CuFe₂O₄, but loading with TiO₂ remarkably increased the methanol yield. Methanol yield over CuFe₂O₄/TiO₂ was found to be about three times higher (651 μmol/g_cat L) than that of CuFe₂O₄ photocatalyst. This occurs because the energy of the band excited electrons lies above the redox potentials of the reaction products CO₂/CH₃OH.

Keywords: Photocatalysis, CuFe2O4/TiO2, band-gap energy, methanol.

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