scholarly journals Shape Tuning of Magnetite Nanoparticles Obtained by Hydrothermal Synthesis: Effect of Temperature

2019 ◽  
Vol 2019 ◽  
pp. 1-15 ◽  
Author(s):  
Nayely Torres-Gómez ◽  
Osvaldo Nava ◽  
Liliana Argueta-Figueroa ◽  
René García-Contreras ◽  
Armando Baeza-Barrera ◽  
...  

In this work, we present a simple and efficient method for pure phase magnetite (Fe3O4) nanoparticle synthesis. The phase structure, particle shape, and size of the samples were characterized by Raman spectroscopy (Rm), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDS), and transmission electron microscopy (TEM). The morphology tuning was controlled by the temperature of the reaction; the nanoparticles were synthesized via the hydrothermal method at 120°C, 140°C, and 160°C, respectively. The Rm and XRD spectra showed that all the nanoparticles were Fe3O4 in a pure magnetite phase. The obtained nanoparticles exhibited a high level of crystallinity with uniform morphology at each temperature, as can be observed through TEM and SEM. These magnetic nanoparticles exhibited good saturation magnetization and the resulting shapes were quasi-spheres, octahedrons, and cubes. The samples showed striking magnetic properties, which were examined by a vibrating sample magnetometer (VSM). It has been possible to obtain a good morphological control of nanostructured magnetite in a simple, economical, and scalable method by adjusting the temperature, without the modification of any other synthesis parameter.

Catalysts ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 899
Author(s):  
Murendeni P. Ravele ◽  
Opeyemi A. Oyewo ◽  
Damian C. Onwudiwe

Pure-phase Cu2−xS (x = 1, 0.2) nanoparticles have been synthesized by the thermal decomposition of copper(II) dithiocarbamate as a single-source precursor in oleylamine as a capping agent. The compositions of the Cu2−xS nanocrystals varied from CuS (covellite) through the mixture of phases (CuS and Cu7.2S4) to Cu9S5 (digenite) by simply varying the temperature of synthesis. The crystallinity and morphology of the copper sulfides were studied using X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), which showed pure phases at low (120 °C) and high (220 °C) temperatures and a mixture of phases at intermediate temperatures (150 and 180 °C). Covellite was of a spherical morphology, while digenite was rod shaped. The optical properties of these nanocrystals were characterized by UV−vis–NIR and photoluminescence spectroscopies. Both samples had very similar absorption spectra but distinguishable fluorescence properties and exhibited a blue shift in their band gap energies compared to bulk Cu2−xS. The pure phases were used as catalysts for the photocatalytic degradation of tetracycline (TC) under visible-light irradiation. The results demonstrated that the photocatalytic activity of the digenite phase exhibited higher catalytic degradation of 98.5% compared to the covellite phase, which showed 88% degradation within the 120 min reaction time using 80 mg of the catalysts. The higher degradation efficiency achieved with the digenite phase was attributed to its higher absorption of the visible light compared to covellite.


Catalysts ◽  
2021 ◽  
Vol 11 (10) ◽  
pp. 1238
Author(s):  
Murendeni P. Ravele ◽  
Opeyemi A. Oyewo ◽  
Sam Ramaila ◽  
Lydia Mavuru ◽  
Damian C. Onwudiwe

In this paper, spherical-shaped pure phase djurleite (Cu31S16) and roxbyite (Cu7S4) nanoparticles were prepared by a solvothermal decomposition of copper(II) dithiocarbamate complex in dodecanthiol (DDT). The reaction temperature was used to control the phases of the samples, which were represented as Cu31S16 (120 °C), Cu31S16 (150 °C), Cu7S4 (220 °C), and Cu7S4 (250 °C) and were characterized by using X-ray diffraction (XRD), scanning and transmission electron microscopy (SEM and TEM), and absorption spectroscopy. The samples were used as photocatalysts for the degradation of tetracycline (TC) under visible light irradiation. The results of the study showed that Cu7S4 (250 °C) exhibited the best activity in the reaction system with the TC degradation rate of up to 99% within 120 min of light exposure, while the Cu31S16 (120 °C) system was only 46.5% at the same reaction condition. In general, roxbyite Cu7S4 (250 °C) could be considered as a potential catalyst for the degradation of TC in solution.


2011 ◽  
Vol 311-313 ◽  
pp. 545-548 ◽  
Author(s):  
Yu Jiang Wang ◽  
Yong Gang Wang

NiWO4 nanoparticles were successfully synthesized by a molten salt method at 270°C. The as-prepared powders were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM), and exhibited a pure phase NiWO4 with about 50 nm in particle size and uniform nearly-spherical particle shape.


2007 ◽  
Vol 62 (12) ◽  
pp. 754-760
Author(s):  
Chao-Chen Yang ◽  
Min-Fong Shu

The electrochemical behaviour of zinc on copper, platinum, and tungsten working electrodes was investigated in a binary ZnCl2-DMSO2 room temperature molten salt electrolyte in the temperature range of 60 - 80◦C. Various over-potentials, −0.1, −0.2, −0.3, −0.4, and −0.5 V, were chosen as deposition potentials. The nucleation/growth of zinc changed from progressive to instantaneous if the over-potentials increased from low to high level. The surface morphology and crystal structure of the deposited layer were investigated using scanning electron microscopy (SEM) and X-ray diffraction (XRD). Moreover, larger grain size and hexagonal close packing of the zinc layer at −0.5 V were observed by transmission electron microscopy (TEM) with electron diffraction mapping.


2018 ◽  
Vol 83 (5) ◽  
pp. 515-538 ◽  
Author(s):  
Andreia Corciova ◽  
Bianca Ivanescu

Nanotechnology is one of the most studied domains, and nanoparticle synthesis, especially of silver nanoparticles, has gained special importance due to their properties, biocompatibility and applications. Today, the processes of nanoparticles synthesis tend toward the development of inexpensive, simple, non-toxic and environmentally friendly methods. Thus, the use of plants in the synthesis of silver nanoparticles has attracted considerable interest because biomolecules can act as both reducing and stabilizing agents. This survey aims at discussing the conditions for obtaining silver nanoparticles using plants and their characterization by several methods, such as FTIR and UV?Vis spectroscopy, X-ray diffraction, and scanning and transmission electron microscopy. In addition, it examines some of the most common biological uses of silver nanoparticles: antibacterial, antioxidant and cytotoxic.


2004 ◽  
Vol 824 ◽  
Author(s):  
A.V. Ochkin ◽  
S.V. Stefanovsky ◽  
A.G. Ptashkin ◽  
N.S. Mikhailenko ◽  
O.I. Kirjanova

AbstractTwo ceramics for immobilization of a Zr-REE-actinide fraction of high level waste (HLW) based on zirconolite or/and pyrochlore structures with minor brannerite/lucasite, and fluorite-structured dioxide-based solid solution, were synthesized and characterized. The samples were produced by melting of oxide mixtures at 1500 °C followed by controlled cooling for crystallization. Phase compositions of the samples obtained and waste elements partitioning among co-existing phases were investigated in detail using powder X-ray diffraction, scanning electron microscopy with energy dispersive spectroscopy, and transmission electron microscopy. Cerium enters cerianite-based solid solution, lucasite (if present), and to a lesser extent, pyrochlore and zirconolite. Europium and gadolinium enter predominantly zirconolite and pyrochlore. The highest uranium concentrations were found in a uraninite-based cubic solid solution or pyrochlore and zirconolite.


2012 ◽  
Vol 430-432 ◽  
pp. 12-15
Author(s):  
Lin Lin Yang ◽  
Yu Jiang Wang ◽  
Shun Li Huang ◽  
Yong Gang Wang

Pure phase Fe doped BaTiO3 crystals have been successfully fabricated at 200°C with 0.7M KOH by a hydrothermal method. The obtained products were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). An obvious morphology evolution from hexagonal shape to sphericity was observed when Fe doping concentration was increased from 0% to 1%, 3%, 6%, and 10%. In addition, the size of the obtained Fe doped BaTiO3 crystals obviously became smaller. The possible mechanism was also discussed.


Author(s):  
R. Gronsky

The phenomenon of clustering in Al-Ag alloys has been extensively studied since the early work of Guinierl, wherein the pre-precipitation state was characterized as an assembly of spherical, ordered, silver-rich G.P. zones. Subsequent x-ray and TEM investigations yielded results in general agreement with this model. However, serious discrepancies were later revealed by the detailed x-ray diffraction - based computer simulations of Gragg and Cohen, i.e., the silver-rich clusters were instead octahedral in shape and fully disordered, atleast below 170°C. The object of the present investigation is to examine directly the structural characteristics of G.P. zones in Al-Ag by high resolution transmission electron microscopy.


Author(s):  
Vicki L. Baliga ◽  
Mary Ellen Counts

Calcium is an important element in the growth and development of plants and one form of calcium is calcium oxalate. Calcium oxalate has been found in leaf seed, stem material plant tissue culture, fungi and lichen using one or more of the following methods—polarized light microscopy (PLM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and x-ray diffraction.Two methods are presented here for qualitatively estimating calcium oxalate in dried or fixed tobacco (Nicotiana) leaf from different stalk positions using PLM. SEM, coupled with energy dispersive x-ray spectrometry (EDS), and powder x-ray diffraction were used to verify that the crystals observed in the dried leaf with PLM were calcium oxalate.


2002 ◽  
Vol 716 ◽  
Author(s):  
Seok Woo Hong ◽  
Yong Sun Lee ◽  
Ki-Chul Park ◽  
Jong-Wan Park

AbstractThe effect of microstructure of dc magnetron sputtered TiN and TaN diffusion barriers on the palladium activation for autocatalytic electroless copper deposition has been investigated by using X-ray diffraction, sheet resistance measurement, field emission scanning electron microscopy (FE-SEM) and plan view transmission electron microscopy (TEM). The density of palladium nuclei on TaN diffusion barrier increases as the grain size of TaN films decreases, which was caused by increasing nitrogen content in TaN films. Plan view TEM results of TiN and TaN diffusiton barriers showed that palladium nuclei formed mainly on the grain boundaries of the diffusion barriers.


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