A Thermal Decomposition Approach for the Synthesis of Iron Oxide Microspheres

2013 ◽  
Vol 1547 ◽  
pp. 155-160 ◽  
Author(s):  
Geetu Sharma ◽  
Jeevanandam Pethaiyan
Keyword(s):  
Electron Microscopy ◽  
Thermal Decomposition ◽  
Iron Oxide ◽  
Environmental Remediation ◽  
Diffuse Reflectance Spectroscopy ◽  
Magnetic Measurement ◽  
Synthetic Methods ◽  
Dimethyl Formamide ◽  
Decomposition Approach ◽  
Wide Range

ABSTRACTIron oxide microspheres possess a wide range of applications in lithium storage batteries, sensors, photocatalysis, environmental remediation, magnetic resonance imaging and drug delivery. The most commonly used method for the preparation of iron oxide microspheres is hydrothermal synthesis. Besides this, other synthetic methods such as co-precipitation, electrostatic self- assembly, microwave and sol-gel have been reported. The reported synthetic methods usually require longer time (2 to 48 hours) and expensive experimental set up. In the present study, a novel low temperature thermal decomposition approach for the synthesis of iron oxide microspheres has been reported. Thermal decomposition of an iron-urea complex ([Fe(CON2H4)6](NO3)3) in a mixture of diphenyl ether and dimethyl formamide at 200 °C for 35 minutes leads to the formation of iron oxide microspheres. The microspheres were characterized using a variety of analytical techniques such as X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), diffuse reflectance spectroscopy (DRS) and magnetometry. The XRD results indicated amorphous nature for the as prepared iron oxide, whereas after calcination at 500 °C, crystalline α-Fe2O3 phase is obtained. The SEM images indicated uniform spheres with an average diameter of 1.2 ± 0.3 μm. The DRS results too gave evidence for the formation of α-Fe2O3 on calcination of the microspheres at 500 oC.The field and temperature dependent magnetic measurement results indicated superparamagnetic behavior for the as prepared iron oxide microspheres indicating that the microspheres consist of iron oxide nanoparticles. On the other hand, an antiferromagnetic behavior was observed for the microspheres calcined at 500 °C. The present synthetic method is a novel method to produce magnetic materials with controlled morphologies.

Synthesis of Iron Oxide Nanoparticles by Thermal Decomposition Approach

2009 ◽  
Vol 67 ◽  
pp. 221-226 ◽  
Author(s):  
Shuchi Dixit ◽  
P. Jeevanandam
Keyword(s):  
Thermal Decomposition ◽  
Oleic Acid ◽  
Iron Oxide ◽  
Iron Oxide Nanoparticles ◽  
Diphenyl Ether ◽  
Oxide Nanoparticles ◽  
One Pot ◽  
Decomposition Approach ◽  
Oleyl Amine ◽  
Acetyl Acetonate

An easy onepot reaction for the synthesis of iron oxide nanoparticles is reported. Thermal decomposition of iron acetyl acetonate (Fe(acac)3) in diphenyl ether, in the presence of oleic acid and oleyl amine followed by calcination, leads to the formation of iron oxide nanoparticles. Variation of concentration of the oleyl amine during the synthesis affects the morphology of the iron oxide nanoparticles produced.

scholarly journals Facile Synthesis of Heterojunctioned ZnO/Bi2S3 Nanocomposites for Enhanced Photocatalytic Reduction of Aqueous Cr(VI) under Visible-Light Irradiation

Catalysts ◽  
2019 ◽  
Vol 9 (7) ◽  
pp. 624 ◽  
Author(s):  
Xiaoya Yuan ◽  
Xue Wu ◽  
Zijuan Feng ◽  
Wen Jia ◽  
Xuxu Zheng ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Visible Light ◽  
Photoelectron Spectroscopy ◽  
Environmental Remediation ◽  
High Efficiency ◽  
Diffuse Reflectance Spectroscopy ◽  
Structured Materials ◽  
X Ray ◽  
Transmission Electron ◽  
Facile Solvothermal Method

Heterojunctioned ZnO/Bi2S3 nanocomposites were prepared via a facile solvothermal method. The obtained photocatalysts were characterized by X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), High resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), UV-Vis diffuse reflectance spectroscopy (DRS), and Photoelectrochemical and Photoluminescence spectroscopy (PL), respectively. The results showed that ZnO/Bi2S3 composites exhibited the sandwiched-like structure, where ZnO nanoparticles were randomly embedded between Bi2S3 nanoflakes. The performance of photocatalytic Cr(VI) reduction under visible light indicated that ZnO/Bi2S3 composites exhibited high-efficiency photocatalytic activity in comparison with either Bi2S3 or ZnO. The 5%-ZnO/Bi2S3 photocatalyst removed 96% of Cr(VI) within 120 min at 20 mg/L initial concentration of Cr(VI). The enhanced performance of ZnO/Bi2S3 photocatalysts could be ascribed to the increased light harvesting and the effective separation and transfer of the photogenerated charge carriers across the heterojunction interface of the ZnO/Bi2S3 composite. This work could pave the way for the design of new hetero-structured materials and has great potential in environmental remediation.

Recent Applications of High Resolution Electron Microscopy to Crystalline Arrays of Virus Particles

1978 ◽  
Vol 36 (3) ◽  
pp. 470-482 ◽  
Author(s):  
R.W. Horne
Keyword(s):  
Electron Microscopy ◽  
Image Processing ◽  
Analytical Techniques ◽  
Staining Technique ◽  
High Resolution Electron Microscopy ◽  
Optical Diffraction ◽  
Full Potential ◽  
Virus Particles ◽  
Resolution Electron ◽  
Wide Range

The technique of surrounding virus particles with a neutralised electron dense stain was described at the Fourth International Congress on Electron Microscopy, Berlin 1958 (see Home & Brenner, 1960, p. 625). For many years the negative staining technique in one form or another, has been applied to a wide range of biological materials. However, the full potential of the method has only recently been explored following the development and applications of optical diffraction and computer image analytical techniques to electron micrographs (cf. De Hosier & Klug, 1968; Markham 1968; Crowther et al., 1970; Home & Markham, 1973; Klug & Berger, 1974; Crowther & Klug, 1975). These image processing procedures have allowed a more precise and quantitative approach to be made concerning the interpretation, measurement and reconstruction of repeating features in certain biological systems.

Applications of Photoelectron Microscopy

1976 ◽  
Vol 34 ◽  
pp. 506-507
Author(s):  
William J. Baxter
Keyword(s):  
Electron Microscopy ◽  
Thermal Decomposition ◽  
Chemical Composition ◽  
Ultraviolet Radiation ◽  
Thin Layer ◽  
Edge Effects ◽  
Electron Optics ◽  
Surface Layers ◽  
Crystalline Orientation ◽  
Fluorescent Screen

In this form of electron microscopy, photoelectrons emitted from a metal by ultraviolet radiation are accelerated and imaged onto a fluorescent screen by conventional electron optics. image contrast is determined by spatial variations in the intensity of the photoemission. The dominant source of contrast is due to changes in the photoelectric work function, between surfaces of different crystalline orientation, or different chemical composition. Topographical variations produce a relatively weak contrast due to shadowing and edge effects.Since the photoelectrons originate from the surface layers (e.g. ∼5-10 nm for metals), photoelectron microscopy is surface sensitive. Thus to see the microstructure of a metal the thin layer (∼3 nm) of surface oxide must be removed, either by ion bombardment or by thermal decomposition in the vacuum of the microscope.

Microwaves: Application in Electron Microscopy

1990 ◽  
Vol 48 (3) ◽  
pp. 140-141
Author(s):  
Anthony S-Y Leong ◽  
David W Gove
Keyword(s):  
Electron Microscopy ◽  
Light Microscopy ◽  
Chemical Reactions ◽  
Electromagnetic Waves ◽  
Tissue Fixation ◽  
Primary Method ◽  
Dipolar Molecules ◽  
Wide Range ◽  
Time Required ◽  
Cryostat Sections

Microwaves (MW) are electromagnetic waves which are commonly generated at a frequency of 2.45 GHz. When dipolar molecules such as water, the polar side chains of proteins and other molecules with an uneven distribution of electrical charge are exposed to such non-ionizing radiation, they oscillate through 180° at a rate of 2,450 million cycles/s. This rapid kinetic movement results in accelerated chemical reactions and produces instantaneous heat. MWs have recently been applied to a wide range of procedures for light microscopy. MWs generated by domestic ovens have been used as a primary method of tissue fixation, it has been applied to the various stages of tissue processing as well as to a wide variety of staining procedures. This use of MWs has not only resulted in drastic reductions in the time required for tissue fixation, processing and staining, but have also produced better cytologic images in cryostat sections, and more importantly, have resulted in better preservation of cellular antigens.

Recent Progress and Plans in Computer-Controlled High Resolution Electron Microscopy

1990 ◽  
Vol 48 (1) ◽  
pp. 154-155
Author(s):  
W.J. de Ruijter ◽  
Peter Rez ◽  
David J. Smith
Keyword(s):  
Electron Microscopy ◽  
Digital Processing ◽  
High Resolution Electron Microscopy ◽  
Objective Lens ◽  
Linear Filter ◽  
Contrast Transfer Function ◽  
Image Displacement ◽  
Spatially Resolved ◽  
Wide Range ◽  
On Line

Digital computers are becoming widely recognized as standard accessories for electron microscopy. Due to instrumental innovations the emphasis in digital processing is shifting from off-line manipulation of electron micrographs to on-line image acquisition, analysis and microscope control. An on-line computer leads to better utilization of the instrument and, moreover, the flexibility of software control creates the possibility of a wide range of novel experiments, for example, based on temporal and spatially resolved acquisition of images or microdiffraction patterns. The instrumental resolution in electron microscopy is often restricted by a combination of specimen movement, radiation damage and improper microscope adjustment (where the settings of focus, objective lens stigmatism and especially beam alignment are most critical). We are investigating the possibility of proper microscope alignment based on computer induced tilt of the electron beam. Image details corresponding to specimen spacings larger than ∼20Å are produced mainly through amplitude contrast; an analysis based on geometric optics indicates that beam tilt causes a simple image displacement. Higher resolution detail is characterized by wave propagation through the optical system of the microscope and we find that beam tilt results in a dispersive image displacement, i.e. the displacement varies with spacing. This approach is valid for weak phase objects (such as amorphous thin films), where transfer is simply described by a linear filter (phase contrast transfer function) and for crystalline materials, where imaging is described in terms of dynamical scattering and non-linear imaging theory. In both cases beam tilt introduces image artefacts.

Substituent Effects on the Thermal Decomposition of Phosphate Esters on Ferrous Surfaces

2019 ◽  
Author(s):  
James Ewen ◽  
Carlos Ayestaran Latorre ◽  
Arash Khajeh ◽  
Joshua Moore ◽  
Joseph Remias ◽  
...  
Keyword(s):  
Thermal Decomposition ◽  
Film Formation ◽  
Substituent Effects ◽  
Vapour Phase ◽  
Industrial Applications ◽  
Phosphate Esters ◽  
Antiwear Additives ◽  
Formation Mechanisms ◽  
Phosphate Ester ◽  
Wide Range

<p>Phosphate esters have a wide range of industrial applications, for example in tribology where they are used as vapour phase lubricants and antiwear additives. To rationally design phosphate esters with improved tribological performance, an atomic-level understanding of their film formation mechanisms is required. One important aspect is the thermal decomposition of phosphate esters on steel surfaces, since this initiates film formation. In this study, ReaxFF molecular dynamics simulations are used to study the thermal decomposition of phosphate esters with different substituents on several ferrous surfaces. On Fe<sub>3</sub>O<sub>4</sub>(001) and α-Fe(110), chemisorption interactions between the phosphate esters and the surfaces occur even at room temperature, and the number of molecule-surface bonds increases as the temperature is increased from 300 to 1000 K. Conversely, on hydroxylated, amorphous Fe<sub>3</sub>O<sub>4</sub>, most of the molecules are physisorbed, even at high temperature. Thermal decomposition rates were much higher on Fe<sub>3</sub>O<sub>4</sub>(001) and particularly α-Fe(110) compared to hydroxylated, amorphous Fe<sub>3</sub>O<sub>4</sub>. This suggests that water passivates ferrous surfaces and inhibits phosphate ester chemisorption, decomposition, and ultimately film formation. On Fe<sub>3</sub>O<sub>4</sub>(001), thermal decomposition proceeds mainly through C-O cleavage (to form surface alkyl and aryl groups) and C-H cleavage (to form surface hydroxyls). The onset temperature for C-O cleavage on Fe<sub>3</sub>O<sub>4</sub>(001) increases in the order: tertiary alkyl < secondary alkyl < primary linear alkyl ≈ primary branched alkyl < aryl. This order is in agreement with experimental observations for the thermal stability of antiwear additives with similar substituents. The results highlight surface and substituent effects on the thermal decomposition of phosphate esters which should be helpful for the design of new molecules with improved performance.</p>

Double Ring-Closing Approach for the Synthesis of 2,3,6,7-Substituted Anthracene Derivatives

2020 ◽  
Author(s):  
Birgit Meindl ◽  
Katharina Pfennigbauer ◽  
Berthold Stöger ◽  
Martin Heeney ◽  
Florian Glöcklhofer
Keyword(s):  
Wittig Reaction ◽  
Condensation Reaction ◽  
Synthetic Methods ◽  
Anthracene Derivative ◽  
Double Ring ◽  
Mild Conditions ◽  
Wide Range ◽  
Anthracene Derivatives

Anthracene derivatives have been used for a wide range of applications and many different synthetic methods for their preparation have been developed. However, despite continued synthetic efforts, introducing substituents in some positions has remained difficult. Here we present a method for the synthesis of 2,3,6,7-substituted anthracene derivatives, one of the most challenging anthracene substitution patterns to obtain. The method is exemplified by the preparation of 2,3,6,7-anthracenetetracarbonitrile and employs a newly developed, stable protected 1,2,4,5-benzenetetracarbaldehyde as the precursor. The precursor can be obtained in two scalable synthetic steps from 2,5-dibromoterephthalaldehyde and is converted into the anthracene derivative by a double intermolecular Wittig reaction under very mild conditions followed by a deprotection and intramolecular double ring-closing condensation reaction. Further modification of the precursor is expected to enable the introduction of additional substituents in other positions and may even enable the synthesis of fully substituted anthracene derivatives by the presented approach.<br>

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