Automated particle analysis in Electron Microscopy

Author(s):  
Tim B. Vander Wood

The ability to quickly and economically characterize particle samples is increasingly important. A knowledge of particle size distributions can be critical in a wide variety of processes, from powder metallurgy to ethical drug delivery. Powdered materials may be contaminated at levels of only one particle in one thousand and still be unsuitable for use. Particulate samples may represent a variety of materials from many sources, requiring complex analyses for complete characterization. The traditional analytical approach to these problems, dictated by the need for economy, has been the application of batch techniques (e.g. light scattering) to the problem of particle sizing and trace component and bulk techniques (e.g. atomic absorption, x-ray fluorescence) to the problems of particle analysis. Scanning electron microscopy (SEM), combined with energy-dispersive x-ray spectrometry (EDS), is capable of directly measuring the required individual particle sizes, morphologies and compositions but has not been widely applied due to the high cost of analysis of several hundred to thousands of particles which may be required to adequately represent an entire population.

1987 ◽  
Vol 111 ◽  
Author(s):  
Roseann Csencsits ◽  
Ronald Gronsky ◽  
Vinayan Nair ◽  
Rosemarie Szostak

AbstractThe effects of various synthesis conditions on the structure and composition of ferrisilicate analogs of zeolite ZSM-5 were considered. Scanning electron microscopy (SEM) was used to determine the particles size distributions and morphologies. Particle sizes vary from tenths of a micron to several microns, depending on degree of agitation during crystal growth, while morphology is additionally dependent on the concentration of iron in the gel during crystallization.X-ray emissive spectroscopy (XES) performed in the transmission electron microscope (TEM) was used to determine their composition variation. The distribution of iron amongst the crystals is more homogeneous if the gel is stirred and it does not depend on particle size.


2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Seyed Abolghasem Kahani ◽  
Zahra Yagini

The preparation of Fe3O4from ferrous salt by air in alkaline aqueous solution at various temperatures was proposed. The synthetic magnetites have different particle size distributions. We studied the properties of the magnetite prepared by chemical methods compared with magnetotactic bacterial nanoparticles. The results show that crystallite size, morphology, and particle size distribution of chemically prepared magnetite at 293 K are similar to biosynthesis of magnetite. The new preparation of Fe3O4helps to explain the mechanism of formation of magnetosomes in magnetotactic bacteria. The products are characterized by X-ray powder diffraction (XRD), infrared (IR) spectra, vibrating sample magnetometry (VSM), and scanning electron microscopy (SEM).


1998 ◽  
Vol 13 (9) ◽  
pp. 2588-2596 ◽  
Author(s):  
K. H. Ryu ◽  
J-M. Yang

The low temperature pressureless sintering of a nanosized Si3N4 powder with doped sintering additives was investigated. The microstructural evolution during sintering at different temperatures was analyzed using x-ray diffraction and scanning electron microscopy. The effect of using nanosized Si3N4 powder as a catalyst to accelerate the α→β–Si3N4 transformation of a commercial Si3N4 powder with larger particle sizes was also investigated. Finally, two stage sintering was used to study the feasibility of controlling the microstructure and the mechanical properties of the nanosized silicon nitride.


MRS Advances ◽  
2020 ◽  
Vol 5 (29-30) ◽  
pp. 1623-1623
Author(s):  
Adriana Valério ◽  
Sérgio L. Morelhão ◽  
Alex J. Freitas Cabral ◽  
Márcio M. Soares ◽  
Cláudio M. R. Remédios

2016 ◽  
Vol 22 (1) ◽  
pp. 39-47 ◽  
Author(s):  
Eva M. Pala ◽  
Sudip Dey

AbstractConventional and highly sophisticated analytical methods (Cyria et al., 1989; Massar et al., 2012a) were used to analyze micro-structural and micro-analytical aspects of the blood of snake head fish, Channa gachua, exposed to municipal wastes and city garbage. Red (RBC) and white blood cell (WBC) counts and hemhemoglobin content were found to be higher in pollution affected fish as compared with control. Scanning electron microscopy revealed the occurrence of abnormal erythrocytes such as crenated cells, echinocytes, lobopodial projections, membrane internalization, spherocytes, ruptured cells, contracted cells, depression, and uneven elongation of erythrocyte membranes in fish inhabiting the polluted sites. Energy-dispersive X-ray spectroscopy (EDS) revealed the presence of silicon and lead in the RBCs of pollution affected fish. Significance of the study includes the highly sophisticated analytical approach, which revealed the aforementioned micro-structural abnormalities.


2015 ◽  
Vol 1109 ◽  
pp. 314-318
Author(s):  
Nor Diyana Abdul Aziz ◽  
Kelimah Elong ◽  
Norlida Kamarulzaman

Tin Oxide (SnO2) is a metal oxide which has many applications in industry. In this study, SnO2 powders were synthesized by a self-propagating combustion (SPC) method. The product was annealed at 800 °C for 12 and 24 h before characterizing with X-Ray Diffraction (XRD) for phase studies. X-Ray Diffraction results showed that both samples are pure of tetragonal structure with space group P42/mnm. The sample annealed at a longer period, that is, 24 h, shows a higher degree of crystallinity compared to the 12 h annealed sample. It also shows a smaller full width at half maximum (FWHM), indicating larger crystallite size for the 24 h annealed sample. The particle size analysis reveals that there are two groups of particle size distributions for both samples. SEM results give values that are different from the particle sizer results due to the different nature of the measurement methods.


1970 ◽  
Vol 14 ◽  
pp. 29-37 ◽  
Author(s):  
S. T. Silk ◽  
S. Z. Lewin

AbstractIt is shown that the integrated intensities of diffraction lines from calcite and aragonite powders prepared by precipitation vary markedly, due to variations in sample packing efficiency arising from different degrees of polydispersity in the particle size distributions. Since prolonged grinding to equalize initially divergent distributions changes the polymorph composition, the packing effect imposes the principal limitation on the precision of the x-ray method for certain types of calcium carbonate preparations.


Crystals ◽  
2020 ◽  
Vol 10 (7) ◽  
pp. 580
Author(s):  
Victor R.A. Dubach ◽  
Albert Guskov

X-ray crystallography and single-particle analysis cryogenic electron microscopy are essential techniques for uncovering the three-dimensional structures of biological macromolecules. Both techniques rely on the Fourier transform to calculate experimental maps. However, one of the crucial parameters, resolution, is rather broadly defined. Here, the methods to determine the resolution in X-ray crystallography and single-particle analysis are summarized. In X-ray crystallography, it is becoming increasingly more common to include reflections discarded previously by traditionally used standards, allowing for the inclusion of incomplete and anisotropic reflections into the refinement process. In general, the resolution is the smallest lattice spacing given by Bragg’s law for a particular set of X-ray diffraction intensities; however, typically the resolution is truncated by the user during the data processing based on certain parameters and later it is used during refinement. However, at which resolution to perform such a truncation is not always clear and this makes it very confusing for the novices entering the structural biology field. Furthermore, it is argued that the effective resolution should be also reported as it is a more descriptive measure accounting for anisotropy and incompleteness of the data. In single particle cryo-EM, the situation is not much better, as multiple ways exist to determine the resolution, such as Fourier shell correlation, spectral signal-to-noise ratio and the Fourier neighbor correlation. The most widely accepted is the Fourier shell correlation using a threshold of 0.143 to define the resolution (so-called “gold-standard”), although it is still debated whether this is the correct threshold. Besides, the resolution obtained from the Fourier shell correlation is an estimate of varying resolution across the density map. In reality, the interpretability of the map is more important than the numerical value of the resolution.


2010 ◽  
Vol 65 (8) ◽  
pp. 1033-1037 ◽  
Author(s):  
Sridhar Komarneni ◽  
Young Dong Noh ◽  
Joo Young Kim ◽  
Seok Han Kim ◽  
Hiroaki Katsuki

Anatase and Ca, Sr and Ca0.5Sr0.5 hydroxyapatites were synthesized by conventional-hydrothermal (C-H) as well asmicrowave-hydrothermal (M-H)methods.Microwave-assisted reactions led to accelerated syntheses of anatase but no such acceleration of reactions could be detected with the syntheses of hydroxyapatites because the crystallization of the latter materials occurred at very low temperature. Cu and Au metal powders were produced by using glucose, fructose or sucrose as reducing agents under C-H conditions at 160 ℃, where fructose and sucrose were found to be stronger reducing agents than glucose. The crystallinity of all the powders was characterized by powder X-ray diffraction, and morphology and particle sizes were determined by scanning or transmission electron microscopy


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