Applicability of Routine Methods of Crystallite Size Analysis

1963 ◽  
pp. 191-201 ◽  
Author(s):  
Robert C. Rau
Nanomaterials ◽  
2020 ◽  
Vol 10 (8) ◽  
pp. 1500
Author(s):  
Laura Madalina Cursaru ◽  
Roxana Mioara Piticescu ◽  
Dumitru Valentin Dragut ◽  
Robert Morel ◽  
Caroline Thébault ◽  
...  

Iron oxide nanoparticles have received remarkable attention in different applications. For biomedical applications, they need to possess suitable core size, acceptable hydrodynamic diameter, high saturation magnetization, and reduced toxicity. Our aim is to control the synthesis parameters of nanostructured iron oxides in order to obtain magnetite nanoparticles in a single step, in environmentally friendly conditions, under inert gas atmosphere. The physical–chemical, structural, magnetic, and biocompatible properties of magnetite prepared by hydrothermal method in different temperature and pressure conditions have been explored. Magnetite formation has been proved by Fourier-transform infrared spectroscopy and X-ray diffraction characterization. It has been found that crystallite size increases with pressure and temperature increase, while hydrodynamic diameter is influenced by temperature. Magnetic measurements indicated that the magnetic core of particles synthesized at high temperature is larger, in accordance with the crystallite size analysis. Particles synthesized at 100 °C have nearly identical magnetic moments, at 20 × 103 μB, corresponding to magnetic cores of 10–11 nm, while the particles synthesized at 200 °C show slightly higher magnetic moments (25 × 103 μB) and larger magnetic cores (13 nm). Viability test results revealed that the particles show only minor intrinsic toxicity, meaning that these particles could be suited for biomedical applications.


2017 ◽  
Vol 32 (S1) ◽  
pp. S27-S34 ◽  
Author(s):  
D. Ectors ◽  
F. Goetz-Neunhoeffer ◽  
J. Neubauer

In this study, the application of (an)isotropic size determination using a recently proposed model for the double-Voigt approach is demonstrated and validated against line profile simulations using the Whole Powder Pattern Modelling approach. The fitting of simulated line profiles demonstrates that the attained crystallite sizes and morphologies are in very reasonable agreement with the simulated values and thus demonstrate that even in routine application scenarios credible size and morphology information can be obtained using the double-Voigt approximation. The aim of this contribution is to provide a comprehensive introduction to the problem, address the practical application of the developed model, and discuss the accuracy of the double-Voigt approach and derived size parameters. Mathematical formulations for the visualization of modeled morphologies, supporting the application of the recently developed macros, are additionally provided.


1962 ◽  
Vol 6 ◽  
pp. 191-201
Author(s):  
Robert C. Rau

AbstractSeveral methods for the routine determination of crystallite size by means of X-ray diffraction line-broadening have previously been reported. Although these techniques have proven useful and reliable when utilized with the single X-ray diffractometer and instrumental geometry used to originally develop the methods, it was not known whether other instruments would provide similar reliability. Therefore a study was performed to evaluate the applicability of routine methods of crystallite size analysis to other X-ray diffraction units. A series of six beryllium oxide powder specimens, whose average crystallite sizes ranged stepwise from about 35 to nearly 3000 Å, were used to test a number of X-ray diffractometers. By using a predetermined diffraction geometry for each instrument tested, measured crystallite sizes were found to be quite reproducible and well within the limits of experimental error. The testing procedure, instrumental conditions, and individual performance results are presented in this paper.


1996 ◽  
Vol 457 ◽  
Author(s):  
D. Sriram ◽  
R. L. Snyder ◽  
V. R. W. Amarakoon

ABSTRACTNanocrystalline copper ferrite (Cu0.5Fe2.5O4) was synthesized using a forward strike gelation method with polyacrylic acid (PAA) as a gelating agent. The dried gel was calcined at a low temperature of 400 °C to get the final powder. The effect of pH and the ratio of the cation to the carboxylic group in the initial gel were studied with respect to both the phases and the crystallite size of the final powders synthesized. Phase and crystallite size analysis were done using x-ray diffraction and TEM. Saturation magnetization results were obtained using a SQUID magnetometer. The reactions occurring in the nano-size copper ferrite, in air as a function of temperature, were tracked using adynamic high temperature x-ray diffraction (HTXRD) system.


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