Thickness and composition determinations from T.E.M. specimens using both x-ray and backscattered electron data

Author(s):  
M.D. Ball ◽  
H. Lagace ◽  
M.C. Thornton

The backscattered electron coefficient η for transmission electron microscope specimens depends on both the atomic number Z and the thickness t. Hence for specimens of known atomic number, the thickness can be determined from backscattered electron coefficient measurements. This work describes a simple and convenient method of estimating the thickness and the corrected composition of areas of uncertain atomic number by combining x-ray microanalysis and backscattered electron intensity measurements.The method is best described in terms of the flow chart shown In Figure 1. Having selected a feature of interest, x-ray microanalysis data is recorded and used to estimate the composition. At this stage thickness corrections for absorption and fluorescence are not performed.

Author(s):  
G. Cliff ◽  
M.J. Nasir ◽  
G.W. Lorimer ◽  
N. Ridley

In a specimen which is transmission thin to 100 kV electrons - a sample in which X-ray absorption is so insignificant that it can be neglected and where fluorescence effects can generally be ignored (1,2) - a ratio of characteristic X-ray intensities, I1/I2 can be converted into a weight fraction ratio, C1/C2, using the equationwhere k12 is, at a given voltage, a constant independent of composition or thickness, k12 values can be determined experimentally from thin standards (3) or calculated (4,6). Both experimental and calculated k12 values have been obtained for K(11<Z>19),kα(Z>19) and some Lα radiation (3,6) at 100 kV. The object of the present series of experiments was to experimentally determine k12 values at voltages between 200 and 1000 kV and to compare these with calculated values.The experiments were carried out on an AEI-EM7 HVEM fitted with an energy dispersive X-ray detector.


Author(s):  
R. Sinclair ◽  
B.E. Jacobson

INTRODUCTIONThe prospect of performing chemical analysis of thin specimens at any desired level of resolution is particularly appealing to the materials scientist. Commercial TEM-based systems are now available which virtually provide this capability. The purpose of this contribution is to illustrate its application to problems which would have been intractable until recently, pointing out some current limitations.X-RAY ANALYSISIn an attempt to fabricate superconducting materials with high critical currents and temperature, thin Nb3Sn films have been prepared by electron beam vapor deposition [1]. Fine-grain size material is desirable which may be achieved by codeposition with small amounts of Al2O3 . Figure 1 shows the STEM microstructure, with large (∽ 200 Å dia) voids present at the grain boundaries. Higher quality TEM micrographs (e.g. fig. 2) reveal the presence of small voids within the grains which are absent in pure Nb3Sn prepared under identical conditions. The X-ray spectrum from large (∽ lμ dia) or small (∽100 Ǻ dia) areas within the grains indicates only small amounts of A1 (fig.3).


2021 ◽  
Author(s):  
Yan Chen ◽  
Yuemei Lan ◽  
Dong Wang ◽  
Guoxing Zhang ◽  
Wenlong Peng ◽  
...  

A series of Gd2-xMoO6:xEu3+(x=0.18-0.38) nanophosphors were synthesized by the solvothermal method. The properties of this nanophosphor were characterized by x-ray diffraction (XRD), transmission electron microscope (TEM), fluorescence spectra and diffuse...


2011 ◽  
Vol 80-81 ◽  
pp. 217-220 ◽  
Author(s):  
Xue Qing Yue ◽  
Hai Jun Fu ◽  
Da Jun Li

Graphite encapsulated nickel nanoparticles were prepared by ball milling andsubsequently annealing a mixture of expanded graphite with nickel powders. The products were characterized by transmission electron microscope and X-ray diffraction. The formation mechanism of the products was discussed. Results show that the products have a size range of 20-150 nm. The graphite and nickel in the products all exhibit a high crystallinity.


2011 ◽  
Vol 311-313 ◽  
pp. 1713-1716 ◽  
Author(s):  
Yan Rong Sun ◽  
Tao Fan ◽  
Chang An Wang ◽  
Li Guo Ma ◽  
Feng Liu

Nano-hydroxyapatite with different morphology was synthesized by the co-precipitation method coupled with biomineralization using Ca(NO3)2•4H2O and (NH4)2HPO4 as reagents, adding chondroitin sulfate, agarose and aspartic acid as template. The structure and morphology of the prepared powders were characterized by X-ray diffraction (XRD) and transmission electron microscope (TEM).


Nanopages ◽  
2019 ◽  
pp. 1-11
Author(s):  
G. M. Taha ◽  
M. N. Rashed ◽  
M. S. El-Sadek ◽  
M. A. Moghazy

Abstract BiFeO3 (BFO) nanopowder was synthesized in a pure form via a sol- gel method based on glycol gel reaction. Effect of drying and preheating temperature on preventing other phases was studied. Many parameters were studied as calcination temperature and time & stirring temperature as well. The prepared powder was characterized by X-Ray Diffraction of powder (XRD) and Transmission Electron Microscope (TEM). High pure BiFeO3 was obtained by preheated process at 400 °C for 0.5 h and calcination at 600 °C for 0.5 h without any impurities compared to dry at110 °C.


2001 ◽  
Vol 7 (2) ◽  
pp. 211-219 ◽  
Author(s):  
Patrick Echlin

Abstract A brief description is given of the events surrounding the development of biological X-ray microanalysis during the last 30 years, with particular emphasis on the contribution made by research workers in Cambridge, UK. There then follows a broad review of some applications of biological X-ray microanalysis. A more detailed consideration is given to the main thrust of current procedures and applications that are, for convenience, considered as four different kinds of samples. Thin frozen dried sections which are analyzed at ambient temperatures in a transmission electron microscope (TEM); semithin frozen dried sections which are analyzed at low temperature in a scanning transmission electron microscope (STEM); thick frozen hydrated sections which are analyzed at low temperature in a scanning electron microscope (SEM), and bulk samples which are analyzed at low temperature in the same type of instrument. A brief outline is given of the advantages and disadvantages of performing low-voltage, low-temperature X-ray microanalysis on frozen hydrated bulk biological material. The article concludes with a consideration of alternative approaches to in situ analysis using either high-energy beams or visible and near-visible photons.


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