Quantitative Energy Dispersive X-ray Microanalysis of Electron Beam-Sensitive Alloyed Nanoparticles

2008 ◽  
Vol 14 (2) ◽  
pp. 166-175 ◽  
Author(s):  
Nadi Braidy ◽  
Zygmunt J. Jakubek ◽  
Benoit Simard ◽  
Gianluigi A. Botton
Keyword(s):  
Electron Beam ◽  
Electron Microscope ◽  
Energy Dispersive ◽  
Laser Evaporation ◽  
Composition Series ◽  
Ag Nps ◽  
X Ray ◽  
Nanoscale Structures ◽  
Transmission Electron ◽  
20 Nm

An energy dispersive X-ray spectrometry (EDXS) method is developed to evaluate the composition of alloyed nanoparticles (NPs) where one of the alloying elements is removed under the electron beam during microanalysis with a transmission electron microscope (TEM). The method is demonstrated for alloyed Au-Ag NPs of a diameter ranging from 6 to 20 nm produced by laser evaporation of a water-suspended Ag-Au powder mixture of varying composition. Series of EDXS spectra are recorded for 30 NPs from samples with five different Ag:Au ratios revealing Ag depletion from NPs during electron irradiation. By studying the evolution of NPs composition as a function of dose, the initial Ag content for each NP is extrapolated. The rate of Ag depletion is discussed in terms of sputtering and knock-on damage. On average, approximately one Ag atom is lost from the NP for each Ag L X-ray detected. To assess the limitations of microanalysis in these sensitive nanoscale structures, the concept of detectability limit is adapted to our method. This benchmark is then evaluated for Ag in Au-Ag NPs of various sizes and acquisition times. This study should be regarded as a guide for the design of analytical TEM measurements of beam-sensitive NPs.

Aspects of microanalysis in a transmission electron microscope

1978 ◽  
Vol 36 (1) ◽  
pp. 510-511
Author(s):  
R. Sinclair ◽  
B.E. Jacobson
Keyword(s):  
Grain Size ◽  
Electron Beam ◽  
Electron Microscope ◽  
Chemical Analysis ◽  
Transmission Electron Microscope ◽  
Vapor Deposition ◽  
Critical Currents ◽  
X Ray ◽  
Fine Grain ◽  
Transmission Electron

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).

The Effect of Focused Ion Beam (Fib) Specimen Geometry on X-Ray Fluorescence During Energy Dispersive X-Ray Spectroscopy (EDS) Analysis in the Transmission Electron Microscope (TEM)

1998 ◽  
Vol 4 (S2) ◽  
pp. 856-857
Author(s):  
David M. Longo ◽  
James M. Howe ◽  
William C. Johnson
Keyword(s):  
Electron Microscope ◽  
Transmission Electron Microscope ◽  
Focused Ion Beam ◽  
Materials Science ◽  
Bulk Material ◽  
Ion Beam ◽  
Energy Dispersive ◽  
Specimen Preparation ◽  
X Ray ◽  
Transmission Electron

The focused ion beam (FIB) has become an indispensable tool for a variety of applications in materials science, including that of specimen preparation for the transmission electron microscope (TEM). Several FIB specimen preparation techniques have been developed, but some problems result when FIB specimens are analyzed in the TEM. One of these is X-ray fluorescence from bulk material surrounding the thin membrane in FIB-prepared samples. This paper reports on a new FIB specimen preparation method which was devised for the reduction of X-ray fluorescence during energy dispersive X-ray spectroscopy (EDS) in the TEM.Figure 1 shows three membrane geometries that were investigated in this study on a single-crystal Si substrate with a RF sputter-deposited 50 nm Ni film. Membrane 1 is the most commonly reported geometry in the literature, with an approximately 20 urn wide trench and a membrane having a single wedge with a 1.5° incline.

scholarly journals Cytotoxicity Property of Nano-TiO2Sol and Nano-TiO2Powder

2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
Pingting He ◽  
Jie Tao ◽  
Jianjun Xue ◽  
Yulan Chen
Keyword(s):  
Electron Microscope ◽  
Average Length ◽  
Synthesis Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structure And Morphology ◽  
Transmission Electron ◽  
Experimental Protocols ◽  
20 Nm

A homogeneous and transparent titania (TiO2) sol with nanosized anatase TiO2particles was prepared by hydrothermal synthesis method. The transmission electron microscope and X-ray diffraction were used to characterize the structure and morphology of particulates in the TiO2sol and purchased TiO2powder. The results show that the homogeneous anatase crystalline phase was formed and the size of the spindle-like particle in sol was about 20 nm in width and 150 nm in average length, and the particulates of the purchased powder were globular-like about 50 nm in diameter. In addition, a consistent set of in vitro experimental protocols was used to study the effects of nano-TiO2sol as prepared and nano-TiO2powder on mouse peritoneal macrophage. The cytotoxicity tests in vitro indicate that, with the increasing of TiO2sol concentration contaminated with the cells, the relative proliferation rate of macrophage cells was improved slightly after the cells contaminated for 24 h, but it reduced rapidly after contaminated for 48 h. The purchased nano-TiO2powder inhibited the growth of the cells obviously as cultivating with macrophage both for 24 h and 48 h.

X-ray Energy-Dispersive Spectrometry During In Situ Liquid Cell Studies Using an Analytical Electron Microscope

2014 ◽  
Vol 20 (2) ◽  
pp. 323-329 ◽  
Author(s):  
Nestor J. Zaluzec ◽  
M. Grace Burke ◽  
Sarah J. Haigh ◽  
Matthew A. Kulzick
Keyword(s):  
Electron Microscope ◽  
Analytical Electron Microscopy ◽  
Scanning Transmission Electron Microscope ◽  
Energy Dispersive ◽  
X Ray ◽  
Transmission Electron ◽  
Analytical Electron ◽  
Scanning Transmission ◽  
Liquid Cell

AbstractThe use of analytical spectroscopies during scanning/transmission electron microscope (S/TEM) investigations of micro- and nano-scale structures has become a routine technique in the arsenal of tools available to today’s materials researchers. Essential to implementation and successful application of spectroscopy to characterization is the integration of numerous technologies, which include electron optics, specimen holders, and associated detectors. While this combination has been achieved in many instrument configurations, the integration of X-ray energy-dispersive spectroscopy and in situ liquid environmental cells in the S/TEM has to date been elusive. In this work we present the successful incorporation/modifications to a system that achieves this functionality for analytical electron microscopy.

Electron beam-induced surface modification and nano-engineering of carbon nanotubes: Single-walled and multiwalled

2006 ◽  
Vol 21 (12) ◽  
pp. 3109-3123 ◽  
Author(s):  
S. Gupta ◽  
R.J. Patel ◽  
R.E. Giedd
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Raman Spectroscopy ◽  
Electron Beam ◽  
Electron Microscope ◽  
High Resolution ◽  
Band Intensity ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron

Influence of low and medium energy electron beam (E-beam) irradiation on the single-walled (SW) and multiwalled (MW) carbon nanotube films grown by microwave chemical vapor deposition are investigated. These films were subjected to electron beam energy of 50 keV from scanning electron microscope for 2.5, 5.5, 8.0, and 15 h and 100, 200, and 300 keV from transmission electron microscope electron gun for a few minutes to approximately 2 h continuously. To assess the surface modifications/structural degradation, the films were analyzed prior to and post-irradiation using x-ray diffraction and micro-Raman spectroscopy in addition to in situ monitoring by scanning and high-resolution transmission electron microscopy. A minimal increase in intertube or interplanar spacing (i.e., d002) for MW nanotubes ranging from 3.25–3.29 Å (∼3%) can be analogized to change in c-axis of graphite lattice due to thermal effects measured using x-ray diffraction. Resonance Raman spectroscopy revealed that irradiation generated defects in the lattice evaluated through variation of: the intensity of radial breathing mode (RBM), intensity ratio of D to G band (ID/IG), position of D and G bands and their harmonics (D* and G*). The increase in the defect-induced D band intensity, quenching of RBM intensity, and only a slight increase in G band intensity are some of the implications. The MW nanotubes tend to reach a state of saturation for prolonged exposures, while SW transforming semiconducting to quasi-metallic character. Softening of the q = 0 selection rule is suggested as a possible way to explain these results. It is also suggestive that knock-on collision may not be the primary cause of structural degradation, rather a local gradual reorganization, i.e., sp2+δ ⇔ sp2+δ, sp2 C seems quite possible. Experiments showed that with extended exposures, both kinds of nanotubes displayed various local structural instabilities including pinching, graphitization/amorphization, and forming intra-molecular junction (IMJ) within the area of electron beam focus possibly through amorphous carbon aggregates. They also displayed curling and closure forming nano-ring and helix-like structures while mending their dangling bonds. High-resolution transmission electron microscopy electrons corroborated these conclusions. Manufacturing of nanoscale structures “nano-engineering” of carbon-based systems is tentatively ascribed to irradiation-induced solid-state phase transformation, in contrast to conventional nanotube synthesis from the gas phase.

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