Achieving High Spatial Resolution in Elemental Mapping of Metal Samples from Archaeological Contexts

2002 ◽  
Vol 712 ◽  
Author(s):  
Scott Lea ◽  
Don Baer ◽  
Ernesto Paparazzo ◽  
Peter Northover ◽  
Chris Salter

ABSTRACTImproving the characterisation of archaeological artifacts brings a need to understand better the relationships between composition, structure and properties. With archaeological material there is also a requirement to consider the effects of ageing and environmental interactions in altering the original structure and composition, both in the bulk and at the surface. However, curatorial constraints and, frequently, the condition of the objects preclude the sampling methods required for the most powerful means of structural analysis of materials, the high resolution transmission electron microscope. The samples normally available are small bulk samples and we must find other means of maximising spatial resolution in microchemical and microstructural analysis of both bulk and surface regions of the samples. This paper describes ways in which this is being achieved using the scanning proton microprobe (SPM) with both particle induced X-ray emission (PIXE) and Rutherford back scattered proton (RBS) spectra at resolutions down to ca. 1:m, electron probe microanalysis (EPMA) at 250-300nm, and scanning Auger microscopy (SAM) at resolutions of 10-20nm, but only from the surface layers of atoms in a sample. Examples will be given which demonstrate the contribution that each instrument can make, and that new and useful information is obtained each time resolution is increased. They will also show that structural features can be identified which are invisible to other microscopies. It will also be shown how modern PC-based software has greatly enhanced the mapping capability of all instruments.

1999 ◽  
Vol 577 ◽  
Author(s):  
John Henry J. Scott

ABSTRACTThe fabrication of nanoscale magnetic materials and novel heterostructures has placed great demands on the analytical tools used to characterize the chemical and structural variations in these samples. Attempts to determine the composition, phase, crystallinity, and interface structure of nanoscale materials often involve tradeoffs between accuracy, sensitivity, and spatial resolution. Traditional techniques such as electron energy-loss spectroscopy (EELS), energy dispersive x-ray spectrometry (EDS), secondary ion mass spectrometry (SIMS), and scanning Auger microscopy (SAM) will be surveyed in this context. Powerful new tools for probing the chemical heterogeneity of materials at ultrafine length scales will also be discussed, including energy-filtered transmission electron microscopy (EFTEM) and spectrum imaging, as well as recent advances in new methods such as backscattered electron Kikuchi patterns (BEKP) and microcalorimetry.


Author(s):  
C. M. Jantzen ◽  
D. G. Howitt

The mullite-SiO2 liquidus has been extensively studied, and it has been shown that the flattening of the liquidus is related to the existence of a metastable region of liquid immiscibility at sub-liquidus temperatures which is detectable by transmission electron microscopy (TEM) (Fig. 1).


Author(s):  
H. Weiland ◽  
D. P. Field

Recent advances in the automatic indexing of backscatter Kikuchi diffraction patterns on the scanning electron microscope (SEM) has resulted in the development of a new type of microscopy. The ability to obtain statistically relevant information on the spatial distribution of crystallite orientations is giving rise to new insight into polycrystalline microstructures and their relation to materials properties. A limitation of the technique in the SEM is that the spatial resolution of the measurement is restricted by the relatively large size of the electron beam in relation to various microstructural features. Typically the spatial resolution in the SEM is limited to about half a micron or greater. Heavily worked structures exhibit microstructural features much finer than this and require resolution on the order of nanometers for accurate characterization. Transmission electron microscope (TEM) techniques offer sufficient resolution to investigate heavily worked crystalline materials.Crystal lattice orientation determination from Kikuchi diffraction patterns in the TEM (Figure 1) requires knowledge of the relative positions of at least three non-parallel Kikuchi line pairs in relation to the crystallite and the electron beam.


2015 ◽  
Author(s):  
Ludmila L. Meisner ◽  
Alexey A. Neiman ◽  
Alexander I. Lotkov ◽  
Nikolai N. Koval ◽  
Viktor O. Semin ◽  
...  

1990 ◽  
Vol 110 (4) ◽  
pp. 883-894 ◽  
Author(s):  
R Reichelt ◽  
A Holzenburg ◽  
E L Buhle ◽  
M Jarnik ◽  
A Engel ◽  
...  

Nuclear pore complexes (NPCs) prepared from Xenopus laevis oocyte nuclear envelopes were studied in "intact" form (i.e., unexposed to detergent) and after detergent treatment by a combination of conventional transmission electron microscopy (CTEM) and quantitative scanning transmission electron microscopy (STEM). In correlation-averaged CTEM pictures of negatively stained intact NPCs and of distinct NPC components (i.e., "rings," "spoke" complexes, and "plug-spoke" complexes), several fine structural features arranged with octagonal symmetry about a central axis could reproducibly be identified. STEM micrographs of unstained/freeze-dried intact NPCs as well as of their components yielded comparable but less distinct features. Mass determination by STEM revealed the following molecular masses: intact NPC with plug, 124 +/- 11 MD; intact NPC without plug, 112 +/- 11 MD; heavy ring, 32 +/- 5 MD; light ring, 21 +/- 4 MD; plug-spoke complex, 66 +/- 8 MD; and spoke complex, 52 +/- 3 MD. Based on these combined CTEM and STEM data, a three-dimensional model of the NPC exhibiting eightfold centrosymmetry about an axis perpendicular to the plane of the nuclear envelope but asymmetric along this axis is proposed. This structural polarity of the NPC across the nuclear envelope is in accord with its well-documented functional polarity facilitating mediated nucleocytoplasmic exchange of molecules and particles.


2012 ◽  
Vol 730-732 ◽  
pp. 715-720
Author(s):  
Telmo G. Santos ◽  
João Faria ◽  
Pedro Vilaça ◽  
R.M. Miranda

Eddy currents are based on electromagnetic induction and analysis of electrical currents on conductive materials. This method is used for thickness measurements, corrosion and defects detection, electrical conductivity and magnetic permeability measurements. Recently, it has been exploited as a materials characterization technique, namely in solid state welding, since, compared to hardness, it is based in distinct physical phenomena. Electrical conductivity is controlled by electronic mobility, while hardness depends on crystal defects and thus a scale factor exists. This paper presents results of this characterization technique applied to multipass solid state friction stir processing (FSP) of AA1100 alloy. These results were compared to microstructural analysis and hardness measurements and show that eddy current is a feasibly, reliable and expedite technique to characterize processed materials. The electrical conductivity measured by eddy currents, maps more precisely structural features, while hardness does not. Measurement of electrical conductivity field suggests having potential to constitute an alternative and/or complement to hardness evaluation with the further advantage of being a non-destructive method.


2013 ◽  
Vol 19 (5) ◽  
pp. 1159-1169 ◽  
Author(s):  
Carla Silva ◽  
Joao Perdigao ◽  
Elsa Alverca ◽  
António P. Alves de Matos ◽  
Patricia A. Carvalho ◽  
...  

AbstractTuberculosis (TB) is a major health problem. The emergence of multidrug resistant (MDR)Mycobacterium tuberculosis(Mtb) isolates confounds treatment strategies. In Portugal, cases of MDR-TB are reported annually with an increased incidence noted in Lisbon. The majority of these MDR-TB cases are due to closely related mycobacteria known collectively as theLisboafamily and Q1 cluster. Genetic determinants linked to drug resistance have been exhaustively studied resulting in the identification of family and cluster specific mutations. Nevertheless, little is known about other factors involved in development of mycobacteria drug resistance. Here, we complement genetic analysis with the study of morphological and structural features of theLisboafamily and Q1 cluster isolates by using scanning and transmission electron microscopy. This analysis allowed the identification of structural differences, such as cell envelope thickness, between Mtb clinical isolates that are correlated with antibiotic resistance. The infection of human monocyte derived macrophages allowed us to document the relative selective advantage of theLisboafamily isolates over other circulating Mtb isolates.


2003 ◽  
Vol 36 (6) ◽  
pp. 1319-1323 ◽  
Author(s):  
A. Morawiec

A method that improves the accuracy of misorientations determined from Kikuchi patterns is described. It is based on the fact that some parameters of a misorientation calculated from two orientations are more accurate than other parameters. A procedure which eliminates inaccurate elements is devised. It requires at least two foil inclinations. The quality of the approach relies on the possibility to set large sample-to-detector distances and the availability of good spatial resolution of transmission electron microscopy. Achievable accuracy is one order of magnitude better than the accuracy of the standard procedure.


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