Low-voltage microscopy and position-tagged spectrometry of ceramic microstructures

Author(s):  
J. J Friel ◽  
V. A. Greenhut

Ceramic microstructures are ideally suited for low-voltage field emission microscopy on uncoated samples. Most elements of interest in ceramics have useful X-ray lines below 5 keV, thus permitting the use of accelerating voltages between 3 and 8 kV. One analytical consequence of the use of low voltage is a reduced interaction volume with the electron beam, so that X-ray maps can be collected at submicrometer resolution. To produce usable maps at low voltage, the SEM must be capable of sufficient beam current, and the X-ray detector geometry must be optimal. Another way to optimize X-ray microanalysis is to collect an entire spectrum at every point in the microstructure even at high resolution. Although this capability would permit an X-ray spectrum to be displayed from one pixel, a much more productive approach is to create a spectrum based on all pixels of a particular phase.

1998 ◽  
Vol 4 (S2) ◽  
pp. 190-191
Author(s):  
Patrick Echlin

Although high resolution (2nm), low voltage (lkV), SEM of bio-organic materials can now be performed more or less routinely using instruments fitted with a field emission source, virtually no low voltage x-ray microanalysis has been carried out on this type of specimen. Boyes and Nockolds showed that quantitative microanalytical information could be obtained from polished inorganic samples at a spatial resolution of l00nm at 5kV and Johnson et al obtained similar type of data at a spatial resolution of 150nm at 3kV. High spatial resolution (l0nm) microanalysis can be achieved in frozen dried or chemically compromised sections of biological material examined at high voltage in the TEM but frozen hydrated chemically unfixed sections are damaged. The other approach is to use the SEM with frozen hydrated, chemically uncompromised samples, usually at about 10-15kV, in order to obtain sufficient signal from the elements of interest which typically lie in the range Na (Z=l 1) to Ca (Z=20).


Author(s):  
W.W. Adams ◽  
D.L. Vezie

Low-voltage, high-resolution (LVHR) scanning electron microscopy (SEM) of polymers is becoming more widespread as the new LVHRSEMs become more available to the general microscopy public. Although low-voltage SEM has been known for many years, the availability of new high-resolution microscopes with high-brightness field emission electron guns (FEG) and lens systems optimized for lower operating voltages (especially the immersion lens designs) has revolutionized the field of polymer surface morphology. The adequate beam current and excellent resolution at low voltages (4.0 nm at 1.0 keV) results in a dramatic improvement in image contrast at low voltages due to reduced beam spread and smaller interaction volume. In addition, imaging can be performed near the E2 crossover voltage, which means there is little or no sample charging, necessitating little or no sample coating with conducting metals or carbon, thus simplifying sample preparation.


Author(s):  
T. Miyokawa ◽  
S. Norioka ◽  
S. Goto

Field emission SEMs (FE-SEMs) are becoming popular due to their high resolution needs. In the field of semiconductor product, it is demanded to use the low accelerating voltage FE-SEM to avoid the electron irradiation damage and the electron charging up on samples. However the accelerating voltage of usual SEM with FE-gun is limited until 1 kV, which is not enough small for the present demands, because the virtual source goes far from the tip in lower accelerating voltages. This virtual source position depends on the shape of the electrostatic lens. So, we investigated several types of electrostatic lenses to be applicable to the lower accelerating voltage. In the result, it is found a field emission gun with a conical anode is effectively applied for a wide range of low accelerating voltages.A field emission gun usually consists of a field emission tip (cold cathode) and the Butler type electrostatic lens.


Author(s):  
David Joy ◽  
James Pawley

The scanning electron microscope (SEM) builds up an image by sampling contiguous sub-volumes near the surface of the specimen. A fine electron beam selectively excites each sub-volume and then the intensity of some resulting signal is measured. The spatial resolution of images made using such a process is limited by at least three factors. Two of these determine the size of the interaction volume: the size of the electron probe and the extent to which detectable signal is excited from locations remote from the beam impact point. A third limitation emerges from the fact that the probing beam is composed of a finite number of discrete particles and therefore that the accuracy with which any detectable signal can be measured is limited by Poisson statistics applied to this number (or to the number of events actually detected if this is smaller).


Author(s):  
Matthew T. Johnson ◽  
Ian M. Anderson ◽  
Jim Bentley ◽  
C. Barry Carter

Energy-dispersive X-ray spectrometry (EDS) performed at low (≤ 5 kV) accelerating voltages in the SEM has the potential for providing quantitative microanalytical information with a spatial resolution of ∼100 nm. In the present work, EDS analyses were performed on magnesium ferrite spinel [(MgxFe1−x)Fe2O4] dendrites embedded in a MgO matrix, as shown in Fig. 1. spatial resolution of X-ray microanalysis at conventional accelerating voltages is insufficient for the quantitative analysis of these dendrites, which have widths of the order of a few hundred nanometers, without deconvolution of contributions from the MgO matrix. However, Monte Carlo simulations indicate that the interaction volume for MgFe2O4 is ∼150 nm at 3 kV accelerating voltage and therefore sufficient to analyze the dendrites without matrix contributions.Single-crystal {001}-oriented MgO was reacted with hematite (Fe2O3) powder for 6 h at 1450°C in air and furnace cooled. The specimen was then cleaved to expose a clean cross-section suitable for microanalysis.


Author(s):  
Y. Sato ◽  
T. Hashimoto ◽  
M. Ichihashi ◽  
Y. Ueki ◽  
K. Hirose ◽  
...  

Analytical TEMs have two variations in x-ray detector geometry, high and low angle take off. The high take off angle is advantageous for accuracy of quantitative analysis, because the x rays are less absorbed when they go through the sample. The low take off angle geometry enables better sensitivity because of larger detector solid angle.Hitachi HF-2000 cold field emission TEM has two versions; high angle take off and low angle take off. The former allows an energy dispersive x-ray detector above the objective lens. The latter allows the detector beside the objective lens. The x-ray take off angle is 68° for the high take off angle with the specimen held at right angles to the beam, and 22° for the low angle take off. The solid angle is 0.037 sr for the high angle take off, and 0.12 sr for the low angle take off, using a 30 mm2 detector.


Author(s):  
W.W. Adams ◽  
G. Price ◽  
A. Krause

It has been shown that there are numerous advantages in imaging both coated and uncoated polymers in scanning electron microscopy (SEM) at low voltages (LV) from 0.5 to 2.0 keV compared to imaging at conventional voltages of 10 to 20 keV. The disadvantages of LVSEM of degraded resolution and decreased beam current have been overcome with the new generation of field emission gun SEMs. In imaging metal coated polymers in LVSEM beam damage is reduced, contrast is improved, and charging from irregularly shaped features (which may be unevenly coated) is reduced or eliminated. Imaging uncoated polymers in LVSEM allows direct observation of the surface with little or no charging and with no alterations of surface features from the metal coating process required for higher voltage imaging. This is particularly important for high resolution (HR) studies of polymers where it is desired to image features 1 to 10 nm in size. Metal sputter coating techniques produce a 10 - 20 nm film that has its own texture which can obscure topographical features of the original polymer surface. In examining thin, uncoated insulating samples on a conducting substrate at low voltages the effect of sample-beam interactions on image formation and resolution will differ significantly from the effect at higher accelerating voltages. We discuss here sample-beam interactions in single crystals on conducting substrates at low voltages and also present the first results on HRSEM of single crystal morphologies which show some of these effects.


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