The electron probe microanalyzer (EPMA) provides quantitative analysis for nearly all chemical elements with a spatial resolution of analysis about ~1 μm, which is relevant to microstructures in a wide variety of materials and mineral specimens. Recent implementation of the Schottky emitter field-emission gun (FEG) electron source in the EPMA has significantly improved the spatial resolution and detectability of the EPMA technique.
An Sn-patch formed in Ni(V)-based under bump metallization during reflow and aging. To elucidate the evolution of the Sn-patch, the detailed compositions and microstructure in Sn–Ag–Cu and Ti/Ni(V)/Cu joints were analyzed by a field emission electron probe microanalyzer (EPMA) and transmission electron microscope (TEM), respectively. There existed a concentration redistribution in the Sn-patch, and its microstructure also varied with aging. The Sn-patch consisted of crystalline Ni and an amorphous Sn-rich phase after reflow, whereas V2Sn3 formed with amorphous an Sn-rich phase during aging. A possible formation mechanism of the Sn-patch was proposed.
Whereas the spatial resolution for standard secondary electron (SEI) imaging in a scanning electron microscope or electron probe microanalyzer is related to the incident probe diameter, the spatial resolution for x-ray microanalysis is related to the convolution of the probe diameter with the spatial extent of the analyzed volume for a point probe. The latter is determined by electron scattering in the specimen and the subsequent emission of excited x-rays from the specimen. As such, it is possible that “What you see is not what you get”. This is especially true for instruments with high brightness electron sources (field emission). This problem is compounded by probe aberrations which at Gaussian image focus can produce significant electron tails extending tens of microns from the center of the probe.
AbstractWe report the installation and performance evaluation of a probe aberration-corrected high-resolution JEOL JEM-ARM200F transmission electron microscope (TEM). We provide details on construction of the room that enables us to obtain scanning transmission electron microscope (STEM) data without any evident distortions/noise from the external environment. The microscope routinely delivers expected performance. We show that the highest STEM spatial resolution and energy resolution achieved with this microscope are 0.078 nm and 0.34 eV, respectively. We report a direct comparative evaluation of the performance of this microscope with a Schottky thermal field-emission gun versus a cold field-emission gun. Cold field-emission illumination improves spatial resolution of the high current probe for analytical spectroscopy, the TEM information limit, and the electron energy resolution compared to the Schottky thermal field-emission source.
There is increasing interest in X-ray microanalysis of thin specimens and the present paper attempts to define some of the factors which govern the spatial resolution of this type of microanalysis. One of these factors is the spreading of the electron probe as it is transmitted through the specimen. There will always be some beam-spreading with small electron probes, because of the inevitable beam divergence associated with small, high current probes; a lower limit to the spatial resolution is thus 2αst where 2αs is the beam divergence and t the specimen thickness.In addition there will of course be beam spreading caused by elastic and inelastic interaction between the electron beam and the specimen. The angle through which electrons are scattered by the various scattering processes can vary from zero to 180° and it is clearly a very complex calculation to determine the effective size of the beam as it propagates through the specimen.
X-ray microanalysis in the analytical electron microscope (AEM) refers to a technique by which chemical composition can be determined on spatial scales of less than 10 nm. There are many factors that influence the quality of x-ray microanalysis. The minimum probe size with sufficient current for microanalysis that can be generated determines the ultimate spatial resolution of each individual microanalysis. However, it is also necessary to collect efficiently the x-rays generated. Modern high brightness field emission gun equipped AEMs can now generate probes that are less than 1 nm in diameter with high probe currents. Improving the x-ray collection solid angle of the solid state energy dispersive spectrometer (EDS) results in more efficient collection of x-ray generated by the interaction of the electron probe with the specimen, thus reducing the minimum detectability limit. The combination of decreased interaction volume due to smaller electron probe size and the increased collection efficiency due to larger solid angle of x-ray collection should enhance our ability to study interfacial segregation.
Among the ultra-light elements B, C, N, and O nitrogen is the most difficult element to deal with in the electron probe microanalyzer. This is mainly caused by the severe absorption that N-Kα radiation suffers in carbon which is abundantly present in the detection system (lead-stearate crystal, carbonaceous counter window). As a result the peak-to-background ratios for N-Kα measured with a conventional lead-stearate crystal can attain values well below unity in many binary nitrides . An additional complication can be caused by the presence of interfering higher-order reflections from the metal partner in the nitride specimen; notorious examples are elements such as Zr and Nb. In nitrides containing these elements is is virtually impossible to carry out an accurate background subtraction which becomes increasingly important with lower and lower peak-to-background ratios. The use of a synthetic multilayer crystal such as W/Si (2d-spacing 59.8 Å) can bring significant improvements in terms of both higher peak count rates as well as a strong suppression of higher-order reflections.
Use of the Disk-of-least-confusion in X-ray Microanalysis