We have been developing superconducting tunnel junctions (STJs) for use as high-resolution energy dispersive spectrometers. STJ detectors simultaneously offer energy resolution better than 15 eV at 1 keV, count rates in excess of 10,000 counts per second, broad bandwidth and high efficiency. These attributes make them desirable detectors in a variety of applications, including x-ray microanalysis.When an x-ray photon is absorbed in a superconductor, about 60% of its energy is used to break the Cooper pairs that make up the superconducting ground state into excited electron-like and hole-like states called quasiparticles. This process is analogous to the creation of electron-hole pairs in a conventional energy dispersive spectrometer (EDS) based on silicon or germanium. The difference is that the superconducting energy gap Δ is on the order of a few millielectron volts, roughly a factor of 1000 less than the band gap in common semiconductors.
Instruments combining a 100 kV transmission electron microscope (TEM) with scanning transmission (STEM), secondary electron (SEM) and x-ray energy dispersive spectrometer (EDS) attachments to give analytical capabilities are becoming increasingly available and useful. Some typical applications in the field of materials science which make use of the small probe size and thin specimen geometry are the chemical analysis of small precipitates contained within a thin foil and the measurement of chemical concentration profiles near microstructural features such as grain boundaries, point defect clusters, dislocations, or precipitates. Quantitative x-ray analysis of bulk samples using EDS on a conventional SEM is reasonably well established, but much less work has been performed on thin metal foils using the higher accelerating voltages available in TEM based instruments.
ABSTRACTCu(90 nm)/Ti(20 nm) bilayers and Cu(Ti 27 at.%) alloy films were deposited on SiO2 and annealed in an NH3 ambient at temperatures 400–700° C for 30 min. During annealing Ti segregated to both the free surface and the alloy/SiO2 interface. At the surface Ti reacted with NH3 to form TiN, whereas at the interface the Ti reacted with the SiO2 to form a TiO/Ti5Si3 structure. High resolution energy dispersive x-ray analysis revealed the presence of interfacial Cu between the Ti-silicide and Ti-oxide layers at temperatures greater than 450°C. Using Cu-Ti alloy films enhanced the Si02 consumption rate by a factor of 3-4 compared to that of pure Ti. It is suggested that the interfacial Cu is responsible for the increased rate. It is plausible that an interfacial Cu2O component has a catalytic effect on the Ti- SiO2 reaction.
A new correction method for high-resolution energy-dispersive x-ray analyses in the environmental scanning electron microscope