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578 CD DOI: 10.

1017/S1431927607071383

Microsc Microanal 13(Suppl 2), 2007 Copyright 2007 Microscopy Society of America

Advances in Energy Dispersive X-ray Spectrometry: The Impact of Silicon Drift Detectors (SDD) on the Characterization of Nanostructures and Nanomaterials
D. Newbury, J. H. Scott, N. Ritchie, D. Bright, and J. Small National Institute of Standards and Technology, Gaithersburg, MD 20899-8370 Developments in silicon drift detector (SDD) technology have resulted in a new class of energy dispersive x-ray spectrometers (EDS) with performance that is equal to or better than the classic Si(Li) EDS in nearly every measure of analytical performance except efficiency at high photon energy above 10 keV [1]. For a given detector active area, SDDs actually have better resolution than Si(Li), despite operating at about – 30 oC rather than requiring liquid nitrogen cooling (-190 o C) [2]. The SDD uses Peltier electronic cooling, and the exhaust heat is removed with a convection heat pipe and passive radiators so that there are no moving parts, thus eliminating a possible source of vibration that might compromise service on a high resolution microscope. For the critical issue of x-ray throughput (output count rate vs. input count rate, OCR vs. ICR), the SDD performance has improved so rapidly that recent technical articles have become obsolete within months of publication [3]. The single detector OCR peak is now above 250 kHz with a peaking time of 400 ns while achieving a resolution better than 131 eV (MnΚα), while a cluster of four such detectors with multiplexed signals exceeds 1 MHz OCR while retaining resolution below 140 eV. This extraordinary OCR vs. ICR performance makes it highly advantageous to collect x-ray data from heterogeneous structures by operating in the x-ray spectrum image (XSI) mode, where a complete x-ray spectrum is recorded at each discrete pixel. The resulting XSI databases can easily exceed 100 Mbytes with only 10 s total accumulation when the OCR is 1 MHz. Fortunately, software tools have been developed to efficiently mine these large databases, including tools that can detect and recover unexpected elements that occur only rarely in the spatial domain, down to the single pixel limit [4,5,6]. An example of elemental images recovered from an XSI (320 x 240 pixels) of electronic circuit structures recorded in only 10 seconds at an OCR of 900 kHz (three SDDs, 300 kHz per detector) is shown in Figure 1. Nanostructures and nanomaterials present a special challenge to elemental characterization by electron-excited x-ray spectrometry because their small size generally leads to a low x-ray emission rate. The rate of x-ray production depends on many factors, one of which is the spatial extent of the target object compared to the electron range. For materials in bulk form analyzed under “conventional” conditions (beam energy E0 > 10 keV), the electron range has dimensions of 1 µm or greater, depending on composition and beam energy. As the spatial dimensions of a synthetic structure or material are decreased below 1 µm, the x-ray production from a specific nanoscale feature scales approximately with the volume fraction of the feature compared to the bulk interaction volume. To improve the spatial resolution, “low voltage microanalysis”, for which E0 < 5 keV, reduces the interaction volume dimensions proportional to E01.67. However, the decrease in source brightness with E0 means that a nanometer-scale beam necessarily carries reduced beam current, reducing the x-ray production rate. Thus, the high OCR capabilities of the SDD are unlikely to be exploited in the analysis of nanostructures and nanomaterials. However, other attributes of SDD technology, such as the simplicity of cooling combined with large detector area, 50 mm2 or more, may enable new instrumentation configurations that can be more effective for the

. a new detector configuration might be possible that increases the solid angle of collection for x-rays and that observes the specimen from previously inaccessible locations. This is 10 second data! . 15 (1998) 11. 2007 579 CD analysis at the nanoscale. et al. Acta. http://www.Microsc Microanal 13(Suppl 2). Such a “look down” x-ray detector would permit microanalytical access to features located in holes that can be now be imaged with existing electron detectors. Newbury. Bright. et al. Lispix. [3] D. Element maps derived from XSI (320x240 pixels. Bright SCANNING. 27 (2005) 15. 27 (2005) 227. SCANNING. three 10 mm2 SDDs. Barkan. such as an annular “look down” detector placed near the electron beam to obtain a very high take-off angle [2]. Struder. [2] S. each operating at 300 kHz OCR (peaking time 220 ns). but which are currently inaccessible to x-ray microanalysis because of the relatively low take-off angles of existing EDS detector configurations.nist. such as the “through the lens secondary electron detector” of the high vacuum SEM and the “gaseous secondary electron detector” of the variable pressure/environmental SEMs. Microanal. References: [1] L. 130 µs dwell) E0 = 20 keV. [6] D. [5] D. 9 (2003) 1. Microscopy Today. (2004) 36. a pc-based image processing engine. Suppl. For example. Micros. [4] P. Mikrochim. Kotula et al. Newbury and D. 12.gov/lispix/ O Al Si Ti 10 µm Figure 1.