We evaluated factors affected the accuracy and precision of quantitating trace concentration of Ca with electron energy loss spectroscopy (EELS). These factors include internal reflection in the spectrometer, precision of correlation between standards and experimental spectra, and radiation damage-induced spectral changes. We present methods of correcting for these effects and improving the reliability of trace Ca quantitation. A two-step fitting procedure is described that improves the retrieval of small Ca signals from the large background common to biological specimens. After optimizing the experimental conditions and data processing procedures, our current system can detect about 2.2 mmol/kg Ca in a 730-Å thick specimen at a total dose of about 410 nA . sec at 95% confidence level by fitting the first difference spectra. Because of the 0.1% residual gain variation after gain normalization, the first difference spectrum fitting is still the preferred method for trace Ca quantitation. Our study also demonstrates the clear advantage of using a 200 keV system, instead of 120 keV or lower accelerating voltages, for EELS analysis of relatively thick biological cryosections.

We have fabricated amorphous thin-film specimens containing light elements (B, C, N, O, F, and Mg) in addition to silicon, and have measured their composition using electron energy-loss spectroscopy (EELS). The films appear to be stable during storage in air and during irradiation by an electron beam, for doses below 105 C/cm2. Used with a transmission electron microscope fitted with an energy-dispersive X-ray (EDX) detector, they provide a convenient means of determining light-element k-factors for X-ray microanalysis. For a TEM equipped with an electron energy-loss spectrometer, the specimens can also be used to check the EELS instrumentation and elemental-quantification procedures.

Materials science requires the use of increasingly powerful tools in materials analysis. The last 20 years have witnessed the development of a number of analytical techniques. However, among these techniques, only a few allow observation and analysis of materials at the nanometer level. The tomographic atom probe (TAP) is a three-dimensional atom-probe (3-DAP) developed at the University of Rouen. In this instrument, the specimen is field evaporated, atomic layer by atomic layer, and the use of a position-sensing system makes it possible to map out the chemical identity of individual atoms within each field-evaporated layer on a nearly atomic scale. After analysis, the volume of matter removed from the specimen can be reconstructed atom by atom in the three dimensions of real space. The main advantages of the 3-DAP is its single-atom sensitivity and very high spatial resolution. In addition to 3-D visual information on chemical heterogeneity, 3-D images give an accurate measurement of the composition of any feature without any convolution bias. This study first describes the history of the 3-DAP technique. Its main features and the latest developments of the TAP are then detailed. The performance of this instrument is illustrated through two recent applications in materials science. Possible ways to further improve the technique are also discussed.

Determining the three-dimensional atomic structure of grain boundaries is a crucial first step toward understanding how these defects control the overall bulk properties of materials. In this report we discuss the correlation of experimental atomic resolution Z-contrast images and electron energy loss spectrometry (EELS) to achieve this goal. Initial structural analysis is afforded through empirical bond-valence potentials. This structure is then refined using multiple scattering analysis of the energy loss spectra. These techniques are demonstrated in the analysis of a 27° MgO [001] tilt grain boundary. Through this analysis, we were able to determine specific atomic locations of Ca dopants found present at this grain boundary.

X-ray cone-beam reconstruction from incomplete projection data has important practical applications, especially in microtomography. We developed expectation maximization (EM)-type and algebraic reconstruction technique (ART)-type iterative cone-beam reconstruction algorithms for metal artifact reduction and local reconstruction from truncated data. These iterative algorithms are adapted from the emission computerized tomography (CT) EM formula and the ART. A key step in our iterative algorithms is introduction of a projection mask and computation of a 3-D spatially varying relaxation factor that allows compensation for beam divergence and data incompleteness. The algorithms are simulated with projection data synthesized from mathematical phantoms. In simulation, the EM-type and ART-type iterative algorithms are demonstrated to be effective for metal artifact reduction and local region reconstruction. They perform similarly in terms of visual quality, image noise, and discrepancy between measured and reprojected data. The EM-type and ARTtype iterative cone-beam reconstruction algorithms have potential for metal artifact reduction and local region reconstruction in X-ray CT.