Microbeam and Nanobeam Analysis PDF
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~ ~ I I I I I I I I I Microbeam and Nanobeam Analysis Edited by D. Benoit, J.-F. Bresse, L. Van't dack, H. Werner, J. Wernisch Mikrochimica Acta Supplement 13 Springer-Verlag Wien GmbH Dr. Daniele Benoit Beauchamp, France Dr. Jean-Francois Bresse Department PAP/CDP/CMT, C.N.E.T. France Telecom Bagneux, France Luc Van't dack Department of Chemistry, University of Antwerp (UlA), Antwerp-Wilri jk, Belgium Univ.-Prof. Dr. Helmut Wemer Waalre, The Netherlands Univ.-Doz. Dr. Johann Wemisch Institut fiir angewandte und technische Physik, Technische Universităt, Wien, Austria This work is subject to copyright. Ali rights are reserved, whether the whole or part of the material is concemed, specifically those of translation, reprinting, re-use of illustrations, broadcasting, reproduction by photocopying machine or similar means, and storage in data banks. © 1996 Springer-Verlag Wien Originally published by Springer-Verlag/Wien in 1996 Product Liability: The publisher can give no guarantee for information about drug dosage and appli cation thereof contained in this book. In every individual case the respective user must check its accuracy by consulting other pharmaceuticalliterature. The use of registered names, trademarks, etc. in this publication does not imply, even in the absence of a specific statement, that such names are exempt from the relevant protective laws and regulations and therefore free for general use. Typesetting: Thomson Press, New Delhi, India Graphic design: Ecke Bonk Printed on acid-free and chlorine free bleached paper. With 394 partly coloured Figures Die Deutsche Bibliothek -CIP-Einheitsaufnahme Microbeam and nanobeam analysis / D. Benoit ... (ed.). -Wien ; New York: Springer, 1996 (Mikrochimica acta : Supplementum ; 13) ISBN 978-3-211-82874-8 ISBN 978-3-7091-6555-3 (eBook) DOI 10.1007/978-3-7091-6555-3 NE: Benoit, Daniele [Hrsg.]; Mikrochimica acta / Supplementum ISSN 0026-3672 ISBN 978-3-211-82874-8 Preface This supplement of Mikrochimica Acta contains selected papers from the Fourth Workshop of the European Microanalysis Society (EMAS) on "Modern Develop ments and Applications in Microbeam Analysis" which took place in May 1995 in Saint Malo (France). EMAS was founded in 1986 by members from almost all european countries in order to stimulate research, applications and development of all forms of microbeam methods. One important EMAS activity is the organisation of biennial workshops for demonstrating the current status and developing trends of microanalytical techniques. For this meeting, EMAS chose to highlight the following topics: Monte-Carlo simula tions, transport calculations and use of soft X-rays for electron probe microanalysis (EPMA), dynamic secondary ion mass spectrometry (SIMS), detection of small quan tities using different techniques: synchrotron radiation X-ray fluorescence, particle in duced X-ray emission (PIXE), cathodoluminescence microscopy (CL). Two new kinds of instrumental techniques were also presented: atomic probe and scanning probe microscopy (STM). The aim of the conference is to give introductory lectures corresponding to the topics of the meeting and to have contributions in the form of po ster sessions. More than 80 posters were presented. Most of them gave a short oral pre sentation. The poster subjects were related to the use of microanalytical techniques: EPMA with wavelength dispersive spectrometry (WDS) and energy dispersive spec trometry (EDS), Auger electron spectrometry (AES), secondary ion mass spectro metry (SIMS), scanning electron microscopy and other topographical methods like scanning tunneling microscopy (STM) or atomic force microscopy (AFM). The field of applications is very broad: metallurgy, mineralogy, semiconductor, ceramic, glass, composite, polymer and biological material. The authors originate from almost all european countries, including eastern euro pean ones and Russia. One invited lecture was given by a USA speaker. This issue contains the full texts of the ten introductory lectures and 50 brief arti cles. These articles are the condensed scientific informations of the poster sessions. They were subjected to peer-review according to the usual procedure and some of them were rejected. Proceedings of previous EMAS workshops were also published, either as a sup plement to or in a regular issue of Mikrochimica Acta. We hope that these contributi ons to the field of microbeam techniques will be found to be useful. September 1996 The Editors Contents Invited Speakers Monte Carlo Simulation Techniques for Quantitative X-Ray Microanalysis L. Reimer ................................ 1 Transport Equation Approach to Electron Microbeam Analysis: Fundamentals and Applications W S. M. Werner. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 13 Use of Soft X-Rays in Microanalysis J.-L. Pouchou ......... . 39 Intensity Measurement of Wavelength Dispersive X-Ray Emission Bands: Ap plications to the Soft X-Ray Region G. Remond, C. Gilles, M. Fialin, O. Rouer, R. Marinenko, R. Myklebust, D. Newbury . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. 61 Synchrotron Radiation Induced X-ray Microfluorescence Analysis K. Janssens, L. Vincze, B. Vekemans, A. Aerts, F. Adams, K. W Jones, A. KnOchel . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87 Particle-Induced X-Ray Emission - A Quantitative Technique Suitable for Microanalysis K. G. Malmqvist. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117 Cathodoluminescence Microscopy and Spectroscopy of Semiconductors and Wide Bandgap Insulating Materials J. F. Bresse, G. Remond, B. Akamatsu . . . . . . . . . . . . . . . . . . . . 135 Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) P. Bertrand, L.-T. Weng . . . . . . . . . . . . . . . . . . . . . . . . 167 Three-Dimensional Nanoanalysis with the Tomographic Atom-Probe D. Blavette, A. Bigot, C. Schmuck, F. Danoix, P. Auger .......... 183 Microanalysis at Atomic Resolution S. J. Pennycook, D. E. Jesson, N. D. Browning, M. F. Chisholm ...... 195 Contributed Papers Composition of Vanadium Carbides Formed by Solidification in Fe-V-C-M Alloys: Influence of Additions (M = AI, Cu, Mo) L. Adnane, R. Kesri, S. Hamar-Thibault .................. 209 VIII Contents Electron Transmission Coefficient for Oblique Angle of Incidence M. Andrae, P. Klein, K. Rohrbacher, J. Wernisch .... . . . . . . . 217 Depth Distribution Function for Oblique Angle of Incidence M. Andrae, K. Rohrbacher, P. Klein, J. Wernisch . . . . . . . . . . 225 Simulation of EDS Spectra Using X-RES Software M. Aouine, C. Esnouf, T. Epicier ...... . 233 On the Use of the GeLa Line in Thin Film X-Ray Microanalysis of Si1_x Gex lSi Heterostructures A. Armigliato, T. Lews, R. Rosa. . . . . . . . . . . . . . . . . . . . . . . . 241 Computer Simulations ofthe X-Ray Intensity Distribution from Submicron Par ticles Embedded in a Matrix A. Berner, I. Levin .............................. 251 Determination of Rare Earth Elements in Biological and Mineral Apatite by EPMA and LAMP-ICP-MS S. Chenery, T. Williams, T. A. Elliott, P. L. Forey, L. Werdelin . . . . . . 259 Quantitative Analysis of the Compound Layer of Plasma Nitrided Pure Iron J. D'Haen, M. D'Olieslaeger, L. De Schepper, L. M. Stals. . . . . . . . . . 271 Correction of the Edge Effect in Auger Electron Microscopy L. Frank, F. Matejka. . . . . . . . . . . . . . . . .. .......... 279 Low Energy Imaging of N onconductive Surfaces in SEM L. Frank, M. ZadraZil, I. Miillerova. . . . . . . . . . 289 Investigation of the Bonding Mechanism of Glass Ceramic Layers on Metal Alloys M. Frigge, G. Volksch . . . . . . . . . . . . . . . . . . . . . . . . . .. 299 Monte Carlo Method for Quantitative Analysis of Bulk and Layered Samples O. Gedeon, V. Hui(nskj, K. Jurek, M. Simeekova ............. 307 SIMS Linescan Profiling of Chemically Bevelled Semiconductors: a Method of Overcoming Ion Beam Induced Segregation in Depth Profiling c.-M. Hsu, D. S. McPhail .......................... 317 Experimental Verification of Theoretical Models Simulating the Temperature Increase in EPMA of Glass V. Hui(nskj, K. Jurek, O. Gedeon ...................... 325 Quantitation of Mineral Elements of Different Fruit Pollen Grains M. J. Bucsek, J. Nytki, Z. Szabo, A. Kadar. . . . . . . . . . . . . . . . . . 333 Electron Beam Induced Migration of Alkaline Ions in Silica Glass K. Jurek, V. Hui(nskj, O. Gedeon .............. . 339 Application of the Boltzmann Transport Equation in the Thickness Determination of Thin Films G. Kaltsas, N. Glezos, E. Valamontes, A. G. Nassiopoulos. . . . . . . . . . 349 Contents IX Characterisation of the Shape of Microparticles via Fractal and Fourier Analyses of Scanning Electron Microscope Images V. V. Kindratenko, P. J. M. Van Espen, B. A. Treiger, R. E. Van Grieken 355 Calculation ofthe Surface Ionisation Using Analytical Models of Electron Back scattering P. Klein, M. Andrae, K. Rohrbacher, J. Wernisch 363 Thickness Determination of Thin Insulating Layers P. Klein, K. Rohrbacher, M. Andrae, J. Wernisch 377 High Energy and Angular Resolution Dynamic Secondary Ion Mass Spectro metry A. A. Kosyachkov 391 EPMA and Mass Spectrometry of Soil and Grass Containing Radioactivity from the Nuclear Accident at Chernobyl 0. Lejevre, M. Betti, L. Koch, C. T. Walker. . . . . . . . . . . . . . . . . . 399 Application of a New Monte Carlo Simulation Algorithm to Electron Probe Microanalysis X. Llovet, A. Riveros, F. Salvat . . . . . . . . . . 409 Topography Development on Single Crystal MgO Under Ion Beam Bom- bardment N. J. Montgomery, D. S. McPhail ........ 419 Determination of SPM TIP Shape Using Polystyrene Latex Balls P. Nagy, G. 1. Mark, E. Baldzs . . . . . . . . . . . . . . .. ....... 425 Combined Characterization of Nanostructures by AEM and STM V. P. Oleshko, R. H. Gijbels, W A. Jacob, M. V. Alfimov 435 Study of Quasi-Fractal Many-Particle-Systems and Percolation Networks by Zero-Loss Spectroscopic Imaging, Electron Energy-Loss Spectroscopy and Digital Image Analysis V. P. Oleshko, V. V. Kindratenko, R. H. Gijbels, P. J. M. Van Espen, W A. Jacob 443 Calculation of Bremsstrahlung Spectra for Multilayer Samples A. Pfeiffer, C. Schiebl, J. Wernisch . . . . . . . . . . . . . 453 Thickness Measurement of Thin Films by EPMA - Influence of ¢(O), MAC's and Substrate P. Polt, B. StOckl. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 463 A Simple Procedure to Check the Spectral Response of an EDX Detector M. Pro cop .................................. 473 Virtual WDS S. J. B. Reed, A. Buckley 479 Monte Carlo Simulation Program with a Free Configuration of Specimen and Detector Geometries L. Reimer, M. Kiissens, L. Wiese 485 X Contents Barriers to Energy Dispersive Spectrometry with Low Energy X-Rays D. G. Rickerby . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 493 Measurements of Gal_xAlxAs Layers on GaAs with EDS K. Rohrbacher, P. Klein, M. Andrae, 1. Wernisch .. 501 The Relative Intensity Factor for La Radiation Considering the Different Mass Absorption of La and Lf3 Radiation K. Rohrbacher, M. Andrae, P. Klein, 1. Wernisch .............. 507 Determination of the Solubility of Cerium in BaTi0 by Quantitative WDS Elec 3 tron Probe Microanalysis Z. Samardiija, M. Ceh, D. Makovec, D. Kolar. . . . . . . . . . . . . 517 Simulation of X-Ray Diffraction Profiles of Gradually Relaxed Epilayers A. Sanz-Hervas, E. 1. Abril, M. Aguilar, G. de Benito, C. Llorente, M. Lopez .................................... 525 Monte Carlo Simulation of Electron Scattering for Arbitrary 2D Structures Using a Modified Quadtree Geometry Discretization C. 0. Schiebl, A. Pfeiffer, H. W Wagner, W s. M. Werner, H. Stippel 533 Chemical-Bond Characterization of Nanostructures by EELS R. Schneider, 1. Woltersdorf, A. Roder . . . . . . . . . . 545 Local Determination of Carbon by Combining Beta-Autoradiography and Elec tron Microprobe Analysis V. G. Sen in, S. N. Shilobreeva ........................ 553 The Check of the Elastic Scattering Model in Monte-Carlo Simulation V. Stary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. .... 559 True Colour X-Ray Vision for Electron Microscopy and Microanalysis P. 1. Statham. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 573 Determination of the Oxidation States of Nb by Auger Electron Spectroscopy Z. Tass, G. Horvath. . . . . . . . . . . . . . . . . . . . . . . . . . .. . 581 Study by SIMS of the 54Cr and 180 Diffusion in Cr2 0 3 and in Cr203 Scales S. C. Tsai, A. M. Huntz, C. Dolin, C. Monty .............. 587 Comparison of Back- Foil Scanning X -Ray Microftuorescence and Electron Probe X-Ray Microanalysis for the Elemental Characterisation of Thin Coatings E. Valamontes, A. G. Nassiopoulos. . . . . . . . . . . . . . . . . . . . . . 597 Electron Probe X-Ray Microanalysis of Coatings E. Valamontes, A. G. Nassiopoulos. . . . . . 605 Analysis of Layers: X-Ray Maps of Change in Thickness Obtained by Electron Macroprobe D. Viale, G. Petitgand ............................ 611 Comparison of Simulated and Experimental Auger Intensities of Au, Pt, Ni and Si in Absolute Units H. W Wagner, C. O. Schiebl, W S. M. Werner . . . . . . . . . . . . . . . . 623 Practical Aspects and Applications of EPMA at Low Electron Energies P Willich, R. Bethke. . . . . . . . . . . . . . . . . . . . . . . .. .... 631 Oxidation and Reduction Processes of Be/BeO Induced by Electrons P Zanel, H. Hammer ............................ 639 Listed in Current Contents Mikrochim. Acta [Supp!.] 13, 1-12 (1996) © Springer-Verlag 1996 Monte Carlo Simulation Techniques for Quantitative X-Ray Microanalysis Ludwig Reimer Physikalisches Institut, Universitat Munster, Wilhelm-Klemm Str. 10, D-48149 Munster, Federal Republic of Germany Abstract. Monte Carlo simulations of electron diffusion become of increasing interest for scanning electron microscopy (SEM), X-ray microanalysis (XRMA) and Auger electron spectroscopy (AES) due to the increasing speed and storage capability of modern PCs. Depth distribution functions can be calculated in less than a minute also for complex specimen structures. To apply Monte Carlo simulations in the energy range of0.1-50keV it is necessary to use a data base of Mott elastic cross-sections calculated by the partial-wave method. For most applications it is sufficient to consider inelastic scattering by the Bethe continous-slowing-down approximation and inner-shell ionisations with energy losses larger than 100-200eV by the Gryzinski cross-section. In future, energy-loss functions obtained by a Kramers-Kronig analysis of experimental electron energy-loss spectra (EELS) will become of interest for a better consideration of straggling effects during the slowing-down. Key words: Monte Carlo simulation, electron scattering, X-ray microanalysis, scanning electron microscopy. We need for the X-ray microanalysis (XRMA) with 1-50 ke V electrons the depth distribution functions lI>(pz) of ionizing the corresponding inner atomic shells to calculate the ratio (1) of X-ray counts from an element (a) in the specimen and a pure-element or compound standard (s) with the ZAF factors for atomic mumber, absorption and fluorescence correction, respectively. This allows to calculate the fraction calc of s mass concentrations from the measured ratio NaiNs of X-ray counts. The depth distribution function is strongly influenced by the electron diffusion which can be described by a Boltzmann transport equation but not by an analytical solution. In case of plane surfaces and multilayers on substrates the transport equation can be simplified because the number of orginally 7 coordinates reduces to 3, one z coordinate (depth below surface), one angle 8 relative to the surface z
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