Accurate Thickness Measurements in Thin Films with Surface Analysis

Abstract

Quantification in surface analysis using Auger electron spectroscopy and X-ray photoelectron spectroscopy has been the topic of significant work at NPL. A new approach to the quantification of materials that are homogeneous over the analysis volume has been developed using new average matrix relative sensitivity factors. These show agreement between theory and experiment at ~10% for all peaks and elements analysed. For samples that are not homogeneous, layer thicknesses are often required. For ultra-thin gate oxides, the International Technology Roadmap for Semiconductors requires 1.3% accuracy. For this purpose, angle-resolved XPS is a good candidate. In a wide study under the auspices of the Consultative Committee for Amount of Substance (CCQM), the accuracy of measurements of the thicknesses of SiO2 layers <8 nm thick on Si have been assessed. This study involved 45 sets of measurements in laboratories using MEIS, NRA, RBS, EBS, XPS, SIMS, ellipsometry, GIXRR, NR and TEM. The relative strengths and weaknesses become clear. These show that if XPS is used under reference conditions it can be reliable and fast with an accuracy, based on a calibration from the study, ~ 1%. Inter-method correlations as good as 0.05 nm are achieved over the 8 nm range. Furthermore, certain methods, thought to be accurate, suffer from incompleteness of the measurement method. For thicker layers, sputtering is generally used. Here a new method has been tested to generate a sputter yield database, for argon ions, of 26 critical elements. This database has been used to help evaluate a new semi-empirical theory of sputtering yields that includes terms missing from the current semi-empirical theories and removes errors that are up to, and may exceed, a factor of 5. The new theory agrees with published data at ~ 10% and shows why certain elements have anomalously high yields.