We propose an improved system that enables simultaneous excitation and measurements of at least two resonance frequency spectra of a vibrating atomic force microscopy (AFM) cantilever. With the dual resonance excitation system it is not only possible to excite the cantilever vibrations in different frequency ranges but also to control the excitation amplitude for the individual modes. This system can be used to excite the resonance frequencies of a cantilever that is either free of the tip-sample interactions or engaged in contact with the sample surface. The atomic force acoustic microscopy and principally similar methods utilize resonance frequencies of the AFM cantilever vibrating while in contact with the sample surface to determine its local elastic modulus. As such calculation demands values of at least two resonance frequencies, two or three subsequent measurements of the contact resonance spectra are necessary. Our approach shortens the measurement time by a factor of two and limits the influence of the AFM tip wear on the values of the tip-sample contact stiffness. In addition, it allows for in situ observation of processes transpiring within the AFM tip or the sample during non-elastic interaction, such as tip fracture.
Atomic force acoustic microscopy (AFAM) is a non-destructive method able to determine the indentation modulus of a sample with high lateral and depth resolution. We used the AFAM technique to measure the indentation modulus of film-substrate systems M sam and then to extract the value of the indentation modulus of the film M f . The investigated samples were films of silicon oxide thermally grown on silicon single crystal substrates by use of dry and wet oxidation methods. The thickness of the samples ranged from 7 nm to 28 nm as measured by ellipsometry. Our results clearly show that the values of M sam obtained for the film-substrate systems depended on the applied static load and the film thickness. The observed dependency was used to evaluate the indentation modulus of the film. The values obtained for M f ranged from 77 GPa to 95 GPa and were in good agreement with values reported in the literature.
The atomic force acoustic microscopy (AFAM) technique has been used to determine elastic properties of films with thicknesses decreasing from several hundreds of nanometers to several nanometers. It has been shown that metal films as thin as 50 nm can be characterized directly without the need to consider the influence of the substrate. For films with thicknesses ranging from about 30 to 50 nm, measurement parameters can be chosen such as to allow characterization of the elastic properties of either the film or the film–substrate interface. This attribute has been combined with the ability of the method to obtain qualitative stiffness images to show variations in the film–substrate adhesion. The AFAM technique has been also used to determine the indentation modulus of thin films of silicon oxide with thicknesses ranging from 7 to 28 nm. In this case, elastic properties of the substrate had to be considered. The examples of the applications of the AFAM method reported here for characterization of elastic properties of very thin films have shown that this technique has the lateral and depth resolution required to characterize the very thin films used nowadays in microelectronics industry.
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