Surface characterization and force measurements applied to industrial materials with atomic force microscopy

University dissertation from Luleå tekniska universitet

Abstract: The thesis focuses on the application of force measurements with atomic force microscopy (AFM) on materials with a few surface contacts/asperities and chemically modified surfaces. The technique allows measurements of ultra-small intermolecular and surface forces, down to the piconewton level. The force measurements between surfaces of well-defined geometry are often used to measure and model the interaction between different systems of charged and neutral surfaces in various environments. However, detailed knowledge of the contacting surface profile geometry and surface properties is required to model the fundamental forces involved in the interaction. The preparation of such well-defined and idealized surfaces is often time consuming and the surfaces may not possess the behavior and properties of a source material in real processes, such as in industry. Moreover, external factors such as magnetic fields, ionic strengths and pH-values in a solution, may further complicate the evaluation. Hence, it is desirable to explore and develop techniques for trustable measurements of forces between “real” surfaces. These are often a complex composition of various force interactions and multiple surface contacts. The AFM probe technique was explored to measure force interactions between “real” particle surfaces. The work shows the applicability of the AFM technique to study the interaction forces despite the forecasted difficulties with the roughness of the particles. A technique to measure the adhesion and work of adhesion from AFM force curves was implemented and used. The thermal tune method was implemented in our commercial NT-MDT microscope to determine cantilever spring constants. The force interactions between natural microsize (m-s) magnetite particles and synthetic nanosize (n-s) magnetite particles were studied in calcium solution with concentrations of 1, 10, 100 mM and at pH values 4, 6 and 10. The changes in force interactions, due to variations in calcium concentration and pH were investigated. The adhesion force change with the concentration and pH was similar for m-s/m-s and m-s/n-s systems, and the adhesion force increased with the concentration at pH 6, except for the highest calcium concentration of 100 mM at pH 10. It was found that the magnetite surface modification could appear at the highest calcium concentration at pH 10. Moreover, the thesis contains preliminary results of the force interaction study between natural and synthetic bentonite-magnetite particles in calcium solution with concentrations of 1, 10 and 100 mM at pH 6. The influence of roughness on the calculation of contact mechanics parameters were studied with AFM and Vertical Scanning Interferometry (VSI). This is important for future development of a model to describe and characterize the force interaction between samples with multiple surface contacts. It was found that the optical artifacts, induced by VSI, have a large influence on all the roughness parameters calculated on the calibration grids, which represent extreme surface topographies.

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