Force modulation atomic force microscopy: background, development and application to electrodeposited cerium oxide films

In force modulation atomic force microscopy FMAFM., vertical oscillation of the scanning tip of the AFM is added purposely and the deflection of the tip, which is influenced by surface features of the sample, is used as the z dimension to construct images. FMAFM represents a powerful technique for scientific research, but its merit has not been realized adequately to date. In this paper, the basic principles and particular features, as well as potential drawbacks of the technique, are presented and demonstrated systematically, through its application to electrochemically deposited cerium oxide films. Comparisons are also made with the more familiar contact mode AFM CMAFM.and tapping mode AFM TMAFM.. It is shown that FMAFM reveals the major topographic features of CMAFM, but affords i. greater resolution for sample features that are difficult in CMAFM, and ii. continuous two-dimensional mapping of local mechanical properties on a scale of nanometres that the CMAFM, TMAFM and any other techniques, are not capable of sensing. This information can be used to elucidate other properties of the investigated surface, such as crystallinity variation, phase separation and distribution, and mechanisms of formation of deposited films. Major artifacts associated with the technique include ‘wedge cavity effect’ and ‘tip slip effect’, for which a geometric model is proposed to elucidate their origins. The cerium oxide films are shown to be composed of relatively hard crystalline grains, of well-defined individual geometry and comparatively regular packing, alongside relatively soft amorphous patches, devoid of distinct geometry and assembled disorderly. These features are consistent with a nucleation and growth mechanism of the deposition, in which crystalline nuclei arise and grow from an intermediate cerium gel mass, produced in the interfacial region during deposition. q1998 Elsevier Science B.V.