Page 308 - Book Hosokawa Nanoparticle Technology Handbook
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5.3 SURFACE STRUCTURE                                                        FUNDAMENTALS
                  Table 5.3.2                                    Instruments) and noncontact mode. Small piezoelec-
                  Setting of scan rate in several conditions.    tric device on the cantilever holder is oscillated by
                                                                 applying the AC voltage and the cantilever is exter-
                                                     Scan rate   nally oscillated at or close to its resonance frequency.
                                                                 The frequency characteristic of the cantilever called Q
                  To prevent the distortion in image (reduce drift) Higher
                  To clear the image (improve surface tracking)  Lower  curve is derived from a plot of frequency versus
                  To reduce scratching in image       Lower      amplitude (Fig. 5.3.6a).
                  To image with wide scan area        Lower       The resonance frequency is found by the Q curve.
                                                                 When the probe tip interacts with a surface, the ampli-
                                                                 tude of oscillation generally shifts to a lower value.
                                                                  In the tapping mode, a constant amplitude shift is
                  for getting good image. During scanning, the drift of  maintained by the feedback control during the
                  tip sometimes occurs due to vibration and thermal  Ruster scanning and the topographical image is
                  expansion of AFM instrument. The drift depends on  obtained. While scanning, the oscillating cantilever
                  measurement environment and individual instrument.  contacts the sample surface intermittently in repul-
                  It also influences the optimum scan rate and it is  sive force region and the lateral friction between the
                  determined by trial and error as shown in Table 5.3.2.   tip and the sample surface is very small.  Thus it
                    In the contact mode, AFM provides the atomic image  moderates the wear of the tip while scanning and it
                  of apical oxygen on the freshly cleaved mica surface  provides reproducible and good images of the sam-
                  easily. Thus cleaved mica is commonly used as a stan-  ple surface that are otherwise easily damaged. In
                  dard sample for a validation test of the AFM instru-  addition, this mode allows scanning without scratch-
                  ment. However, the image is not real atomic image  ing and imaging the sample surface with large
                  because single point-like defects are not observed. In  roughness, e.g., nanoparticles.
                  addition, the radius of curvature is not small enough to  Fig. 5.3.7 shows tapping-mode AFM image of gold
                  get atomic image in the contact mode.          nanoparticles with 30 nm diameter immobilized onto
                    Today, it is believed that cyclic friction during  Langmuir–Blodgett film by electrostatic adsorption [2].
                  scanning induces pseudo-atomic image. However,  In the noncontact mode, the tip hovers above the
                  it is still useful to obtain the lattice parameter and  sample surface with small distance while scanning. A
                  crystal orientation of the sample. This problem is  constant frequency shift is maintained by the feed-
                  not so important for observation of nanoparticles  back control during the Ruster scanning (Fig. 5.3.6b).
                  because the size of the nanoparticles is same as or  The mechanical resonance frequency (Q) of the can-
                  larger than the radius of curvature of the tip of the  tilever is low, several hundreds in air. However it
                  cantilever. However it is often difficult to get good  reaches several tens of thousands in vacuum and it
                  image of nanoparticles because the tip often grabs a  allows controlling very small force in attractive force
                  nanoparticle during the scan and moves it. In such  region. The AFM in this mode is called non-contact
                  situation, dynamic mode is useful as described in  AFM (NC-AFM).
                  next section.                                   The real atomic image is derived by NC-AFM with-
                                                                 out contact during scanning when atomically sharp tip
                    5.3.1.5 Topographic imaging 2: dynamic mode  is used. After the instruments to detect frequency shift
                  Dynamic mode is classified into tapping mode   precisely are commercially available, NC-AFM
                  (tapping mode is a registered trademark of  Veeco  becomes widely used.



                                         response
                                         frequency

                                                                               Δf
                              A                                      A
                                     ΔA





                                    set frequency       f                                     f

                  Figure 5.3.6
                  (a) Tapping mode. (b) Non-contact mode.

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