Basic Laboratory. Materials Science and Engineering. Atomic Force Microscopy (AFM)

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1 Basic Laboratory Materials Science and Engineering Atomic Force Microscopy (AFM) M108 Stand: Aim: Presentation of an application of the AFM for studying surface morphology. Inhalt 1.Introduction Basic Principles Tip-sample interaction Basic modes of operation Contact mode Tapping mode Tip effects Test proceeding and evaluation Questions Literature... 7

2 1. Introduction The atomic force microscope (AFM) was invented in 1986 by Binning, Quate and Gerber as a logical step in the development of scanning tunneling microscopy (STM), which was used only for studying conductive surfaces. The AFM is used to solve processing and materials problems in a wide range of technologies and sciences. The materials investigated include thin films, ceramics, composites, synthetic and biological membranes, polymers, metals, and semiconductors. In addition to its superior resolution, the AFM has some advantages: Compared with SEM, the AFM provides extraordinary topographical contrast of the surfaces (no coating is necessary for dielectric samples). Compared with TEM, 3-dimensional AFM images obtained give a complete information better than 2 dimensional profiles of cross-sectioned samples without an expensive sample preparation. Compared with optical interferometric microscopes, AFM provides unambiguous measurement of step heights, independent of reflectivity differences between materials. 2. Basic Principles Like every scanning probe microscopes, the AFM utilizes a sharp probe raster scanning the sample surface. In the case of the AFM, different types of tip are available, for biological samples colloidal probe technique is used where a particle is glued to the end of a cantilever. Otherwise atomically sharp tip is utilized (radius R ~10 nm). The cantilever bends in response to the force between the tip and the sample. The general setup of any AFM apparatus with an atomically sharp tip including several components allows line-by-line scanning while monitoring nanometer scale cantilever deflections in vertical and horizontal directions (Figure 1). Figure 1: General AFM instrumentation. 2

3 Precise 3-D movements of the sample and the cantilever within a fraction of a nanometer are provided by a piezo element. A microfabricated probe consists of a silicon nitride cantilever with an integrated pyramid tip of several microns in height and a tip radius in the range of 5 to 100nm (Figure 2). Figure 2: Types of AFM probes and the cantilever. The AFM tip deflection is monitored, for example by an array of photodiodes. Typical software for 3-D image analysis includes a variety of corrections, filtration and evaluations such as planefit, flatten and frequency filters that can greatly improve visibility of surface morphology details and allow evaluation of the geometrical surface dimensions. The normal load exerted on the tip varies with a typical force range of 0.1 to 100 nn for routine measurements. For a nominal tip-sample contact area of several square nanometers, this load corresponds to local pressure in the range of several MPas to tens of GPas. The AFM can be operated in two principal modes: with feedback control without feedback control With the feedback control, the positioning piezo, which is moving the sample up and down, responds to any changes in force detected, and alter the tip-sample separation to restore the force to a pre-determined value. This mode of operation is known as constant force mode, and usually a reliable topographical image can be obtained. Without the feedback control, the microscope is said to be operating in the deflection mode. This is practical for imaging very flat samples at high resolution. Often it is best to have a small amount of a feedback-loop gain to avoid damaging the tip. This is also known as error signal mode. 3

4 3. Tip-sample interaction Two electrically neutral and non-magnetic bodies held at a distance of few nanometers, Van der Waals (vdw) forces usually is the dominating force between them. Non-polar molecules possess finite fluctuating dipoles and higher multi-pole moments at short time intervals. This gives rise to dispersion forces between them. The dispersion forces, generally termed as vdw forces, are typically attractive and rapidly increase as atoms or bodies approach each other. The forcedistance (F-s) dependence here is described by, F.vdW 1/s 7 The vdw forces acting between two macroscopic bodies can be calculated by assuming the vdw forces to be additive. For a tip with radius of curvature R held at a distance s from the surface, FvdW = (hr/6s 2 ) Where h is the material-dependent Hamaker constant i.e., h = - π 2 Cρ 1 ρ 2, with interaction parameter of point-point interaction C, and the number of molecules per unit volume in both tip and the sample surface ρ 1 ρ 2. Contact mode means the interaction force is in the repulsive regime of the intermolecular force curve (Figure 5). Figure 3: The force-distance curve and different regimes of the tip-surface interaction. The forces can be derived from the deflection of the cantilever ΔZ, according to Hooke`s law, F = k ΔZ Where k is the cantilever (spring) constant. For atomic resolution, k has to be less than k at, the effective spring constant for interatomic coupling in solids, which is in the order of: k at = ω at 2 m at = 10 Nm -1 4

5 For microfabricated cantilevers with typical lateral dimensions of about 100 μm and thicknesses of about 1 μm, this constant is in the range of 0.1 to 1 Nm-1 and resonant frequencies of 10 to 100 khz. 4. Basic modes of operation The image contrast can be achieved in many ways. The different modes available depending on the interaction are: contact mode, intermittent contact mode, friction force mode, non-contact, tapping mode, force modulation, etc. (Figure 4). Figure 4: Different scanning modes in AFM. 5. Contact mode In this mode, the AFM tip is dragged over the sample surface at a constant velocity and under a constant normal load. The tip is in intimate contact with the surface (point A on a force-distance curve). Scanning can be done in two ways: one is constant height mode, where the cantilever deflection is kept constant by extending or retracting piezoelement and the other is deflection mode if the piezotube extension is kept constant and the cantilever deflection is recorded. 5

6 The contact mode allows us to obtain surface topography with high precision and also provides the highest lateral resolution up to 0.2 to 0.3 nm, but imposes high local pressure and shear stress on the surface. The small contact area (10 to 100 nm 2 ) and significant contribution of the capillary forces are major features of the AFM operations in air. Thus, even very low normal forces in the range of nanonewton result in very high normal pressure and shear stresses in 0.1 to 100 GPa range, which can easily damage soft sample like polymers. For extremely soft materials such as, gels, the fluid contact mode is the best choice. Water or alcohol is the typical used fluid. 6. Tapping mode Tapping mode is an advanced mode between contact mode and non-contact mode in AFM, is applied to avoid high-lateral forces between the cantilever and the sample surface, and dragging the tip across the sample. This can be done by vibrating the cantilever with constant amplitude. In this mode high resolution topographic imaging of sensitive and soft surfaced samples can be done. Tapping mode overcomes typical issues with friction, adhesion, electrostatic forces, etc. The tapping mode oscillates back and forth on the force-distance curve figure 3. This is only an average response to the interaction between the tip and the surface. By selection of the optimal oscillation frequency and force on the sample is automatically set. Force can be maintained to the lowest possible level. As the tip passes over a bump on the sample surface, the cantilever has less room to oscillate hence the amplitude of the oscillation reduces. On the contrary, as the tip passes over a dip, the cantilever has more room for oscillation, increasing the amplitude. The amplitude of the oscillation of the cantilever is measured by the detector. The amplitude is kept constant with the help of feedback loop. Unlike contact and non-contact modes, tapping mode prevents the tip from sticking to the surface and causing damage during the scanning as the probe has sufficient oscillation to overcome the tip-sample adhesion forces. 7. Tip effects One of the most important factors influencing the resolution that maybe achieved with the AFM is the sharpness of the tip. The best tips may have a radius of curvature of around 5 to 10 nm. The necessity for sharp tips is normally explained in terms of tip convolution. The main influences are broadening, compression, interaction forces, and aspect ratio. Tip broadening arises when the radius of curvature of the tip is comparable with, or greater than, the size of the feature trying to be imaged. As the tip scans over the specimen, the sides of the tip make contact before the apex, and the microscope begins to respond to the feature. Compression occurs when the tip is over the feature trying to be imaged (it is important for very soft samples such as biological DNA). Some changes, which may be perceived as being topographical, may in fact be due to a change in the 6

7 interaction force. In this case, the tapping images may be useful to distinguish between the two. The aspect ratio (or cone angle) of a particular tip is crucial when imaging steep sloped features. 8. Test proceeding and evaluation This test must be done under supervision. Do not try to operate any part of the AFM equipment by yourself as the equipment is very expensive. Test 1: AFM imaging on a Si surface with nanoclusters. Comparison with SEM-images. Test 2: Substrate roughness analysis (Si wafers with a deposited metal film). Line and surface region measurements (to study the dependence of the average roughness on the analysis area). 9. Questions 1. What are the main advantages and disadvantages of AFM compared with SEM, TEM and Optical Interferometric Microscopes? 2. Which tip-sample interaction is important when imaging in contact mode? 3. How much is the contact area (tip-sample) and local pressure on the surface? 4. What does rms roughness mean? 5. Which mode of operation can be used for phase identification of samples? 10. Literature Scanning probe microscopy and spectroscopy, R. Wiesendanger, Cambridge University Press, Scanning Force microscopy D.Sarid, Oxford Uni. Press, NY,

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