TITLE: STUDY OF SURFACE MORPHOLOGY OF ANY GIVEN SPECIMEN BY ATOMIC FORCE MICROSCOPE (AFM)

THEORY: Scanning probe microscopes (SPM) define a broad group of instruments used to image and measure properties of material, chemical, and biological surfaces. SPM images are obtained by scanning a sharp probe across a surface while monitoring and compiling the tipsample interactions to provide an image. The two primary forms of SPM are scanning tunneling microscopy (STM) and atomic force microscopy (AFM) Atomic force microscopy (AFM) or scanning force microscopy (SFM) is a very high-resolution type of scanning probe microscopy, with demonstrated resolution on the order of fractions of a nanometre, more than 1000 times better than the optical diffraction limit. The precursor to the AFM, the scanning tunneling microscope, was developed by Gerd Binnig and Heinrich Rohrer in the early 1980s at IBM Research - Zurich, a development that earned them the Nobel Prize for Physics in 1986. Binnig, Quate and Gerber invented the first atomic force microscope (also abbreviated as AFM) in 1986. The first commercially available atomic force microscope was introduced in 1989. The AFM is one of the foremost tools for imaging, measuring, and manipulating matter at the nanoscale. The information is gathered by "feeling" the surface with a mechanical probe. Piezoelectric elements that facilitate tiny but accurate and precise movements on (electronic) command enable the very precise scanning. In some variations, electric potentials can also be scanned using conducting cantilevers. In newer more advanced versions, currents can even be passed through the tip to probe the electrical conductivity or transport of the underlying surface.

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Fig: Electron micrograph of a used AFM cantilever image width ~100 micrometers.

BASIC WORKING PRINCIPLE: The AFM consists of a cantilever with a sharp tip (probe) at its end that is used to scan the specimen surface. The cantilever is typically silicon or silicon nitride with a tip radius of curvature on the order of nanometers. When the tip is brought near sample surface, forces (Depending on the situation, forces that are measured in AFM can be mechanical contact force, van der Waals forces, capillary forces, chemical bonding, electrostatic forces, magnetic forces, Casimir forces, solvation forces) between the tip and the sample lead to a deflection of the cantilever according to Hooke's law. F = -kz, Where, F is the force, k is the stiffness of the lever, and z is the distance the lever is bent. This deflection is usually measured using a laser spot reflected from the top surface of the cantilever into an array of photodiodes or piezoresistive AFM cantilevers. These cantilevers are fabricated with piezoresistive elements that act as a strain gauge. Moreover, in most cases a feedback mechanism is employed to adjust the tip-to-sample distance to maintain a constant force between the tip and the sample. Traditionally, the sample is mounted on a piezoelectric tube, that can move the sample in the z direction for maintaining a constant force, and the x and y directions for scanning the sample. The resulting map of the area s = f(x,y) represents the topography of the sample.

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VARIOUS TYPES OF AFM: The AFM can be operated in a number of modes, depending on the application. In general, possible imaging modes are divided into static (also called contact) modes and a variety of dynamic (or non-contact) modes where the cantilever is vibrated. Contact Mode In this case, the tip is raster-scanned across the surface; it is deflected as it moves over the surface corrugation. In constant force mode, the tip is constantly adjusted to maintain a constant deflection, and therefore constant height above the surface. It is this adjustment that is displayed as data. This is useful for small, highspeed atomic resolution scans, and is known as variable-deflection mode.Because the tip is in hard contact with the surface, the stiffness of the lever needs to be less that the effective spring constant holding atoms together, which is on the order of 1 - 10 nN/nm. Most contact mode levers have a spring constant of < 1N/m. Noncontact mode Noncontact mode uses an oscillating cantilever. A stiff cantilever is oscillated in the attractive regime, meaning that the tip is quite close to the sample, but not touching it (hence, noncontact). The forces between the tip and sample are quite low, on the order of pN (10 -12 N). The detection scheme is based on measuring changes to the resonant frequency or amplitude of the cantilever.

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EXPERIMENTAL SET-UP: The schematic of the scanning set up is given below. In our experimental set up, the sample is actually mounted on the piezoresistive substance and the tip is moved over the sample.

Fig. AFM beam deflection detection Laser light from a solid state diode is reflected off the back of the cantilever and collected by a position sensitive detector (PSD) consisting of two closely spaced photodiodes whose output signal is collected by a differential amplifier. Angular displacement of cantilever results in one photodiode collecting more light than the other photodiode, producing an output signal (the difference between the photodiode signals normalized by their sum) which is proportional to the deflection of the cantilever. It detects cantilever deflections <1 (thermal noise limited). A long beam path (several cm) amplifies changes in beam angle. We have obtained the surface morphology of a ZnO thin film deposited on Si substrate using RF magnetron sputtering technique. The scanning was performed in non contact mode. The observed image of the surface is shown below followed by additional data colleted from the scanning.

Steps: 1. Mount the sample onto the holder. i) ii) iii) First clean up the sapphire holder with acetone. Stick a both side tape onto the sapphire. Stick the thin film on the tape.

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iv) v)

Use a blower to blow up any surface dust particle. Mount the sapphire with the sample on the mount-place of the instrument.

2. Install the cantilever into the holder i) ii) iii) Carefully take a non-contact mode AFM tip with the fine tweezers. Mount the tip on to the proper place of the tip holder. Use the associated computer to check that cantilever has been installed properly.

3. Adjustments of the Laser and the Photodiode i) Run the program ii) Switch on the unit. iii) Look at the signal and the position of the laser spot on the cantilever/tip.

Run the program. Switch on the unit. Adjust the laser and the photodiode to get the maximum laser signal.

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Fig.2 2D surface of ZnO thin film

Fig.2 Histogram of size distribution of ZnO thin film

Sample: thin Film

ZnO Value(nm) 83.6712

Average Particle size

rms surface 17.1405 roughness

Table1. Surface information of ZnO thin film

Fig.3 3D surface of ZnO thin film

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PRECAUTIONS: 1) Special care was taken while choosing the sample that the sample is not too rough, otherwise it may harm the sensitivity of the system. 2) The tip (within the cantilever) was mounted car carefully efully and slowly to avoid any damage of it. 3) The system was operated in an environment which is vibration free upto most possible limit to avoid noise in the morphology. 4) The sample was carefully attached with the Safire holder to avoid its movement at the time of scanning.

DISADVANTAGES: Scanning Area: A disadvantage of AFM compared with the scanning electron microscope (SEM) is the single scan image size. In one pass, the SEM can image an area on the order of square millimeters with a depth of field on the order of millimeters, whereas the AFM can only image a maximum height on the order of 10 10-20 micrometers and a maximum scanning area of about 150150 150150 micrometers. One method of improving the scanned area size for AFM is by using parallel probes in a fashion similar to that of millipede data storage. Scanning Speed: The scanning speed of an AFM is also a limitation. Traditionally, an AFM cannot scan can images as fast as a SEM, requiring several minutes for a typical scan, while a SEM is capable of scanning at near real real-time, time, although at relatively low quality. The relatively slow rate of scanning during AFM imaging often leads to thermal drift in the image making the AFM microscope less suited for measuring accurate distances between topographical features on the image. However, several fast fastacting designs were suggested to increase microscope scanning productivity including what is being termed video AFM (reasonable quality images are being obtained with video AFM at video rate: faster than the average SEM). To eliminate image distortions induced by thermal drift, several methods have been introduced.

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Effect of piezoelectric material: AFM images can also be affected by hysteresis of the piezoelectric material. and cross-talk between the x, y, z axes that may require software enhancement and filtering. Such filtering could "flatten" out real topographical features. However, newer AFMs utilize closed-loop scanners which practically eliminate these problems. Some AFMs also use separated orthogonal scanners (as opposed to a single tube) which also serve to eliminate part of the cross-talk problems. As with any other imaging technique, there is the possibility of image artifacts, which could be induced by an unsuitable tip, a poor operating environment, or even by the sample itself. These image artifacts are unavoidable however, their occurrence and effect on results can be reduced through various methods. AFM Probe: Due to the nature of AFM probes, they cannot normally measure steep walls or overhangs. Specially made cantilevers and AFMs can be used to modulate the probe sideways as well as up and down (as with dynamic contact and non-contact modes) to measure sidewalls, at the cost of more expensive cantilevers, lower lateral resolution and additional artifacts.

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