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Physics 366 Lab Report 3

Michael Dobbs, Sonoma State University
December 1, 2014
Abstract
Atomic Force Microscopy was used to analyze multiple samples to
identify their surface composition and determine their top structure.
Compiled data was used to calculate the roughness of the sample.

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Introduction

Atomic Force Microscopy is a powerful tool used to identify the surface structure of a solid by contouring the top layer with a sharp tipped probe and
amplifying the hills and troughs via laser reflection and detection. Piezoelectric materials are used to finely tune the x and y distance parameters, and a
harmonic oscillator is utilized in close contact mode to move the cantilever
in the z direction. A Scanning Probe Microscopy program processes the data
and calculates the roughness of the sample.

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Background

Gustav Schmalz designed the first Optical Profiler in 1929 in Germany. He
ran a probe attached to a cantilever across the surface, shined white light to a
mirror attached to the probe, and amplified the signal to photographic film.
The film was exposed to the reflected light of various wavelengths, causing
multiple colors to show up on the film, corresponding to varying heights on
the surface. This older design was subject to possible bending or crashing of
the probe, causing a much lower resolution of the surface on the film. Refer
to Figure 1.
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This follows the potential energy diagram in Figure 6. a force sensor is used to monitor the potential energy as a function of distance between the tip and the sample. Refer to Figure 5.2 Contact Mode In contact mode. [1] The attached probe can be pyramidal or conical in shape and a sharp tip is desired for the most accurate results. Refer to Figure 2. The motion and direction depend on the type and shape of the material. and K is the piezo constant. Each dimension (x. The computer calculates this force following: F = kz 2 (2) . usually leaving the tip only a couple of molecules thick. The battery voltage is applied and the distance change follows the equation: d2 d1 = KV (1) where d1 and d2 are the initial and final lengths respectively. Refer to Figures 3 and 4. 2. piezoelectric materials are used. y. V is the applied voltage.1 Probe Mechanics Modern atomic force microscopes utilize lasers of a single wavelength and a detector that monitors the position that the light hits it as a function of x and y distance. Refer to Figure 7. To obtain the desired radius of curvature around 2 nanometers. the tip is slid across the surface of the sample and a feedback loop maintains a constant distance between the cantilever and the sample by vertically moving the scanner to keep the force the same. and z) are controlled by a di↵erent piezoelectric. and the field strength which is controlled by applying a current through the material. the material is chemically etched.2. Piezoelectric materials (such as Quartz or Lead Zirconate Titanate) undergo a change of geometry when placed in an electric field. To keep the tip close to the sample. To control the movement of the cantilever at such fine distances. They can be triangular or rectangular in shape and are primarily made of silicon or silicon nitride. [1] K must have a smaller value that allows for the change in voltage to induce a very small change in distance. one must be able to finely tune the position of the probe to obtain the most accurate results. Cantilevers are attached to the electronics and hold the probe in place. When the surface of a sample is very small. or ion milled.

3 Operation To obtain accurate results. This mode is advantageous because the tip gets closer to the sample. which causes a square well to be seen as a triangular well.3 Close Contact Mode In close contact mode.1 Probe Exchange To replace or substitute probes. show contrast on flat samples. one must follow operating instructions carefully so as not to damage the probe tip or obtain questionable results. Using tweezers. 3. The only drawback is that each scan takes longer than contact mode. one can release the scanner and slide it out for easier access. display atomic resolution. resulting in higher lateral resolution. The tip is harder to break because the force is smaller and does less damage to soft samples.01 N/m. and work in air or liquid. 2. Lateral forces are eliminated due to the oscillation of the probe. This mode is advantageous because the tip can scan rough samples.where k is the spring constant and z is the cantilever deflection. [1] So as to not break the sensitive tip. 3 . [1] Refer to Figure 8. Replace the scanner and begin loading the sample. a harmonic oscillator attached to the cantilever oscillates the probe at an amplitude of 20 to 100 nanometers. Put the new tip in and check that the magnet has captured the cantilever. Drawbacks include the damaging of soft samples by the dragging of the probe and the distortion of features due to the lateral force between the probe and the grooves of a dip in the sample. A magnet connects the cantilever to the scanner and keeps the probe in place. The tip of the probe taps the surface at the bottom of the wave and a feedback loop maintains a constant amplitude. carefully take out the cantilever and monitor which side contains the probe as it cannot be seen with human eyes. the force is on the magnitude of .

After scanning. The electronics in the AFM are controlled by the computer.2 Computer Operation Load the sample and turn on the computer.3. 4 Data Analysis Three samples were scanned via Atomic Force Microscopy using contact mode and close contact mode. amplitude. Refer to Figure 3. the computer displays the surface height as a function of x-y position using the contrast of color. Various characteristics of the sample were calculated 4 . One must align the tip and load the correct software for the current tip. Approach the tip to the surface of the sample using the coarse and piezoelectric z motion transducers. Set the frequency. which can be converted to a 3D image. the computer compiles the data and displays a square spectra representing the surface of the sample. which operates the following components: [1] • Coarse Z Motion Translator: used for moving the probe in the z direction for long distances • Coarse X-Y Translation Stage: used for moving the sample in the x-y direction for long distances • X and Y Piezoelectric Transducer: used for moving the probe in the x-y direction for small distances (on the scale of nanometers) • Force Sensor: detects the potential force between the tip and the surface • Z Piezoelectric Ceramic: used for moving the probe in the z direction over small distances • Feedback Control Unit: connects the force sensor to the computer and signals the piezoelectric materials to change so as to keep a constant distance between the probe and the surface so as to not break the tip • X-Y Signal Generator: generates the voltage to be applied to the piezoelectric materials After the data is obtained and the signal is processed. and position if using close contact mode. Begin scanning by setting an area to scan and a time interval for each x and y component.

Roughness is defined as the standard deviation of the height and can be written as a sum or an integral following: v s u N Z bZ d X 1u 1 t ¯ 2= ¯ 2 dy dx (6) (hi h) (h(x. the surface is rough. y) h) h = N i=1 (b a)(d c) a c and written independently: h. a and b are the scanning limits in the x direction.y = 1 (d c) s Z b (h(x) h¯x )2 dx (7) h¯y )2 dy (8) a s Z d (h(y) c These calculations are displayed in the data tables in the Figures of each spectra. The mean height is defined as the sum of all the measured heights divided by the total number of measurements (N).including the mean of the height. If the deviations are large. 5 . and can be written in summation or integral form following: N X ¯h = 1 hi = N i=1 (b 1 a)(d c) Z bZ a d h(x. h. and the roughness of the sample. h¯y = 1 (d c) Z d h(y) dy (5) c The roughness is an account of the deviations of a surface from the mean of that surface. Since x and y are independent. the root mean square of the height. y) dy dx (3) c where hi is a characteristic height on the spectra. and vice versa. the mean height of each variable may also be written as: Z b 1 h¯x = h(x) dx (4) (b a) a and. and c and d are the scanning limits in the y direction.x = 1 (b a) and.

and the roughness increased to 128. A Silicon wafer was scanned using contact and close contact tips. Refer to Figures 9 and 10.19 mv while close contact mode calculated 6.A Silicon coated glass sample was scanned using contact and close contact tips. one may compare a roughness that doesnt include the bump to one that does. whereas the larger area contained a great portion of it that was relatively flat. Refer to Figures 11.11 nm (including the bump).66 mv and 71.09 mv due to the smaller area having greater variations in height comparably. 12. The program calculated a roughness average of 10. as the roughness calculated using contact mode and close contact mode were 13. the sample is very smooth with only a few aberrations.80 nm (not including the bump) and Line 2 having a roughness of 60.5 and 7.The bump on Line 2 is shown on the right side of the 2D height graph in Figure 15. This sample is a lot smoother than the silicon coated glass sample. A thermally evaporated Aluminum sample was scanned using a close contact tip and the height of the sample was analyzed using the line analysis tool of the program. The same area of 55. a value of 14. The horizontal dark lines visible across the spectra on Figure 10 were due to students bumping the table on which the AFM was placed. The data from Line 1 and Line 2 were fit to a summation of functions using Mathematica and the resulting equations for height were used to calculate the mean height and roughness of the samples using equations 4.55 µm2 was scanned. In Figure 12. The flat area can be seen on the left hand side of the 3D spectra of Figure 13.59 nm. causing the probe to jump and miscalculate the height. An area of 2. using the same scanning speed. Figure 15 shows Line 1 having a roughness of 10. The bits of Silicon caused this sample to have a high standard deviation of height due to the probe being raised over the lumps. causing the standard deviation to increase greatly. Contact mode calculated a roughness of 38. and using Mathematica.72 µm2 of the total 888.8 displayed on the last page of the report.789 nm was calculated. Using line analysis. Refer to Figures 14 and 15.22 µm2 was scanned and found to have a roughness of 20.80 nm for Line 1.47 mv respectively.67 nanometers. and 13. This approximation is higher than the actual due to the fitted 6 . where on the right side it dips and creates a larger roughness. showing the higher precision of close contact mode in comparison to contact mode. a smaller portion of the total area was selected (47.79 µm2 ). As seen from the spectrum of Figure 11. corresponding to the red highlighted result on the page after the figures. The dots seen on the sample are the Silicon bits on the glass. This very high roughness is due to the very tall lump in the top right corner of the spectrum.

line not hitting every point on the spectra. Hongtao. The computer program can calculate the surface roughness. References [1] Shi. accurate analysis of the top layers contours may be conducted.11 nm for Line 2. leading the area under the curve to be greater. This result is smaller than the actual due to my fitting equation not being able to model the quick bump around y = 1.25µm. one may obtain a more precise image of the surface than by using contact mode. otherwise the data is inconclusive due to a wide range of heights.pdf 6 Figures and Data 7 . leading to a smaller area under the curve. url: http://www.physastro. PHYS 366: Intermediate Experimental Physics. and thus a lower roughness. 5 Conclusion Atomic Force Microscopy is a practical tool for analyzing the surface of a sample. and using Mathematica. The program calculated a roughness average of 60.sonoma. As long as one is careful to not break the probe.edu/people/faculty/shi/p366/lectures/afm. Atomic Force Microscopy 2014. a value of 49. which is characteristic of the smoothness of the sample. The AFM is conclusive when the sample is relatively flat so that the calculations give reasonable results. By utilizing close contact mode.366 nanometers was calculated.

Figure 1: Gustav Schmalz Optical Profiler (1929) Figure 2: Schematic of Modern AFM System 8 .

Figure 3: Electronic Schematic of AFM System Figure 4: Piezoelectric Mechanics Figure 5: Typical Cantilever and Probe 9 .

Figure 6: Potential Energy Diagram Between Probe and Surface Figure 7: Contact Mode Mechanics Figure 8: Close Contact Mode Mechanics 10 .

Figure 9: Silicon Coated Glass Sample. Contact Mode Figure 10: Silicon Coated Glass Sample. Close Contact Mode 11 .

Close Contact Mode 12 .Figure 11: Silicon Wafer. Contact Mode Figure 12: Silicon Wafer.

3D Representation Figure 14: Thermal Evaporation Coated Aluminum Sample. Close Contact Mode 13 . Close Contact Mode.Figure 13: Silicon Wafer.

Figure 15: Thermal Evaporation Coated Aluminum Sample. Close Contact Mode. Line Analysis 14 .