BSc (Hons) in Physics & Instrumentation Laboratory Practical LAB3: AFM Tip Characterisation

Kai Neuhaus Co-Worker: Sung Yan GMIT

Galway Mayo Institute of Technology

Lecturer: Jim McComb December 1, 2011

Abstract The tip of a probe from an atomic force microscope (AFM) is characterised by dierent methods. Characterisation of the tip of AFMs is required to assure shape consistency of the expected topography to be scanned and also to obtain reliable results for measurements and resolution. The rst method is the AFM itself (Burleigh) and the second method uses an scanning electron microscope (SEM) (Leica S340). The material composition is characterised by X-ray refraction uorescence spectroscopy and conrms the material of the probe-tip to be Si. The tips geometry is measured with the SEM and the values are used to compare the shapes that are produced by the AFM scan on a calibration grid (grid-spacing 16000nm, grid-height 200nm). The probe measured within the SEM was separately prepared compared to the probe used in the AFM and deviation between the probe geometries were found. The tip radius was found to be 800nm according to SEM measurements and about 500nm according to geometrical analysis of the scan images of the scans of the calibration grid with the AFM. Those values do not agree with the value stated in the specication sheet, that claim a tip radius to be smaller than 10nm. It is shown that the tip characteristics determine signicantly the scan image of an AFM scan and must be taken into account.

LAB3: AFM Tip Characterisation

Contents
1 Introduction 2 Technical Equipment 2.1 AFM . . . . . . . . . . . . . . 2.1.1 Principle Setup . . . . 2.1.2 Controller Adjustments 2.2 SEM . . . . . . . . . . . . . . 2.3 XRF . . . . . . . . . . . . . . 2.4 Sputter Coating . . . . . . . . 3 4 4 4 4 5 5 5 6 8 8 9 10 10 12 14 14 15 17 17 18 19 19 20 22 23 23 24 25 26

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3 Discussion Graphical Post Processing and Measuring 4 Tip 4.1 4.2 4.3 4.4 Characterisation Geometrical Eects of Tip . . . . Spring Constant and its Eects . Estimation of Tip Radius . . . . . Material Composition using XRF

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5 Conclusion 6 Appendix A Correction of bottom length for Spherical Tip B Determination of Spring Constant C Tip Specications C.1 MicroMash . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C.2 Burleigh . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D AFM Measurements D.1 Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D.2 Slope Measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . D.3 Tip Radius Estimation . . . . . . . . . . . . . . . . . . . . . . . . . . . . E SEM Measurements E.1 Tip Height . . . . . . . . . . E.2 Tip Slope . . . . . . . . . . E.3 Lever Geometry, Length and E.4 Tip Radius . . . . . . . . .

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LAB3: AFM Tip Characterisation

Introduction

Tip characterisation of atomic force microscopes (AFM) is essential to assure accurate measurements and shape consistency of the features to be scanned. The spring constant of the lever, were the tip is located on, determines the force the tip will exert on the sample as well as the resonance frequency. The resonance frequency may be of interest to determine the maximum scanning speeds and delay times to avoid oscillation of the tip during scanning. Depending on the material of interest, the actual force should be estimated to assure no deformation of the sample due to the tip. The radius of the tip will restrict the maximum resolution that can be achieved. This report describes the characterisation of the tip for an atomic force microscope (AFM) from Burleigh Instruments, Inc. and the techniques applied to obtain all important parameters of the tip and how the tip shape is aecting the image produced by the AFM. Important parameters for the tip characterisation are the tip shape, height and the tip radius, as well as the material and the properties of the lever the tip is located on. The properties of the lever are its geometrical dimensions and its spring constant. To characterize the tip shape with the AFM a calibration grid (grid spacing 16m, height 0.2m) is used and the resulting image is evaluated. The tip shape was further investigated with an scanning electron microscope (SEM) from LEO Electron Microscopy Ltd. and measured. The properties of the material were evaluated by X-Ray refraction on the same SEM.

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LAB3: AFM Tip Characterisation

2
2.1
2.1.1

Technical Equipment
AFM
Principle Setup

To obtain scanning images an Burleigh atomic force microscope (AFM) (Burleigh Instruments, 1997) was operated in topographic mode together with an calibration grid with a spacing of 1600nm and height of the grid-lines of 200nm. The scan images were taken at dierent magnication and image processing was performed depending on the requirements until an sucient picture for post processing was obtained subsection D.2. A calibration was performed according to the assumed values of the calibration grid subsection D.1. The AFM supplies a scan range of about 70m in x and y, and in z of about 6m. For a zoom factor of 2 that was used for the nal images, the maximum visible range becomes 35x35m. In the pictures this range appears even smaller due to the modied scan limits (590000) according to the correction factor. A The calibration for the z-values was performed by averaging over all z-values and setting the average equal to the assumed height of the grid (200nm).

2.1.2

Controller Adjustments

The scans were consistently preformed with an reference force according to 5V. During some trial scans the integral, dierential and gain controls were adjusted until an sucient image could be obtained. According to the manual (Burleigh Instruments, 1997) the integral gain determines how the controller follows the over-all shape of the sample. The dierential gain determines how sensitive the controller reacts on shape changes (z). Apparently the gain appeared to have the largest eect in improving the image quality. Some further adjustments were performed according to the scanner delays to even improve image quality to avoid oscillation of the tip.

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LAB3: AFM Tip Characterisation

2.2

SEM

Investigating the tip geometry was done with an scanning electron microscope from Leica (Leica S430 Stereoscope). A second tip was prepared, besides of the tip used in the AFM, by coating it with gold of about a 15nm layer by a sputter process. As the tip may be dierent compared to the tip in the AFM, the characterisation may not produce necessarily conclusive results.

2.3

XRF

The x-ray refraction uorescence (XRF) scanning was used to determine the material composition of the tip. This investigation was done equally with the SEM and an attached solid state detector cooled with liquid nitrogen. The solid state detector was counting the amount of the x-rays of dierent energies and the energy values were processed by a software plotting the energy spectrum (subsection 4.4).

2.4

Sputter Coating

One AFM tip was prepared with a gold coating of about 15nm thickness by a sputter coater to be able to use it for the SEM. The tip was processed for about 1min at a pressure of about 1 101 mbar or 10P a. It is to expect that the probe may have assembled a certain amount of dust on its tip that becomes xated and may alter the tip radius visible in the SEM.

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LAB3: AFM Tip Characterisation

Discussion Graphical Post Processing and Measuring

The measurements of the calibration grid on the AFM were performed with the system software and the the pictures of the cross sectional geometry were stored without the use of cursors for measurements. It was anticipated to preserve a rather pristine picture to be able to do measurements on the pictures directly. To assure the accuracy is preserved an estimation of possible errors is discussed in this chapter. Some graphically measurements were performed in Figure 1.

194.54nm / 50.250mm

a bc d

Figure 1: AFM Cross Section Plot of Calibration Grid. Four distances (a,b,c,d) where measured graphically and compared to the known distance measured by the system software (Bearing Level = 150.88nm).

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LAB3: AFM Tip Characterisation To calibrate the graphical tool (Inkscape., 2011) the total height of the measure box (195.54nm 53.58nm = 141.96nm was determined and equalled to the measured length with Inkscape. (50.250mm).

factorcal =

141.96nm = 2.825nm/mm 50.250mm

(1)

To obtain the measuring values for the real heights on the graph

height = factorcal length + 53.58nm

length mm height nm

(2)

a 34.445 b 34.463 c 34.451 d 34.437 mean std

150.89 150.94 150.91 150.87 150.90 0.03

Table 1: Measured Values a,b,c,d The mean value of the heights results in h = 150.90 0.03nm. Comparing this to the measured height directly measured (150.88nm) this is an percentage deviation of 0.1%. To support further the precision that can be achieved with post-graphically processing the subsequent gure Figure 2 is shown here.

Figure 2: High zoom level for accurate positioning of measure bars in Inkscape. The green bar is the lower line at 53.58nm (see Figure 1)

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LAB3: AFM Tip Characterisation

4
4.1

Tip Characterisation
Geometrical Eects of Tip

spherical tip on the edge moving into the groove R 16m image to expect due to R the spherical tip R

D = 5m R= D 2 h=0.2m

Figure 3: Spherical tip shape and expected image produced. The dimensions of the grid height compared of the tip diameter are distorted and the resulting image would have an even shallower edge. The correct size of the bottom should be calculated with Equation 4.

dl =

R2 (R h)2

see Appendix A L = l + 2dl

(3) (4)

asymmetrical pyramidal tip

30 16m 30 possible picture to be obtained by a scan with pyramidal tip

60

h=0.2m

60

Figure 4: Asymmetric pyramidal tip shape and expected image produced. The dimensions of the grid height compared of the tip diameter are distorted and the resulting image would have an even shallower edge. The actual size of the bottom should then be calculated with Equation 5. h h L=l+ + tan(30 ) tan(60 )

(5)

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4.2

Spring Constant and its Eects

The spring constant describes the stiness of the lever where the tip is attached on. During contact mode a certain force is asserted onto the tip and subsequently the lever is deected. The deection creates an angular turning of the tip. This angular displacement would also be visible within the scan-picture depending on its size. The spring constant is given according to Appendix C as 0.12N m1 . No particular force calibration was performed but according to Nanoscience Instruments about 1012 N are to expect. Thus a deviation can be estimated according to Equation 8 (Hookes Law).

F = kx F x= k x= 1012 N = 8.3 1011 m = 83.3pm 0.12N m1 l x t Figure 5: Displacement of the tip caused by the contact force.

(6) (7) (8)

According to Appendix C the lever length l is 290m 5nm (compare with Figure 16 295.68m in Appendix E.3). A deviation of 83.3pm causes by the contact force of 1012 N would cause the tip to turn according to Equation 9.

x = atan( ) = atan l

83.3pm 290m

= 0.000016

(9)

Though, Rabke suggests possible forces of 10 109 N (Rabke, 1998) then the angular displacement would increase to 0.016 . These angular displacements due to the contact force appear very small and it is questionable if they are observable within the image at all. Further estimations according to the spring constant are shown in Appendix B.

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LAB3: AFM Tip Characterisation

4.3

Estimation of Tip Radius

The tip radius is stated by the specication Appendix C as smaller than 10nm. An estimation of the tip radius was performed by the use of the scan images subsection D.3 and compared with the shape obtained with the SEM subsection E.4. The values obtained with the AFM are about 525nm for the tip radius and the value obtained with the SEM is about 800nm for the tip radius. Though, both values are far too large to be comparable with 10nm as stated in the specication, they express some indication that the size may be that large as measured. Dierent eects may cause a larger tip radius, like dust particles accumulating on the tip due to electrostatic forces and wear and tear breaking o fractions of the tip. The tips investigated in the SEM and the AFM were actually dierent tips and larger dierences between the measured values were to expect. The source and the use of the tip measured in the SEM was not known but for the tip of the AFM it can be assumed it was already heavily used by dierent students before.

4.4

Material Composition using XRF

The results of the XRF scan are shown in Figure 6. The largest peak occurs for silicon (Si) as it was to expect, as the the tip was supposed to be composed out of silicon nitride according to the spec-sheet (Figure 10). A small signal can be found for aluminium (Al) as it was the material of the holder but also the the material of the reective coating on the cantilever. Another signal for gold (Au) can be found besides of niobium (Nb). Though, a signal for gold could be expected due to the gold coating, it is usually not visible as the layer of the gold is to thin and no intearction with the electrons occurs to produce any X-rays. The signal for the gold is also not perfectly unique, as the tip of the signal resides between gold and niobium. However, the existence of niobium itself can only be explained due to some contamination. Also the easiest explanation for the peaks for carbon (C), silver (Ag) and cadmium (Cd) are possible contamination eects. The contamination theory is supported by another scan slightly besides from the top of the tip as most of the peculiar peaks disappear (Figure 7). Kai Neuhaus 10/ 27

LAB3: AFM Tip Characterisation

Figure 6: XRF scan directly on top of the tip.

Figure 7: XRF scan of the tips side.

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LAB3: AFM Tip Characterisation

Conclusion

Though, the preparation were restricted to two dierent probe samples, one for the AFM and one for the SEM investigations, introducing unknown dierences, some basic properties of the shape of the tip of an AFM could be shown. The results of the slope obtained from the AFM scans (0.45 and 0.37) and the slope obtained from the tips aspect ratio (3.28) measured do not agree. This can be explained in accordance with the large tip radius that was estimated with about 800nm (see subsection E.4). Considering, that the grid height is only 200nm then the tip radius is signicant for creating the slope. An estimation how the slope would occur with an tip radius of 800nm resulted in a value of 0.882. This agrees much better with the obtained values from the AFM (0.45 and 0.37) and may conrm partially the large tip radius. The dierence between the values of the slopes obtain from tha AFM may be explained by the calibration grid not perfectly leveled within the x-y-plane of the AFM scan range. According to the values in Appendix D.2 the tild angle would be about 4 . However, it is also conceivable, that the tip is tilded during scan due to frictional forces. The large radius of the tip was a bit of an concern, if one assumes the tip prepared for the SEM was an unused tip. But this assumption may be unfounded. However, the large values for the tip radius compared to the radius stated in the spec sheet (10nm) do not concur at all (Appendix C.1) Though, the SEM can achieve a theoretical resolution of 0.5nm it can be assumed the resolution is restricted further by the adjustments of the apertures and the spot size is much larger than 0.5nm. Also the resolution of the SEM is restricted due to the interaction volume. The very end of the tip may well not be visible at all if it does not generate any secondary electrons. The tip radius was also estimated by the radius of the upper edge of the grid slope in the AFM images and resulted in an average value of about 525nm (subsection E.4). This appears also to conrm the relative large tip radius against all other expectations. The spring constant was only compared alone by geometrical means and material properties. Using the measured geometry data of the lever (Appendix E.4) a spring constant k with a value of 16N/m can be obtained (Appendix B). This value does not agree with the values of the specication in Appendix C.1. Though, if adjusting the thickness to 1m a value for the spring constant becomes 0.02N/m - much closer to the expected values, with Equation 16. As mentioned in Appendix B it appears as if the tip is somehow dierent to that of the specication sheet and this would easily explain all kinds of dierences between measured values and expected values. Kai Neuhaus 12/ 27

LAB3: AFM Tip Characterisation However, the measured radii occurring in the AFM images compared to the estimated tip radius of the SEM image appear to concur to some degree. Further more do the scan images of the AFM show signicant shapes that are to expect with a tip and a large tip radius. In general can be assumed, that it is possible to compare the tip of an AFM probe with measurements of its SEM image, if one uses one and the same probe and can access reliable specication sheets describing the parameter of the probe. It is shown that the characteristics of the probe-tip of an AFM contribute signicantly to the resulting scan image and must be taken into account if one wants reliable results from an AFM scan.

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LAB3: AFM Tip Characterisation

6 A

Appendix Correction of bottom length for Spherical Tip

h L u R R=u+h u=Rh 2 R = l 2 + u2 l 2 = R 2 u2 l = R2 u2 substitute u by Equation 11 l= R2 (R h)2 (10) (11) (12) (13) (14) (15)

Figure 8: Deduction for spherical tip

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LAB3: AFM Tip Characterisation

Determination of Spring Constant

The spring constant can be determined by applying dierent forces to the lever and record its deviation from zero according to such forces. Then the spring constant is the slope of the resulting curve. Such a curve could be obtained with the force calibration curve Figure 9. However, depending on the start situation one would have to calibrate for force measurements for each sample. If the spring constant would be unknown, then it would be fairly impossible to calibrate and to measure any force at all. Another way would be to use the cantilevers geometric parameters and the E modulus to estimate the spring constant before hand (Equation 16).

Figure 9: Force Calibration Curve Example. According to Ying, Reitsma and Gates the spring constant can be calculated with Equation 16, where k is the spring constant, E the Youngs modulus, t the thickness of the lever, w the width of the lever and L the length. k= Ewt3 4L3 (16)

MikroMasch states the E with 1.691011 N/m2 (in 110 direction). The lever is a structure comprised by a triangular arrangement of two levers (see Figure 16). The length, width Kai Neuhaus 15/ 27

LAB3: AFM Tip Characterisation and thickness was measured with the SEM as L = 430m, w = 30m, t = 8m. The uncertainty of the values was estimated as 0.1m. To approximate the triangular arrangement to one single lever the width was taken twice into account with w = 60m.

k=

3 169 109 N/m2 60m (8m)3 = 16N/m 4 (430m)3

(17)

The spring constant stated in the specication is 0.12 N/m typically (0.30 N/m max). The estimated value does not concur with the value of the specication (Appendix C.1). A possible explanation for the large discrepancy may be that the tip is not the tip according to the spec-sheet Appendix C.1. Because another specication sheet from the manual of the AFM oers dierent values (Appendix C.2) for the thickness of the lever (1m). Otherwise it is indeed dicult to explain the discrepancy alone by errors made during the measurement with the SEM. Other reasons might be, that the E modulus is dependent of the direction of the lattice structure of silicon and the applied calculation do not account for the direction here, because there was no reliable way to determine it. Using the value for the thickness of the lever from the specication sheet (Appendix C.2) that states a typical thickness with t = 1m, the subsequent value for the spring constant becomes 0.02 N/m. This conrms also the large eect the thickness contributes to the variation of the spring constant. Deviations of the length of the lever account with an exponent of 3. Though, the eect is not large enough to compensate for the deviation that are caused by the measured thickness of 8m. There is a good reason to believe that the available probe tips are not according those stated in the specication sheet. The manual supplies a second type of tips subsection C.2 with a cantilever thickness of 7m that would concur much better with the measurement results of the SEM.

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LAB3: AFM Tip Characterisation

C
C.1

Tip Specications
MicroMash

Figure 10: Tip Specication Sheet

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LAB3: AFM Tip Characterisation

C.2

Burleigh

Table 2: Tip Specication according to the Burleigh Manual.

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D
D.1

AFM Measurements
Calibration

Figure 11: Calibration for Zoom 2x horizontal spacing / nm 16408.3 16629.4 16762.1 mean 16603.3 std 146.7 (0.9%) Table 3: Grid spacing measured for 2x zoom and correction factor The uncertainty introduced by the correction factor appears insignicant compared to the expected uncertainty of the slope values. Assuming a grid spacing of 16000nm and the avearge measured grid spacing of 16603.3nm a correction factor was calculated as 16000.0 = 0.963664. 16603.3

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D.2

Slope Measurements

Figure 12: Measured slopes. Zoom 2X, Plane removal. dX1/nm 492.0100 227.4900* 454.9700 476.1400 248.6500* mean std dX1(corr)/nm 474.1323 219.2239* 438.4382 458.8390 239.6151* 457.14 14.62 dX2/nm dX2(corr)/nm 481.4300 463.9368 544.9100 525.1102 597.8100 576.0880

521.71 45.85

132.93 12.87

Table 4: Values for dX and dY measured. The values are corrected with 0.963664 as in subsection D.1 The marked (*) values were omitted.

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LAB3: AFM Tip Characterisation height 1/nm 140.24 124.58* 140.24 145.72 133.19* height 1(corr)/nm height 2/nm height 2(corr)/nm 203.98 115.19 167.55 138.28 201.13 203.98 145.33 211.39 211.96

Table 5: The height was measured with inkscape section 3. The correction factor for the height was obtained by the mean over all height values as 1.45 (marked (*) values omitted). slope 1 0.43022 0.46525 0.46194 mean 0.45247 std 0.01579 slopes 2 0.36116 0.38303 0.36694 0.37037 0.00926

Table 6: Slopes and angle of slope for dX and height. The values for slope1 and slope2, respectively 0.45 0.02m and 0.37 0.01m are dierent by some degree. The slopes are describing an angle and the dierence between these angles is = atan(0.45) atan(0.37) 4 (18)

This dierence could be explained due to the calibration grid not perfectly in level with the x-y-plane the AFM is scanning and reperesents the angle the calibration grid may be tilded.

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D.3

Tip Radius Estimation

R3 R2 R1

Figure 13: Radius Estimation. Zoom 2X, plane removal, medium pixel averaging. R1=1898nm; R2=571nm; R3=479nm. The value of R1 appears to be too large and probably caused by surface defects or dust particles. The mean of R2 and R3 is 525nm. The tip radius was estimated by constructing circular sections that match best the shape of the radius on the upper edge of the slope. The radius of the circular sections was calculated equally like as in section 3.

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E
E.1

SEM Measurements
Tip Height

Figure 14: Height of AFM tip measured with SEM. Focus= 50 mm EHT=28.59 kV Photo No.=7126 WD= 50 mm Mag= 1.11 K X 5-Dec-2009

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LAB3: AFM Tip Characterisation

E.2

Tip Slope

Figure 15: Slope of the AFM tip. 18.5 + 15.4 = 33.9 73.05 and slope = tan(73.05 ) = 3.28

33.9 2

= 16.95 . 90 16.95 =

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E.3

Lever Geometry, Length and Thickness

Figure 16: The Lever Geometry. The eective distance of the probe tip from the substrate is about 295 1m. The length of the arms are an average of about 430m from the substrate edge to the tip. The thickness of the lever (not shown) is about 8m. The uncertainty is larger than compared to the values shown in the micrograph considering the ability to position the cursors onto the exact position.

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E.4

Tip Radius

Figure 17: Tip Radius estimation. The box size is about 1600nm x 1600nm therefore enclosing a circle of a diameter of 1600nm or about 800nm radius. Assuming an estimated tip radius of 800nm according to the micrograph (Figure 17) it is possible to estimate an initial slope to expect with an equal tip on the AFM by

slope =

R2 (R h)2 = Rh

800nm2 (800nm 200nm)2 = 0.882 800nm 200nm

(19)

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References
Burleigh Instruments, I. (1997), METRIS-2001, Burleigh Instruments (UK) Ltd. 9 Allied Business Center, Coldharbour Lane Harpenden, Herts, AL5 4UT, UK. Webpage. Default. Inaccessible. URL: www. burleigh. com Inkscape. (2011), Webpage. Accessed: 25 Nov 2011. Draw Freely. URL: http://inkscape.org/ MikroMasch (n.d.), Webpage. Accessed 27 Nov 2011. URL: http: // www. spmtips. com/ faq Nanoscience Instruments, I. (2011), Atomic force microscopy overview, Webpage. Accessed 26 Nov 2011. URL: http: // www. nanoscience. com/ education/ afm. html Rabke, C. (1998), Atomic force microscopy., Ceramic Industry 148(13), 52. URL: http: // 0-search. ebscohost. com. library. gmit. ie/ login. aspx? direct= true&db= buh&AN= 1403996&site= ehost-live Ying, Z. C., Reitsma, M. G. and Gates, R. S. (2007), Direct measurement of cantilever spring constants and correction for cantilever irregularities using an instrumented indenter., Review of Scientic Instruments 78(6), 063708. URL: http: // 0-search. ebscohost. com. library. gmit. ie/ login. aspx? direct= true&db= aph&AN= 25684824&site= ehost-live

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