8.
Veeco Scanning Probe Microscope
8.1 Prerequisites
Prior to Veeco SPM training you need to discuss your project with staff to ensure your needs can be
met with the tool. There are two scanners available:
1. 10 × 10 µm (XY) and 2.5 µm (Z) : E scanner - standard
2. 125 × 125 µm (XY) and 5.0 µm (Z) : J scanner - additional training required
In addition, to become authorized you must:
• Complete training with SPM staff. For further documentation see D:\Manuals.
• Have your own AFM tips to use.
• Have your own sample to measure (must fit in an area < 10 × 10 mm).
• Have your own tweezers for mounting tips and samples.
Nano3 is able to supply HQ:NSC15/AL BS AFM tips which have a manufacturers stated resonance
frequency of 325 kHz and spring constant 40 N/m. The cost is $18 per tip. You must have your
own gel pack storage to purchase these tips.
8.2 Computer and Software
PC credentials:
• Username: nano3user
• Password: 123nano3
For offline data analysis you are free to copy the software from D:\Manuals\Software. We recom-
mend using NanoScope Analysis. Select ‘offline’ during installation. Also a free, open source SPM
analysis software called Gwyddion is available from http://gwyddion.net.
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42 Chapter 8. Veeco Scanning Probe Microscope
8.3 Standard Operating Procedure - Tapping Mode
The default scanner is the E scanner, allowing up to 10 × 10 µm2 . Additional training is required to
user other scanners.
1.
Log into your FOM user account, activate Veeco SPM from the calendar.
2.
Begin an entry in the paper log book.
3.
Ensure PC is on.
4.
Turn on controller with switch (back right of unit).
5.
Turn on optical microscope light source
Open Nanoscope software V614r1.
6.
7.
File/Open Workspace. For tapping mode: default_tapping_mm.wks.
Click ‘Scan-Dual’ and ‘Scan ParmList’ from the left pannel to bring up interface. This will
8.
take a few moments.
9. Check the scanner that is installed in the workspace from ‘Scan ParmList’, ‘Serial number’ :
9991EVLR (E scanner) and that it matches the scanner on the machine.
10. Load sample.
• Mount sample on metal disk with carbon tape. The disks are found in the top drawer.
Ensure area of interest is roughly in the center of this disk.
• Ensure back side of metal disk is clean and residue free.
• Remove head by releasing the springs on the left and right sides of the head and
disconnect the power cable.
• Mount sample on piezo stage. The stage is magnetic, so resting your sample on top
will secure your sample magnetically.
• Replace head. Ensure the springs secure the head in place and the power cable is
reconnected.
Important Never attach your sample directly to the piezo stage. This is the most sensitive part
of the AFM and you risk destroying the scanner.
Figure 8.1: Tip Holder. AFM tip seated correctly in holder. Inset: Magnified view of tip placement.
Notice the secured end (left edge) is flush with the metal holder.
11. Load AFM tip into holder. See Fig. 8.1. Flip the tip holder upside down onto the table top.
Press down lightly to open holder spring. Slide AFM tip into the holder ensuring the it is
properly nestled. Gently release downward pressure to secure tip in holder. Practice this
procedure with old tips.
12. Load holder into head and secure. To avoid the AFM tip crashing onto your sample surface
ensure the metal mounting spheres are higher than you sample, see Fig. 8.3. To secure see 4
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8.3 Standard Operating Procedure - Tapping Mode 43
in Fig. 8.2.
13. Align laser to cantilever end. The goal is to adjust X-Y laser placement so that laser is
incident on AFM tip end. See 2 in Fig. 8.2. Use the following techniques to align the laser
correctly.
• Optical microscope: can be used to detect faint reflections from the sample surface to
give a rough indication of laser position. Make sure you are focused on the reflection
of the cantilever for most accurate alignment.
• Paper strip: Following the path of the laser inside the head can give a very rough
indication of laser position.
• ‘SUM’ readout: If the mirror is already in a good position or the AFM was left in a
good condition the laser may be closely aligned already. Simply adjusting the X-Y
positioning to obtain maximum ‘SUM’ may be all that is required.
• Shadow method: With the head removed, project the laser onto a white surface. This
is the best way to get very fine alignment. Good alignment will be when the laser is
blocked by the end cantilever. Fine adjustments to the Y positioning in either direction
should result in an increase of laser intensity (i.e. laser transverses cantilever). Fine
adjustments to the X positioning will only result in an increase of laser intensity in one
direction (i.e. when the laser is moves off the end of the tip).
14. Align photodetector to reflected beam. See 5 and 6 in Fig. 8.2
• Use left switch on AFM base to select ‘AFM & LFM’ mode. This changes the digital
read-out.
• Adjust mirror to maximize ‘SUM’ readout. The exact readout will depend on tip type
and laser alignment. For standard tips aim for SUM> 5 but this may very. Understand
that the specific number is not important - higher simply means more signal of the
reflected beam is captured by the photodetector.
• Adjust detector placement to obtain close to zero ‘VERT’ and ‘HORIZ’ readout. This
should always be set to close to zero. Zero along both axis means the beam is centered
within the photodetector.
• Use left switch of AFM base to select ‘TM AFM’ mode for tapping.
Tip Most issues with the AFM can be solved by checking the laser alignment and/or restarting
the controller and software.
Figure 8.2: Veeco SPM head. Front a) and Back b) view. 1. AFM tip holder 2. X-Y Laser
positioning dials 3. X-Y Translation for coarse cantilever positioning (not needed for aligning laser
or detector) 4. Tip holder release/secure 5. Laser mirror for ‘SUM’ maximization 6. Detector
positioning dials for ‘VERT’ and ‘HORIZ’ alignment.
15. Align optical microscope above head to find cantilever. You may need to adjust the stage
positioning.
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44 Chapter 8. Veeco Scanning Probe Microscope
Figure 8.3: Tip holder mount rests. Arrows indicate the position of three metal spheres where the
AFM tip holder rests. Ensure the top of the spheres are above the sample surface. Adjust with the
’Up’ or ’Down’ switch on AFM base
16. Confirm that you can focus on sample to ensure you are close enough to regions of interest.
Otherwise you will have to remount sample.
17. Click Tune button (blue tuning fork: ). You need to do this when the tip is far away from
sample.
• A new window will pop up. The default parameters are typically okay. If you are using
your own tips ensure the resonant frequency is will be captured by the sweep. Default
0 − 500 kHz.
• Click Auto Tune button (lower left). This measures the vibration frequency of the tip
and sets some default parameters. Make sure you retrieve a nice resonant peak and
backwards ‘s’ shape in phase (See. Fig. 8.4) otherwise you will have to either adjust
laser alignment or replace tip.
• Click Exit button. This will save the measured properties of the cantilever to your
workspace.
• If auto tune times out check the laser alignment. If laser alignment is okay, you may
have to restart the controller and software.
18. Focus on the sample surface with the optical microscope and manually approach tip close
to sample surface using ‘Down’ switch on base of AFM. Be sure to avoid large junk on the
surface. Approach until the cantilever is just out of focus.
Figure 8.4: Typical Auto tune results. Top: Amplitude vs. Drive Frequency. Bottom: Phase vs.
Drive Frequency
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8.3 Standard Operating Procedure - Tapping Mode 45
Important Be careful approaching tip manually with switch. It is possible to crash the tip into
the surface, potentially damaging your sample and tip.
19. Navigate tip close to region of interest using X-Y Translation dials (see 3 in Fig. 8.2)
20. Close cabinet to reduce noise and vibrations.
21. Setup initial scan parameters in software.
• Scan size. Up to ∼ 10 × 10 µm2 for E scanner. Start Small.
• Aspect ratio: 1.00 for a square image.
• X and Y Offset: Initialize to 0.
• Scan angle: 0◦
• Scan Rate: 1 Hz or less for initial optimization.
• Samples/Line: Recommended 128 or less for initial optimization.
• Lines: Same as Samples/Line for equal resolution in both dimensions.
• Slow scan: Enabled for 2D images.
22. Click Engage button . If you see a message ‘Z limit has been reduced’ click Yes. The
AFM will carefully approach surface and start scanning and give you an image line by line.
23. Adjust feedback parameters to achieve best image to improve image quality. The goal is to
get trace and retrace lines as similar as possible and the phase to be as flat as possible (phase
contrast should only occur at topographical boundaries or changes of material stiffness). With
the feedback parameter highlighted you can use the left/right arrow keys on the keyboard for
fine adjustments.
• If it seems as if the tip is not in true contact with your sample decrease the amplitude
setpoint. This will bring the cantilever closer to the sample. Note that decreasing
excessively may damage your sample.
• Increase integral gain as much as possible without getting oscillations. Initial ∼ 0.4.
Typically set no higher than 1 − 2.
• Increase proportional gain as much as possible without getting oscillations. Initial
∼ 1. Should be higher than Integral gain.
• Only increase integral and proportional gains if they improve image. Otherwise leave
at default.
• Lower scan rate.
Tip If you have trouble optimizing the image, disable slow scan whenever the tip is traversing a
feature. This stops the scanning in one direction so that the tip traces and retraces the same line
over and over. Adjust the feedback parameters in this state.
Tip Particularly for new and unknown sample types, it is advisable to image somewhere arbitrary
on the sample surface to determine optimum feedback parameters. When you have got a ‘feel’
for how the tip-sample interaction behaves, retract tip and engage near region of interest slowly
approaching using X and Y offset in the scan parameters.
24. Capture Images.
• Use the ‘RealTime’ dropdown from the menu bar to select ‘capture filename’ and
navigate to the directory you want to save to.
• Using a filename that ends in ‘.001’ will automatically count upwards for each subse-
quent capture.
• Increase scan resolution if desired (Samples/Line and Lines). Optimizing feedback
parameters may be required.
• Click Capture button to enable capture. This will save raw data after frame
completes. The software will only save a full frame if no scan settings were changed
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46 Chapter 8. Veeco Scanning Probe Microscope
during image acquisition.
25. Repeat for other regions of interest. Remember to withdraw the tip each time you want to
explore a new area.
Tip After extended periods of imaging or imaging dirty samples, the tip quality may degrade
from damage or contamination. For the best data it may be necessary to replace tip.
26. When complete, return AFM to starting configuration.
• Click Withdraw button: . Wait for at bottom right.
• Raise tip far from sample using ‘Up’ switch on base.
• Remove AFM tip holder and remove tip.
• Remove samples and return metal disks.
• Replace AFM tip holder and secure.
• Close software, and do not save changes to workspace unless they are your own.
• Turn off controller.
• Turn off optical microscope light source.
• Close Cabinet.
27. Finish paper logbook entry and log out of tool with FOM.
28. Collect images/data from data PC. Note the D: drive is not permanent storage and data may
be removed. Collect all important files ASAP.
8.4 Contact Mode and Nanoindentation
8.4.1 Contact imaging
1. Complete steps 1 through 16 in Section 8.3 with the following considerations:
• Load the contact workspace instead: default_contact_mm.wks.
• Aligning the laser, mirror, and photodetector steps are all the same except you should
adjust the ‘VERT’ reading to be ∼ −2, this gives the detector a greater range to sense
the cantilever deflection (we zero this in tapping mode since the cantilever is oscillating
around an equilibrium point, but contact mode is based on deflection of the cantilever,
typically in one direction only).
• Keep the left switch on AFM base to ‘AFM & LFM’ mode.
• No tuning is required.
2. Begin scanning following steps 18 to 22 in Section 8.3.
3. Adjust feedback parameters to achieve best image to improve image quality. The goal is to
get trace and retrace lines as similar as possible. With the feedback parameter highlighted
you can use the left/right arrow keys on the keyboard for fine adjustments.
• If it seems as if the tip is not in true contact with your sample increase the deflection
setpoint. This will bring the cantilever closer to the sample. Note that increasing
excessively may damage your sample.
• Increase integral gain as much as possible without getting oscillations. Initial ∼ 2.
• Increase proportional gain as much as possible without getting oscillations. Initial
∼ 5. Should be higher than Integral gain.
• Only increase integral and proportional gains if they improve image. Otherwise leave
at default.
• Lower scan rate.
4. Capture Images. When complete return AFM to starting configuration as described in steps
24 through 28 in Section 8.3.
5. When complete, return AFM to starting configuration following steps 26 to 28 in Section 8.3.
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8.4 Contact Mode and Nanoindentation 47
8.4.2 Nanoindentation
This section describes how to use the AFM to probe your samples mechanical properties by poking
it in one location. Analysis of this data to extract material parameters will depend on your own
literature research and fitting. Note that ramping on your sample with an AFM tip will give you
Deflection (of the AFM tip) vs. Z (piezo stage movement), which in general describes the sum of
two springs in series (cantilever response + material response). See Fig. 8.5 for an example ramp.
Therefore, you must first perform an experiment on a substrate much stiffer than your cantilever to
calibrate its sensitivity which will subsequently allow you to isolate the material response from
your data.
1. Initialize AFM in contact mode as described in Section 8.4.1 to obtain image of sample
surface. The AFM tip must be engaged before proceeding to the next step.
2. To switch to indentation mode, open ‘Ch1 Ramp Plot’ and ’Ramp Parameter List’ from the
left panel. The AFM will stop scanning and be ready for indentation or ‘ramping’.
3. Adjust ramp settings
• Ramp size. Up to 2 µm . Start at ∼ 100 − 200 nm.
• Scan rate: Start at ∼ 1 Hz. This setting may be important for polymers which may
show viscoelasticity and plastic deformation.
• X and Y Offset: Initialize to 0 (ramp will occur where the tip is placed).
• Number of samples: 1024. This is the number of data points on your curve.
• Spring constant. Enter the spring constant of your AFM cantilever.
4. Adjust ramp mode
• Trigger mode controls when the AFM will stop ramping in conjunction with Trig
threshold (below). It must be set to relative or absolute to be enabled. Relative means
the ramp will stop when the cantilever reaches the Trig threshold value relative to
the base line (e.g. above ‘VERT’=−2). Absolute means the ramp will stop when the
cantilever reaches the Trig threshold above 0.
• Trig threshold is the limit of cantilever deflection. The higher this number is, the more
the AFM will indent into your sample. Trig threshold must be less than Ramp size to
ensure you capture all the data.
5. Perform ramp. See an example ramp on a polymer in Fig. 8.5.
• Click: for a single ramp measurement.
• Adjust settings as described in steps 3 and 4 as necessary.
6. Capture data
• Use the ‘RealTime’ dropdown from the menu bar to select ‘capture filename’ and
navigate to the directory you want to save to.
• Click Capture button to save the ramp data.
7. To ramp at a specific location, first ensure the AFM is scanning your sample, then choose
‘Point and Shoot’ from the left panel. This will open a new window.
• Choose ‘Main Scope Mode’ to be ‘Image/Scan’ and wait for the image to scan.
• Then choose ‘Main Scope Mode’ to be ‘Ramp/Force Curve’.
• In ‘Image Cursor Mode’ choose ‘M/Ramp’. This means ‘Mark and Ramp’. As soon as
you click on the image, it will mark that location and automatically ramp there using
your ’Ramp Parameter List’ settings.
• The same data is available to view and capture in the ‘Ch1 Ramp Plot’ window.
8. When complete, return AFM to starting configuration following steps 26 to 28 in Section 8.3.
Tip For the highest sensitivity measurement it is recommended to use cantilevers with a spring
constant commensurate with the stiffness of your sample.
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48 Chapter 8. Veeco Scanning Probe Microscope
Figure 8.5: Raw ramp/nanoindentation data on a polymer. Ramp size is the overall data range and
Trig threshold controls the force applied to the material. Deflection (y-axis) is how far the cantilever
bends not how far the tip pushes into the sample. If you open ramp data in the Nanoscope analysis
software and correctly enter spring constant (k) and sensitivity (slope of the ramp data on a very
stiff substrate), then you can plot there data as Force vs. Separation. Force is simply F = −kd,
where d is the deflection. Separation (s) is the distance the tip pushes into the sample s = Z − d
where Z is the ramp coordinate.
Tip There are an number of uncertainties to be aware of. The range of spring constant values
for cantilevers of a given type can be quite large. We do not have the capability to independently
measure the spring constant on the Veeco SPM, however it may be possible to purchase pre-
calibrated cantilevers that have spring constants of high certainty. Also, the AFM tip is very
fragile, and although it has a very small radius initially, many indentation tests will quickly
damage and blunt the tip. One way to mitigate this is to use very tough tips, e.g. diamond
coated.
8.5 J Scanner installation - Additional Training Required
The J scanner (10488JNM) allows for scans up to 100 × 100 µm2 . However, there are two
important points about using this scanner. First, the scanner platform is non-magnetic meaning this
is the only instance which you may apply carbon tape to the scanner (see step 10). Second, the
scanner z is controlled by two manual dials in conjunction with the usual up/down switch.
1. Ensure PC is on.
2. Turn on controller with switch (back right of unit).
3. Turn on optical microscope light source
4. Open Nanoscope software V614r1.
5. File/Open Workspace. For tapping mode: default_tapping_mm.wks.
6. Click ‘Scan-Dual’ and ‘Scan ParmList’ from the left pannel to bring up interface. This will
take a few moments.
7. Remove scanner head entirely (remove springs and disconnect cable).
8. Remove E scanner by disconnecting cable and lifting gently from stage.
Important Always store unused scanner in padded box located in the drawer.
9. Install J Scanner. See Fig. 8.6.
• Gently place the scanner on the stage. You must align the pin and the socket correctly.
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8.5 J Scanner installation - Additional Training Required 49
If they are not aligned then use the up/down switch to rotate the socket. The scanner
should rest securely on the stage.
• Connect J scanner cable to the stage.
• Install both springs. An example is shown in Fig. 8.6 d).
• Navigate to Tool/Select Scanner and choose 10488JNM. The software will need to
reload the workspace. Do not save the workspace unless it is your own.
• Confirm that the J scanner is installed correctly in the workspace by checking the ‘Serial
Number’ in the ‘Scan ParmList’. It should be updated to read 10488JNM.
10. Load sample.
• Mount sample on metal disk with carbon tape. The disks are found in the top drawer.
Ensure area of interest is roughly in the center of this disk.
• Apply a small amount of carbon tape to the back side of the metal disk
• Remove head by releasing the springs on the left and right sides of the head and
disconnect the power cable.
• Mount sample on piezo stage by gently resting the disk on top. Do not apply excessive
pressure to adhere the sample.
• Replace head. Ensure the springs secure the head in place and the power cable is
reconnected.
Important Never place carbon tape directly on the piezo stage. Always attach to the metal
disk first. Be very careful when adhering your sample disk to the piezo stage. This is the most
sensitive part of the AFM and you risk destroying the scanner.
11. Follow steps 11 to 17 in Section 8.3 to align laser and tune cantilever.
Important The head often sits higher on the J scanner than the E scanner. Be careful when
swivelling the optical microscope to and from the AFM to avoid hitting the objective.
Tip Prior to alignment, it might be useful to approach the tip closer to the surface so that you
can use the cantilever reflection for guidance. See approach instructions in step 12.
12. Approach sample surface. You must use the up/down switch on AFM base and the two dials
on the scanner to accomplish this:
• Use optical microscope to focus on sample surface.
• Look at the scanner head and determine if it is level (e.g. if it is tilted left/right or
back/front). Use the up/down switch and dials to level.
• The best technique to approach the tip to the sample surface is to cycle between first
holding the down switch (which will tilt the head backwards) and then turning both dials
on the front in the same direction (which will tilt the head forwards). This ‘rocking’
type approach will allow you to keep the tip in the vicinity of your region of interest.
• While you approach you will notice that the tip will travel in the ±y direction depending
on which way the head is tilting. This is normal.
• Continue this approach method until the cantilever is just out of focus. Pay particular
attention to the head to ensure that it is almost level when your approach is complete. It
is advisable to have the head tilted slightly towards you because the final approach in
the software will only control the socket (up/down switch).
13. Navigate tip close to region of interest using X-Y Translation dials (see 3 in Fig. 8.2).
14. Close cabinet to reduce noise and vibrations.
15. Setup initial scan parameters in software.
• Scan size. Up to ∼ 100 × 100 µm2 for J scanner. Start Small.
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50 Chapter 8. Veeco Scanning Probe Microscope
Figure 8.6: J scanner. a) Top of the J scanner looks the same as the E scanner. It has 3 metal
mountings spheres. For the E scanner the up/down switch controls all spheres simultaneously.
However for the J scanner each sphere is controlled separately. b) Bottom of the J scanner shows
two additional dials not present on the E scanner. The two dials control the vertical positions of the
two front metal mounting spheres. The back metal mounting sphere is controlled by the pin. c)
Empty Veeco SPM stage showing the up/down switch driving socket. The up/down switch turns
this socket. When the scanner is in place correctly, the pin is engaged with this socket. This is
how the back metal mounting sphere is controlled by the switch. d) Proper installation of J scanner
springs.
• Aspect ratio: 1.00 for a square image.
• X and Y Offset: Initialize to 0.
• Scan angle: 0◦
• Scan Rate: 1 Hz or less for initial optimization.
• Samples/Line: Recommended 128 or less for initial optimization.
• Lines: Same as Samples/Line for equal resolution in both dimensions.
• Slow scan: Enabled for 2D images.
16. Click Engage button . If you see a message ‘Z limit has been reduced’ click Yes. The
AFM will carefully approach surface. Note that since the software only controls the up/down
switch socket, the head will tilt backwards during approach and the tip will move upwards
with respect to the sample surface.
17. Adjust feedback parameters and capture images as in steps 23 to 25 in Section 8.3.
Tip For large scan areas it may not be possible to optimize the feedback so that trace and retrace
lines are identical. Adjust the feedback so that common features in the trace and retrace lines
are close to one another.
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8.5 J Scanner installation - Additional Training Required 51
Tip Pay particular attention to the bar on the right which indicates the extension and retraction
limits of the scanner. The scanner can only move in a vertical range of ∼ 5 µm. For large scan
sizes a small tilt angle can cause a large difference in height from one end of the sample to the
other. If you cannot scan your entire region of interest you must withdraw the tip and level the
scanner head.
18. When complete, return AFM to starting configuration. Change the scanner back to E.
• Click Withdraw button: . Wait for at bottom right.
• Raise tip far from sample. First use the ‘Up’ switch on base, then the dials. Cycle using
the switch and the dials until the tip is far from the sample (i.e. reverse of step 12).
• Remove AFM tip holder and remove tip.
• Remove Head completely by removing springs and disconnecting the power cable.
• Remove samples and return metal disks. Be careful when removing the metal disk from
the J scanner stage.
• Disconnect J scanner and remove from the system. Don’t forget to remove the springs.
Store securely in padded box.
• Replace E scanner and reconnect cable.
• Replace Head.
• Replace AFM tip holder and secure.
• Navigate to Tool/Select Scanner and choose 9991EVLR. The software will need to
reload the workspace. Do not save the workspace unless it is your own.
• Confirm that the E scanner has been correctly installed in the software by checking the
serial number.
• Close software, and do not save changes to workspace unless they are your own.
• Turn off controller.
• Turn off optical microscope light source.
• Close Cabinet.
19. Finish paper logbook entry and log out of tool with FOM.
20. Collect images/data from data PC. Note the D: drive is not permanent storage and data may
be removed. Collect all important files ASAP.
Important Always return the AFM to the default configuration by reinstalling the E scanner
hardware and selecting the scanner in the software.
Last Updated: July 11, 2018
