Bruker 004-130-000 Manual
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Bruker 004-130-000 Manual

Bruker 004-130-000 Manual

Spm training notebook
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Document Revision History: SPM Training Notebook
Revision
Date
Rev. F
01/28/2011
Rev. E
10/27/2003
Rev. D
08/05/2003
Rev. C
07/30/2003
Rev. B
08/01/1998
Rev. A
05/09/1997
SPM Training Notebook
004-130-000 (standard)
004-130-100 (cleanroom)
Copyright © 2003, 2011 Bruker Corporation
All rights reserved.
Section(s) Affected
Re-branded
Content and Format Update
Overall Content and Format Update
Content Update
Format Update
Initial Release
Reference
Approval
R.Wishengrad
N/A
C. Kowalski
N/A
L. Burrows
N/A
L. Burrows
N/A
C. Fitzgerald
N/A
J. Thornton

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  • Page 1 SPM Training Notebook 004-130-000 (standard) 004-130-100 (cleanroom) Copyright © 2003, 2011 Bruker Corporation All rights reserved. Document Revision History: SPM Training Notebook Revision Date Section(s) Affected Reference Approval Rev. F 01/28/2011 Re-branded R.Wishengrad Rev. E 10/27/2003 Content and Format Update C.
  • Page 2 Copyright: Copyright © 2003, 2011 Bruker Corporation. All rights reserved. Trademark Acknowledgments: The following are registered trademarks of Bruker Corporation. All other trademarks are the property of their respective owners.

  • Page 3: Table Of Contents

    Table of Contents 1.0 History and Definitions in SPMs ....... . 3 1.1 History .
  • Page 4 13.0 SPM Configurations ........26 14.0 Abbreviated Instructions for Dimension Series AFMs.
  • Page 5 SPM Training Notebook This Notebook is intended to be used as an introduction by the first-time user of Bruker NanoScope Scanning Probe Microscopes (SPM). For further information, please consult the Command Reference Manual and/or the appropriate NanoScope manual. Specifically, this manual covers the following: •...
  • Page 6 • Offline Operation: Page 44 • Tip Shape Issues: Page 53 • Typical Image Artifacts: Page 58 • Calibration: Page 62 Scanning Probe Microscope Training Notebook Rev. F...

  • Page 7: History And Definitions In Spms

    History and Definitions in SPMs History and Definitions in SPMs History Scanning Tunneling Microscope (STM) • Developed in 1982 by Binning, Rohrer, Gerber, and Weibel at IBM in Zurich, Switzerland. • Binning and Rohrer won the Nobel Prize in Physics for this invention in 1986. Atomic Force Microscope (AFM) •...

  • Page 8: Other Forms Of Spm

    History and Definitions in SPMs Other forms of SPM: Lateral Force Microscopy (LFM) Force Modulation Microscopy Magnetic Force Microscopy (MFM) Electric Force Microscopy (EFM) Surface Potential Microscopy Phase Imaging Force Volume Electrochemical STM & AFM (ECM) Scanning Capacitance Microscopy (SCM) Scanning Thermal Microscopy (SThM) Near-field Scanning Optical Microscopy (NSOM or SNOM) Scanning Spreading Resistance (SSRM)

  • Page 9: Scanning Tunneling Microscope

    Scanning Tunneling Microscope Scanning Tunneling Microscope Rev. F Scanning Probe Microscope Training Notebook...
  • Page 10 Scanning Tunneling Microscope Figure 2.0a Feedback Loop Maintains Constant Tunneling Current STM is based on the fact that the tunneling current between a conductive tip and sample is exponentially dependent on their separation. This can be represented by the equation: I ~ Ve •...

  • Page 11: Applications

    Scanning Tunneling Microscope Applications • Atomic resolution imaging (STM is the only technique which detects atomic-scale defects) • Electrochemical STM • Scanning Tunneling Spectroscopy • Low-current imaging of poorly conductive samples Rev. F Scanning Probe Microscope Training Notebook...

  • Page 12: Contact Mode Afm

    Contact Mode AFM Contact Mode AFM Figure 3.0a Feedback Loop Maintains Constant Cantilever Deflection Contact mode AFM operates by scanning a tip attached to the end of a cantilever across the sample surface while monitoring the change in cantilever deflection with a split photodiode detector. The tip contacts the surface through the adsorbed fluid layer on the sample surface.
  • Page 13 Contact Mode AFM The force is calculated from Hooke's Law: where: – • F = Force • k = spring constant • x = cantilever deflection. Force constants usually range from 0.01 to 1.0 N/m, resulting in forces ranging from nN to µN in an ambient atmosphere.

  • Page 14: Tappingmode Afm

    TappingMode AFM TappingMode AFM Figure 4.0a Feedback Loop Electronics TappingMode AFM operates by scanning a tip attached to the end of an oscillating cantilever across the sample surface. The cantilever is oscillated at or slightly below its resonance frequency with an amplitude ranging typically from 20nm to 100nm.

  • Page 15: Non-Contact Mode Afm

    Non-contact Mode AFM Non-contact Mode AFM Figure 5.0a Feedback Loop Maintains Constant Oscillation Amplitude or Frequency The cantilever is oscillated at a frequency which is slightly above the cantilever’s resonance frequency typically with an amplitude of a few nanometers (<10nm), in order to obtain an AC signal from the cantilever.

  • Page 16: Advantages And Disadvantages Of Contact Mode Afm, Tappingmode Afm, And Non-Contact Mode Afm

    Advantages and Disadvantages of Contact Mode AFM, TappingMode AFM, and Non-contact Mode AFM Advantages and Disadvantages of Contact Mode AFM, TappingMode AFM, and Non-contact Mode AFM Contact Mode AFM Advantages: • High scan speeds (throughput). • Contact mode AFM is the only AFM technique which can obtain “atomic resolution” images.

  • Page 17: Non-Contact Mode Afm

    Advantages and Disadvantages of Contact Mode AFM, TappingMode AFM, and Non-contact Mode AFM Non-contact Mode AFM Advantage: • No force exerted on the sample surface. Disadvantages: • Lower lateral resolution, limited by the tip-sample separation. • Slower scan speed than TappingMode and Contact Mode to avoid contacting the adsorbed fluid layer which results in the tip getting stuck.

  • Page 18: Piezoelectric Scanners: How They Work

    Piezoelectric Scanners: How They Work Piezoelectric Scanners: How They Work SPM scanners are made from piezoelectric material, which expands and contracts proportionally to an applied voltage. Whether they elongate or contract depends upon the polarity of the voltage applied. All DI scanners have AC voltage ranges of +220V to -220V for each scan axis.
  • Page 19 Piezoelectric Scanners: How They Work Figure 7.0c Waveforms applied to the piezo electrodes during a raster scan with the X axis designated as the fast axis (Scan Angle = 0°) Schematic of piezo movement during a raster scan. Voltage applied to the X- and Y-axes produce the scan pattern.

  • Page 20: Piezoelectric Scanners: Hysteresis And Aging

    Piezoelectric Scanners: Hysteresis and Aging Piezoelectric Scanners: Hysteresis and Aging Hysteresis Because of differences in the material properties and dimensions of each piezoelectric element, each scanner responds differently to an applied voltage. This response is conveniently measured in terms of sensitivity, a ratio of piezo movement-to-piezo voltage, i.e., how far the piezo extends or contracts per applied volt.
  • Page 21 Piezoelectric Scanners: Hysteresis and Aging Figure 8.1b 100mm x 100mm scans in the forward (trace) and reverse (retrace) directions of a two-dimensional 10mm pitch grating without linearity correction. Both scans are in the down direction. Notice the differences in the spacing, size, and shape of the pits between the bottom and the top of each image. The effect of the hysteresis loop on each scan direction is demonstrated.

  • Page 22: Aging

    Piezoelectric Scanners: Hysteresis and Aging Aging Time The sensitivity of piezoelectric materials decreases exponentially with operation time. This causes most of the change in the sensitivity to occur at the beginning of a scanner's life, as shown in the graph to the left. Scanners are run approximately 48 hours before they are shipped from the factory to get the scanner past the point where the sensitivity changes dramatically over short periods of time.

  • Page 23: Piezoelectric Scanners: Creep And Bow

    Piezoelectric Scanners: Creep and Bow Piezoelectric Scanners: Creep and Bow Creep Creep is the drift of the piezo displacement after a DC offset voltage is applied to the piezo. This may occur with large changes in X & Y offsets, and when using the frame up and frame down commands when the piezo travels over most of the scan area to restart the scan.

  • Page 24: Bow

    Piezoelectric Scanners: Creep and Bow Because scanners are attached at one end and move the sample or tip on the other, the free end does not move in a level plane. The mechanical properties of the piezo, as well as the kinematics of motion, often result in 2nd order or 3rd order curvatures from an ideal plane.

  • Page 25: Probes

    Probes 10.0 Probes 10.1 Silicon Nitride Silicon nitride probes consist of a cantilever integrated with a sharp tip on the end. The properties and dimensions of the cantilever play an important role in determining the sensitivity and resolution of the AFM. For contact mode AFM imaging, it is necessary to have a cantilever which is soft enough to be deflected by very small forces (i.e.

  • Page 26: Silicon

    Probes 10.2 Silicon Silicon probes are used primarily for TappingMode applications. The tip and cantilever are an integrated assembly of single crystal silicon, produced by etching techniques. Only 1 cantilever and tip are integrated with each substrate. These probes can be much stiffer than the silicon nitride probes, resulting in larger force constants and resonant frequencies.

  • Page 27: Types Of Spm Probes

    Types of SPM Probes 11.0 Types of SPM Probes 11.1 Contact Mode Probes • Standard Silicon Nitride Probe (described previously) • Oxide-Sharpened Silicon Nitride (Standard) Probes • Oxide-Sharpened Silicon Nitride Oriented Twin Tip Probes • Olympus Oxide-Sharpened Silicon Nitride Probes •...
  • Page 28 • DDESP - Doped diamond-coated Si probes, with medium to high spring constant For a listing and description of SPM probes available from Bruker Corporation please go to: www.bruker.com > Products > AFM/SPMs/NSOMS > Buy SPM Probes > Probes. Scanning Probe Microscope Training Notebook...

  • Page 29: Atomic Force Microscopy- "Beam Deflection" Detection

    Atomic Force Microscopy- “Beam Deflection” Detection 12.0 Atomic Force Microscopy- “Beam Deflection” Detection Solid State Laser Diode Output: A-B Split Photodiode Detector Cantilever and Tip Used for Contact Mode AFM, Non-contact Mode AFM, and TappingMode AFM. This is the most widely used form of cantilever 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...

  • Page 30: Spm Configurations

    SPM Configurations 13.0 SPM Configurations Figure 13.0a Scanned Tip SPM Figure 13.0b Scanned Sample SPM Labels: 1. Laser 2. Mirror 3. Cantilever 4. Tilt mirror 5. Photodetector Scanning Probe Microscope Training Notebook Rev. F...
  • Page 31 SPM Configurations Figure 13.0c Feedback Loop- Contact Mode 62.5 KHz Rev. F Scanning Probe Microscope Training Notebook...
  • Page 32 SPM Configurations Figure 13.0d Feedback Loop- Tapping Mode 62.5 KHz Scanning Probe Microscope Training Notebook Rev. F...

  • Page 33: Abbreviated Instructions For Dimension Series Afms

    Abbreviated Instructions for Dimension Series AFMs 14.0 Abbreviated Instructions for Dimension Series AFMs 14.1 Mode of Operation 1. In the Other Controls panel, set the AFM Mode to Tapping or Contact, or select Microscope > Profile and then the appropriate mode. 2.

  • Page 34: Focus Surface

    Abbreviated Instructions for Dimension Series AFMs 14.5 Focus Surface 1. Select Stage > Focus Surface (or click the Focus Surface icon). The optics will move to a focus position approximately 1mm below the tip. Focus on the sample surface by rolling the trackball up or down while pressing the bottom left button.

  • Page 35: Adjust Scan Parameters

    Abbreviated Instructions for Dimension Series AFMs 14.9 Adjust Scan Parameters Tapping 1. Select View > Scope Mode (or click on the Scope Mode icon). 2. Check to see if Trace and Retrace are tracking each other well (i.e. look similar). If they are tracking, the lines should look the same, but they will not necessarily overlap each other, either horizontally or vertically.

  • Page 36: Abbreviated Instructions For The Multimode Afm

    Abbreviated Instructions for the MultiMode AFM 15.0 Abbreviated Instructions for the MultiMode AFM 15.1 Mode of Operation In the Other Controls panel, set AFM Mode to Tapping, Contact, or choose the appropriate profile and change the mode switch on the base to TMAFM or AFM & LFM mode, respectively. 15.2 Mount Probe 1.

  • Page 37: Align Laser And Tip-Sample Approach (2 Methods)

    Abbreviated Instructions for the MultiMode AFM 15.6 Align Laser and Tip-Sample Approach (2 Methods) 1. Magnifier Method for Aligning Laser and Tip-Sample: a. Focus on the side-view of the cantilever with the magnifier. If you are having trouble finding the cantilever, try searching for the red light of the laser and focus on that. Use the “paper method”...

  • Page 38: Adjust Photodiode Signal

    Abbreviated Instructions for the MultiMode AFM 15.7 Adjust Photodiode Signal Note where the laser reflection enters the photodiode cavity. If necessary, adjust the mirror (lever on back of optical head) to center the laser reflection into the photodiode cavity. Leave the mirror at an angle such that the SUM signal (circular meter in bottom LCD) is maximized.

  • Page 39: Adjust Scan Parameters

    Abbreviated Instructions for the MultiMode AFM 15.11 Adjust Scan Parameters Tapping a. Select View > Scope Mode (or click on the Scope Mode icon). Check to see if the Trace and Retrace lines are tracking each other well (i.e. look similar). If they are tracking, the lines should look the same, but they will not necessarily overlap each other, either horizontally or vertically.

  • Page 40: Realtime Operation

    Realtime Operation 16.0 Realtime Operation The Realtime parameters are located in the control panels which are available in the Panels pull down menu. The main control panels for topographic imaging are “Scan controls,” “Feedback Controls,” “Other Controls,” and “Channel 1.” There are three primary feedback parameters that need adjusting every time you engage the microscope to capture an image in TappingMode AFM or Contact Mode AFM: Setpoint, Integral Gain, and Scan Rate.

  • Page 41: Integral Gain

    Realtime Operation Figure 16.1a Scope Trace Demonstrating the Effect of the Setpoint Being Adjusted Too Close to the Free Air Amplitude During TappingMode AFM Notice that the tip tracks the surface up the sidewall properly but not down the sidewall with respect to the scan direction.

  • Page 42: Scan Rate

    Realtime Operation Figure 16.2b Scope Trace Demonstrating the Effect of Setting the Integral Gain Too Low Set the Integral Gain as high as possible by increasing the gain until noise is seen, then reduce the gain just lower than the value where the noise disappears. 16.3 Scan Rate The Scan Rate is the number of trace and retrace scan lines performed per second (Hz).

  • Page 43: Other Important Parameters

    Realtime Operation The Scan Rate setting will greatly depend on the scan size and the height of the features being imaged. In general, the taller the features and/or the larger the scan size, the slower the scan rate. Typical Scan Rate settings are 0.5 to 2.0Hz for TappingMode and 1 to 4Hz for Contact Mode. 16.4 Other Important Parameters Scan Size: Adjusts the size of the X,Y scan area...
  • Page 44 Realtime Operation Z-Center Position: The Z-center voltage scale is located to the right side of the image on the display monitor. It represents the current extension or retraction of the Z piezo electrode of the scanner during operation. • It is displayed from -220V to +220V (440V full range) which represents the entire vertical travel of the scanner (i.e.
  • Page 45 Realtime Operation The Full setting is commonly used for everyday imaging. However, the Offset setting can be useful when a first order planefit would negatively affect the measurement of interest. This can be demonstrated in the example below. If the measurement of interest is the height of the step, then setting the Offline Planefit to Full will result in the tilting of the data.

  • Page 46: Force Curves

    Force Curves 17.0 Force Curves Force curves are commonly used to set the imaging force in contact mode and to study attractive, repulsive, and adhesive interactions between the tip and the sample. The Realtime menu for obtaining force curves is found under View > Force Mode > Calibrate. When a force curve is acquired, the lateral (X and Y) movement of the scanner is stopped, and the scanner extends and retracts the Z electrode of the scanner.
  • Page 47 Force Curves The imaging force may be set by using the Setpoint parameter to determine where the sloped portion of the curve (points C & D) intersects the green, horizontal Setpoint line in the center of the graph. • The force may be calculated by Hooke’s Law, F = -kx, where F= force, k = spring constant, and x = deflection.

  • Page 48: Offline Operation

    Offline Operation 18.0 Offline Operation 18.1 File Handling Once images are captured during Realtime operation, they are viewed and measured with the Offline commands. Here we will touch on a few of the basic operations and functions. • Each captured image is immediately stored in the Capture directory in Offline. •...
  • Page 49 Offline Operation Figure 18.2a Cross-Sectional Measurement on a DVD Replica Disk A cross-sectional line can be drawn across any part of the image, and the vertical profile along that line is displayed. The Cursor menu located at the top of the Display monitor provides the ability to draw a fixed, moving, or averaged cross section.
  • Page 50 Offline Operation There are a wide variety of measurements made in Roughness. The roughness parameters which are displayed are chosen under the Screen Layout menu. The measurements made on the entire image are displayed under “Image Statistics.” Roughness measurements of a specific area may be determined by using the cursor to draw a box on the image. After selecting “Execute,”...

  • Page 51: Filters

    Offline Operation Bearing Bearing ratio determination and depth histogram measurements are possible with Bearing. Bearing provides a method to analyze how much of the surface lies below or above a given height. The “bearing ratio” of the surface is the percentage of the surface at a specific depth with respect to the entire area analyzed.
  • Page 52 Offline Operation Flatten Flatten may be used to remove image artifacts due to vertical (Z) scanner drift, image bow, skips, and anything else that may have resulted in a vertical offset between scan lines. Flattening modifies the image on a line-by-line basis. It consists of removing the vertical offset between scan lines in the fast scan direction (X at 0°...
  • Page 53 Offline Operation Since the vertical offset between each line scan is being removed, this has the effect of removing the information in the Y direction. • When applying flatten on very smooth surfaces, this has a negligible effect on the roughness measurements.
  • Page 54 Offline Operation Figure 18.3c Cross sections on first order flattened image of cells on a smooth glass substrate showing how flattening can cause the distortion of the plane next to a raised feature in the fast direction A-A' B-B' Image after 1st Order flatten This problem can be remedied by excluding the raised or depressed features from the flatten calculation by drawing boxes around them with the cursor before executing the flatten.
  • Page 55 Offline Operation Extreme variations in the sample topography can alter the planefit, leaving a slight tilt in the image. This can be remedied by only selecting flat portions of the image to determine the planefit. The calculation is performed only using the chosen areas, and the planefit is extrapolated on to rest of the image.
  • Page 56 Offline Operation Utility Commands The Utility pull down menu provides the ability to output (and input) data in various forms. Print will send whatever is currently on the Display monitor to a printer. This may also be accomplished at any time (in Realtime and Offline) by hitting the Print Screen button at the top of the keyboard.

  • Page 57: Tip Shape Issues

    Tip Shape Issues 19.0 Tip Shape Issues The SPM image is a result of the interaction of the tip shape with the surface topography. There are two primary features of the tip which affect the SPM image: the radius of curvature and the tip sidewall angles.
  • Page 58 Tip Shape Issues Tip Sidewall Angles of Silicon Nitride Probes 35° 35° 35° 35° Cantilever Tip Sidewall Angles of Etched Silicon Probes Scanning Probe Microscope Training Notebook Rev. F...
  • Page 59 Tip Shape Issues The ability to image steep sidewalls on a sample surface is determined by the sidewall angles of the tip. The tip is not able to profile sides of surfaces steeper than the sidewall angle of the tip. •...

  • Page 60: Resolution Issues

    Tip Shape Issues 19.1 Resolution Issues The resolution of AFM images can be thought of in terms of lateral (X,Y) resolution and vertical (Z) resolution. Lateral Resolution Issues Tip Shape: • As discussed in the previous section on tip shape effects, the radius of curvature of the end of the tip will determine the highest lateral resolution obtainable with a specific tip.
  • Page 61 SPM. This may be a result of combined effects from electrical, mechanical, and acoustic noise sources. • Bruker guarantees 0.3 to ~1Å RMS noise levels depending on the type of SPM and SPM environment. Rev. F...

  • Page 62: Typical Image Artifacts

    Typical Image Artifacts 20.0 Typical Image Artifacts If the tip becomes worn or if debris attaches itself to the end of the tip, the features in the image may all have the same shape. What is really being imaged is the worn shape of the tip or the shape of the debris, not the morphology of the surface features (see Figure 20.0a).
  • Page 63 Typical Image Artifacts the top of the scan. The image on the right is an example of skips and streaking caused by loose debris on the sample surface. Often, loose debris can be swept out of the image area after a few scans, making it possible to acquire a relatively clean image.
  • Page 64 Typical Image Artifacts Figure 20.0e Not Tracking In TappingMode, when operating on the high frequency side of the resonance peak, rings may appear around raised features which may make them appear as if they are “surrounded by water.” An example of this can be seen in the image of the Ti grains on the left. Decreasing the Drive Frequency during imaging can eliminate this artifact, as shown in the image on the right (when reducing the Drive Frequency, the Setpoint voltage may need to be reduced as well) (see Figure...
  • Page 65 Typical Image Artifacts Figure 20.0g 2nd Order Bow At large scan sizes, the bow in the scanner may take on an S-shaped appearance (left). This may be removed by performing a 3rd order planefit in X and Y (right). (Data Scale = 324nm) (see Figure 20.0h).

  • Page 66: Calibration

    Calibration 21.0 Calibration Note: This section is meant to introduce the NanoScope user to basic Calibration procedures. For a more detailed discussion, please consult your specific equipment manual. Please refer to your standard for step height information. As described earlier in this manual, the sensitivity of the scanner decreases exponentially with operation time.
  • Page 67 Calibration Figure 21.0a Baring/Depth Analysis Screen If the measurement is not 200nm + 1nm, calculate the new sensitivity by the following formula: Old Sensitivity x Actual Depth (200nm) New Sensitivity = Measured Depth Input the new sensitivity into the Z sensitivity parameter in the Microscope > Calibrate > Z menu, then repeat this procedure until the scanner is calibrated.
  • Page 68 Calibration Scanning Probe Microscope Training Notebook Rev. F...

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