Page 1 Keysight 5500 Scanning Probe Microscope User’s Guide...
Page 3 Technologies as governed by United duplication or disclosure of Software is Printed in USA States and international copyright laws. subject to Keysight Technologies’ stan- Keysight Technologies dard commercial license terms, and 5301 Stevens Creek Blvd. non-DOD Departments and Agencies of Santa Clara, CA 95051 the U.S.
Page 4 Keysight warrants Keysight hardware, accessories and supplies against defects in material and workmanship for a period of one year from date of shipment. If Keysight receives notice of such defects during the warranty period, Keysight will, at its option, either repair or replace products which prove to be defective.
Page 5: Specifications
100/120/220/240 VAC, 50/60 Hz Mains supply voltage fluctuations are not to exceed 10 % of the nominal supply voltage. These specifications apply to the Keysight 5500 system, and do not N OT E guarantee the function of an experiment (including the cantilever) in these conditions.
Page 6 Read This First Voltage and Laser Safety Information The 5500 SPM will be marked with the following Instruction Manual symbol when it is necessary for the user to refer to this User’s Guide: The following symbol indicates hazardous voltages: This system is designed to be used with a Class II or Class III diode laser with an output of up to 1 mW of visible radiation at 670 nm or 980 nm.
Page 7: Power Supply
Power Supply It is not necessary to open the Keysight AFM Controller to make changes to the power supply. However, the power cord should always be unplugged before making any adjustments to the power source. The Keysight SPM Controller has several different power supply options.
Page 8 Information contained herein this User’s Guide is for general information use only. Information is subject to change without notice. Information should not be construed as a commitment by Keysight Technologies. Furthermore, Keysight Technologies assumes no responsibility or liability for any misinformation, errors, or general inaccuracies that may appear in this manual.
Page 9 Read This First Declaration of Conformity N9410-90001 Keysight 5500 SPM User’s Guide...
Page 10 E-mail: AFM-info@keysight.com Web: www.keysight.com Customer Technical Support Tel: +1-480-756-5900 Fax: +1-480-756-5950 E-mail: AFM-Support@keysight.com Technical Sales Tel: +1-480-756-5900 Fax: +1-480-756-5950 E-mail: AFM-info@keysight.com Distributors and Account Representatives Please visit our web site for up-to-date information: www.keysight.com/find/nano N9410-90001 Keysight 5500 SPM User’s Guide...
Page 11: Table Of Contents
I-viii Disclaimers I-viii Declaration of Conformity I-ix Contact Information II Table of Contents 1 Introduction to the Keysight 5500 Overview of Keysight SPM System SPM Basics SPM Techniques Scanning Tunneling Microscopy (STM) Atomic Force Microscopy (AFM) Contact Mode AFM Intermittent Contact AFM...
Page 12 Glove Box 2-25 Electrochemistry 2-26 PicoTREC 2-26 PicoLITH 2-26 3 Setting Up the Keysight 5500 SPM Component and Facility Dimensions Facility Requirements Utilities Noise and Facility Specifications Assembling the Vibration Isolation Chamber Switching Door Orientation N9410-90001 Keysight 5500 SPM User’s Guide...
Page 13 Constant Force Mode Constant Height Mode Fine-Tuning the Image 6 AC Modes Acoustic AC Mode (AAC) AAC Mode Constant Height Mode Magnetic AC (MAC) Mode Standard MAC Mode 6-10 Top MAC Mode 6-12 Q Control 6-13 N9410-90001 Keysight 5500 SPM User’s Guide...
Page 14 Care and Handling of the Probes and Scanner Probes Nose Assembly Scanner Scanner Characteristics Non-Linearity Sensitivity Hysteresis Other Characteristics Calibrating the Multi-Purpose Scanner X Calibration Y Calibration 8-14 Non-Orthogonality 8-17 Z Calibration 8-18 Servo Gain Multiplier 8-19 N9410-90001 Keysight 5500 SPM User’s Guide...
Page 15 Setting Parameters for AM Mode Operation 11-36 Setting Parameters for FM Mode Operation 11-40 Piezoresponse Force Microscopy 11-43 12 Liquid Cell Liquid Cell with Standard Sample Plate 12-2 Liquid Cell with MAC Mode 12-4 Flow-Through Liquid Cell 12-4 N9410-90001 Keysight 5500 SPM User’s Guide...
Page 16 16-3 Electrodes 16-3 Cleaning 16-5 Liquid Cell Cleaning 16-5 Electrode Cleaning 16-6 Sample Plate Cleaning 16-6 Substrate Cleaning 16-6 Assembling and Loading the Liquid Cell 16-6 Troubleshooting 16-8 Electrochemistry Definitions 16-8 Software Controls 16-9 N9410-90001 Keysight 5500 SPM User’s Guide...
Page 17 Keysight 5500 SPM with MAC Mode Controller Keysight 5500 SPM with MAC Mode, Force Modulation Imaging Keysight 5500 SPM with MAC III Option Keysight 5500 SPM with MAC III Option and Closed Loop Scanner Index N9410-90001 Keysight 5500 SPM User’s Guide...
Page 18 1-15 Kelvin Force Microscopy (KFM) 1-15 The Keysight 5500 SPM is the ideal multiple-user research system for Scanning Probe Microscopy (SPM). As the high-performance Atomic Force Microscope (AFM) flagship of Keysight’s product line, the 5500 SPM provides a wealth of unique technological features, including precision temperature control and industry-leading environmental control.
Page 19: Introduction To The Keysight 5500
In this User’s Guide we will begin with a brief introduction to Scanning Probe Microscopy techniques. The sections that follow will show you how to handle the 5500 SPM components and how to image in the available modes. Keysight 5500 SPM User’s Guide...
Page 20: Spm Basics
Introduction to the Keysight 5500 SPM Basics Scanning Probe Microscopy (SPM) is a large and growing collection of techniques for investigating the properties of a sample, at or near the sample surface. The SPM instrument has a sharp probe (with radius of...
Page 21 Introduction to the Keysight 5500 collection of data points is then synthesized into the “SPM image,” a 3-dimensional map of the surface characteristic being examined. The most common SPM images are topography images, in which the third dimension, Z, for any given X/Y coordinates, is the relative height of the sample surface.
Page 22: Spm Techniques
Introduction to the Keysight 5500 SPM Techniques Scanning Tunneling Microscopy (STM) The earliest, widely-adopted SPM technique was Scanning Tunneling Microscopy (STM). In STM, a bias voltage is applied between a sharp, conducting tip and the sample. When the tip approaches the sample, electrons “tunnel”...
Page 23: Atomic Force Microscopy (Afm)
Introduction to the Keysight 5500 current mode is typically slower than constant height mode. However, greater variations in height can be accommodated. Figure 1-4 Constant Height mode STM (above) is faster but is limited to smooth surfaces; Constant Current mode (below) is capable of...
Page 24 Introduction to the Keysight 5500 difference between the Deflection value and the user-specified Set Point is called the “error signal.” Figure 1-5 Basic AFM principles Figure 1-6 shows the force interaction as the tip approaches the sample. At the right side of the curve the tip and sample are separated by large distance.
Page 25: Contact Mode Afm
Introduction to the Keysight 5500 described below, can be generally described by their function within these three domains. Figure 1-6 Zones of interaction as the tip approaches the sample The tip-sample interaction is complicated by additional forces, including strong capillary and adhesive forces that attract the tip and sample.
Page 26: Intermittent Contact Afm
Introduction to the Keysight 5500 tip makes gentle contact with the sample, exerting from ~0.1-1000 nN force on the sample. AFM can be conducted in either constant height or constant force modes. In constant height mode, the height of the scanner is fixed as it scans.
Page 27: Acoustic Ac (Aac) Afm
Introduction to the Keysight 5500 components.The complex tip-sample forces cause changes in the amplitude, phase and resonance frequency of the oscillating cantilever. Thus, topography, amplitude and phase can be collected simultaneously. The phase and amplitude images may highlight physical properties that are not readily discernible in the topographic map.
Page 28: Magnetic Ac (Mac) Mode
(c.) is used as a feedback signal to maintain constant amplitude of the cantilever motion. Acoustic AC Mode is an option for the 5500 SPM and requires the N OT E additional Mac Mode or MAC III controller.
Page 29: Current Sensing Mode (Csafm)
MAC Mode. Top MAC Mode is an option for the 5500 SPM and requires the N OT E additional MAC Mode or MAC III controller, as well as a Top MAC nose assembly.
Page 30: Force Modulation Microscopy (Fmm)
Introduction to the Keysight 5500 between the conducting cantilever and sample, a current is generated which is used to construct a conductivity image. CSAFM is compatible with measurements in air, under controlled environments, and measurements with temperature control. The technique is useful in molecular recognition studies and can be used to spatially resolve electronic and ionic processes across cell membranes.
Page 31: Lateral Force Microscopy (Lfm)
Introduction to the Keysight 5500 FMM requires MAC Mode or MAC III. N OT E Lateral Force Microscopy (LFM) Lateral Force Microscopy (LFM) is a derivative of Contact AFM with the scan direction perpendicular to the long axis of the cantilever. In LFM, the tip is constantly in contact with the sample surface.
Page 32: Magnetic Force Microscopy (Mfm)
AAC (or MAC) in Intermittent Contact Mode. The two images can then be displayed side-by-side to highlight any correlation between the electrostatic response and topography. EFM is an option for the 5500 SPM and requires the additional MAC III N OT E controller.
Page 33 As in EFM mode, KFM uses a conductive tip and either standard AAC or MAC Modes. KFM is an option for the 5500 SPM and requires the additional MAC III N OT E controller. Keysight 5500 SPM User’s Guide...
Page 34 Keysight 5500 SPM User’s Guide Keysight 5500 SPM Components Microscope Probes Nose Assembly One-Piece Nose Assemblies Two-Piece Nose Assemblies Scanner Detector Sample Plates 2-10 Video System 2-12 Head Electronics Box (HEB) 2-13 AFM Controller 2-15 Breakout Box 2-16 Vibration Isolation Chamber...
Page 35: Keysight 5500 Spm Components
Keysight 5500 SPM Components The major components for the Keysight 5500 SPM are shown in Figure 2-1. Figure 2-1 Components of the Keysight 5500 SPM Keysight 5500 SPM User’s Guide...
Page 36: Microscope
X/Y positioning micrometers, magnetic supports for the sample plates, and interconnections for all electronics. The support stand is hinged to allow easy access to the sample plate area. Figure 2-2 5500 SPM with support stand Keysight 5500 SPM User’s Guide...
Page 37: Probes
Chapter 1, “Introduction to the Keysight 5500,” are performed using either a wire tip (for STM) or, for AFM imaging, a tip at the free end of a cantilever (a “probe”). STM tips are made by cutting or electrochemical etching Platinum-Iridium or tungsten wire.
Page 38: Nose Assembly
Figure 2-3 One-piece nose assemblies. Clockwise from upper left: Top MAC, CSAFM, Contact Mode, AAC, STM The CSAFM nose assembly cannot be used for imaging in liquid. C A U T I ON Keysight 5500 SPM User’s Guide...
Page 39: Two-Piece Nose Assemblies
Currently the two-piece nose assembly is only available for AC Mode/Contact Mode imaging. The two-piece nose assembly cannot be used for imaging in liquid. C A U T I ON Figure 2-4 Two-piece nose cone with removal tool and assembly fixture Keysight 5500 SPM User’s Guide...
Page 40: Scanner
Keysight 5500 SPM Components Scanner The Keysight 5500 is a tip-scanning system, in which the cantilever sits on a scanner and is moved in raster fashion across the stationary sample. The scanner (Figure 2-5) includes one or more elements made from piezoceramic material.
Page 41 Z axis only, or all three (X, Y, Z) axes. Closed-loop scanning provides superior lateral positioning control and more accurate Z-position. • An STM-specific scanner is purpose-built for Scanning Tunneling Microscopy. Keysight 5500 SPM User’s Guide...
Page 42: Detector
Enabling the gain is useful when using very non-reflective cantilevers to ensure a high enough Sum value is provided to the control system. Figure 2-6 Detector assembly, top and bottom views Keysight 5500 SPM User’s Guide...
Page 43: Sample Plates
Keysight 5500 SPM Components Sample Plates The Keysight 5500 SPM is designed to allow scanning from above the sample. A variety of sample plates provide mounting options and micro-environments for imaging (Figure 2-7). The standard sample plate has a magnetic core that will securely hold samples mounted on magnetic backings.
Page 44 The microscope stand is equipped with three magnetic posts from which a sample plate is mounted (Figure 2-8). Micrometers enable manual X/Y positioning with total travel of approximately ±5 mm. Figure 2-8 Sample plate on microscope stand Keysight 5500 SPM User’s Guide 5-11...
Page 45: Video System
It includes a camera and optics on an adjustable stand (Figure 2-9) along with a separate illumination source (Figure 2-10). A USB cable connects the camera to the computer. Figure 2-9 Video system Figure 2-10 Video system light source Keysight 5500 SPM User’s Guide 5-12...
Page 46: Head Electronics Box (Heb)
(LFM) depending on the state of the switch directly below the meter. The Open/Close switch is used to move the sample and tip further apart (Open) or closer together (Close). Figure 2-11 Head Electronics Box Keysight 5500 SPM User’s Guide 5-13...
Page 47 Keysight 5500 SPM Components The HEB back panel connections are shown in Figure 2-12: Figure 2-12 HEB back panel connectors and controls Keysight 5500 SPM User’s Guide 5-14...
Page 48: Afm Controller
±10 V and the input is scaled up by the controller to ±215 V. The External Sync BNC is a signal that is sent each time a frame, line, or pixel is completed. This can be used in Custom Spectroscopy or Keysight 5500 SPM User’s Guide 5-15...
Page 49: Breakout Box
SPM. This box is shown in Figure 2-14 and described in Table “Breakout Box Connections must be made properly and are shown in Figure 2-15 on page 20: Figure 2-14 Breakout box for AFM controller Keysight 5500 SPM User’s Guide 5-16...
Page 50 This input is displayed by the software with units of current. This signal is not affected by the presence of the AC Mode controller in the system. This input has a range of ±10 V. Keysight 5500 SPM User’s Guide 5-17...
Page 51 This output is ±215 V and is current limited to 70 mA. Z HV This is the Z High Voltage signal used to drive the piezo for scanning in the Z direction. This output is ±215 V and is current limited to 70 mA. Keysight 5500 SPM User’s Guide 5-18...
Page 52: Breakout Box
Connect the other end of the cable to the appropriate 9-pin connector located on the side of the N9744A breakout box. Connect one end of a second DB-9 cable (included with the breakout box) to the second 9-pin Keysight 5500 SPM User’s Guide 5-19...
Page 53 Keysight 5500 SPM Components connector on the side of the breakout box. Connect the other end of the second cable to the 9-pin connector on the 5500 microscope base. Figure 2-15 Wiring diagram for breakout box Keysight 5500 SPM User’s Guide...
Page 54: Vibration Isolation Chamber
Keysight 5500 SPM Components Vibration Isolation Chamber The isolation chamber (Figure 2-16) isolates the 5500 SPM from vibration, air turbulence and acoustic noise which would adversely affect imaging. It also, to an extent, helps control temperature variability. The chamber provides acoustic isolation for the instrument with multiple layers of sound-damping materials.
Page 55: Software
Keysight 5500 SPM Components Software The Keysight 5500 SPM includes PicoView, a powerful software package for controlling all aspects of alignment, calibration, imaging and more. Integrated in the software are windows for controlling digital cameras and displaying video or still-image output. The post-acquisition PicoImage software for image analysis and data manipulation offline is an available option and highly recommended.
Page 56: System Options
Keysight 5500 SPM Components System Options Many options are available for the Keysight 5500 SPM. As discussed above, probes, nose assemblies and sample plates are available for particular applications. Scanner options include large and small scan ranges, closed-loop scanning, and a dedicated STM scanner. Other...
Page 57: Temperature Control
Additional information is provided in Chapter Environmental Chamber The environmental chamber (Figure 2-19) allows imaging in controlled atmospheres. Ports and fittings enable gases, liquids and probes to be Keysight 5500 SPM User’s Guide 5-24...
Page 58: Glove Box
Additional information is provided in Chapter Figure 2-19 Environmental chamber Glove Box The 5500 SPM body can be place directly on top of this small glove box, shown in Figure 2-20, offering greater environmental control. Since the piezo and electronic parts are totally isolated from the imaging environment, it is possible to perform experiments under very reactive conditions without damaging the system or the sample.
Page 59: Electrochemistry
Figure 2-21 PicoTREC controller PicoLITH PicoLITH is an optional package for nanoscale positioning and manipulation, and nanolithography. The PicoLITH option includes its own documentation and is not covered in this manual. Keysight 5500 SPM User’s Guide 5-26...
Page 60: Setting Up The Keysight 5500 Spm
Here are the approximate dimensions of some of the components of the Keysight 5500 SPM: • 5500 Microscope: 210 mm W x 190 mm H x 160 mm D (8 in W x 8 in H x 6 in D)
Page 61 • Vibration Isolation Chamber: 521 mm W × 915 mm H × 603 mm D (20.5 in W x 36 in H x 23.75 in D) The most common system configuration includes the 5500 SPM within a vibration isolation chamber, with the controls on a separate table from...
Page 62 Setting Up the Keysight 5500 SPM pounds; therefore, a solid table that can easily accommodate 300 pounds is required. Figure 3-1 Top and front views of Keysight 5500 SPM suspended inside the isolation chamber, on the left. The control station is on the right.
Page 63: Facility Requirements
Setting Up the Keysight 5500 SPM Facility Requirements Following these guidelines for preparing the Keysight 5500 SPM facility will ensure a smooth installation, will make using the system more convenient and will improve system performance for the life of the SPM: •...
Page 64: Utilities
(Figure 3-2), to define acceptable environmental noise. For operation of the Keysight 5500 SPM, facility acoustic noise should be less than 75 dBc. In order to achieve the Keysight 5500 SPM User’s Guide...
Page 65: Temperature And Humidity Variation
Setting Up the Keysight 5500 SPM specified noise level, the vibration isolation chamber installation surface must meet Criterion D. Figure 3-2 Vibration criterion curves and ISO guidelines Temperature and Humidity Variation Changes in temperature and humidity will affect both resolution and repeatability of imaging.
Page 66: Assembling The Vibration Isolation Chamber
Setting Up the Keysight 5500 SPM Assembling the Vibration Isolation Chamber Unpack the vibration isolation chamber from the box and remove the packing bag. Save the packing materials for subsequent use. The chamber is very heavy. Using the lifting handles (see...
Page 67 Setting Up the Keysight 5500 SPM Remove the accessory bag from the chamber. This bag contains four adjustable bungee mounts, four bungee cords and a 2.5 mm hex wrench for assembly. Place the instrument platform, included in a smaller box, on the floor of the chamber.
Page 68: Switching Door Orientation
Setting Up the Keysight 5500 SPM Figure 3-5. Turning the mount to the right will raise the bungee mount; turning the mount to the left will lower the bungee mount. Figure 3-5 Adjusting bungee mounts to level the instrument platform Switching Door Orientation The door may be hinged on either the left or right side as needed.
Page 69: Managing Cables
Setting Up the Keysight 5500 SPM Use wrench to detach latch attachment screws (Figure 3-7). Note orientation of latch parts. Keep screws and latch parts for subsequent reattachment. Figure 3-7 Latch with latch attachment screws Support weight of enclosure door from below. Use wrench to detach screws which attach the hinge to the enclosure body.
Page 70 Setting Up the Keysight 5500 SPM Figure 3-8 Cables installed with good seal. Keysight 5500 SPM User’s Guide 5-11...
Page 71: Connecting The Components
Setting Up the Keysight 5500 SPM Connecting the Components The cabling for the standard 5500 SPM is shown in Figure 3-9. Other cabling configurations are included in Appendix Figure 3-9 Cabling for basic 5500 SPM configuration Always make sure that all cables are connected before turning on any of C A U T I O N the components.
Page 72: Guidelines For Moving The System
• Turn off all components before disconnecting cables. • Disconnect all cables before moving any components. • Remove the scanner, detector and sample from the 5500 SPM before moving the microscope base. • Remove the microscope base from the vibration isolation chamber and transport both separately.
Page 73: Care And Handling Of The Probes And Scanner
Setting Up the Keysight 5500 SPM Care and Handling of the Probes and Scanner Probes Always store probes at room temperature in their protective cases. Handle probes gently with tweezers, following the procedures described earlier in this chapter. If a probe is dropped it may very well be damaged. You can check whether the cantilever is intact by viewing it through a magnifier.
Page 74 If the nose assembly housing becomes loose or can be wiggled when in place, contact Keysight support for assistance. Cracked or broken piezoelectrodes will result in abnormal imaging.
Page 75: Preparing For Imaging
Using the Video System 4-29 The Keysight 5500 SPM is capable of imaging in many different modes. Several steps of the imaging process are similar or identical, however, for all modes. This chapter will cover the steps that are common to most imaging procedures.
Page 76: One-Piece Nose Assembly
Ensure that the ends of the metal spring for retaining the cantilever are C A U T I ON not caught in between the nose cone and the socket. Keysight 5500 SPM User’s Guide...
Page 77 LARGE torques about the anchor point for the piezoes, where most breakage occurs. Do NOT push down on the top of the nose assembly as this will damage the spring clip and/or glass window. Keysight 5500 SPM User’s Guide...
Page 78: Removing The One-Piece Nose Assembly
Position your thumb on the flat surface of the removal tool and your fingers on BOTH sides of the extraction arm. Gently pull up with your fingers while pushing down with your thumb (Figure 4-4). Keysight 5500 SPM User’s Guide...
Page 79 4-5).Tweezers can create a pivot point to lever the nose out of the scanner, placing large lateral forces on the piezo assembly. The nose assembly removal tool is the only acceptable method for extracting the nose from the scanner. Keysight 5500 SPM User’s Guide...
Page 80: Inserting A Probe In The One-Piece Nose Assembly
Inserting a Probe in the One-Piece Nose Assembly Keysight nose assemblies are designed with a spring and guides to retain the probe in the proper position for imaging. A spring key (Figure 4-6) is included with the system to let you safely hold back the spring while inserting the probe.
Page 81 Ensure that the ends of the metal spring for retaining the cantilever are C A U T I ON not caught in between the nose cone and the socket. Keysight 5500 SPM User’s Guide...
Page 82 Figure 4-7 on page 7. Figure 4-9 Hold back the retaining spring while placing the probe Gently lower the spring clip to hold the probe in place. Keysight 5500 SPM User’s Guide...
Page 83: Two-Piece Nose Assembly
As with the one-piece nose assembly, the body of the two-piece assembly is held in the scanner by an O-ring. To insert the body, first place the scanner in the scanner mounting fixture (Figure 4-1 Keysight 5500 SPM User’s Guide...
Page 84: Removing The Body Of The Two-Piece Nose Assembly
Position thumb on the flat surface of the removal tool and fingers on BOTH sides of the extraction arm. Gently pull up with fingers while pushing down the thumb. Keysight 5500 SPM User’s Guide 5-10...
Page 85: Inserting A Probe In The Two-Piece Nose Assembly
Using tweezers, gently grasp a probe from its sides, applying just enough pressure to secure it in the tweezers. Move the assembly fixture lever to the right, which will slightly separate the nose assembly disk (Figure 4-13). Keysight 5500 SPM User’s Guide 5-11...
Page 86: Inserting The Scanner And Connecting Cables
Make sure there is adequate clearance below the scanner socket in the middle of the microscope. Place the scanner assembly into the scanner socket, with the scanner’s frosted screen facing up and forward (Figure 4-14). Keysight 5500 SPM User’s Guide 5-12...
Page 87 C/L socket on the rear of the Head Electronics Box. Be sure to withdraw tip from sample surface before disconnecting C A U T I ON cables and removing scanner from microscope base. Keysight 5500 SPM User’s Guide 5-13...
Page 88: Aligning The Laser
The next step is to ensure that the scanner laser spot is aligned to reflect off of the cantilever. Several methods can be used to do so. In most cases, particularly with highly reflective samples, you can use the 5500 SPM video system to focus on the cantilever and align the laser spot (Figure 4-15).
Page 89 Preparing for Imaging detector. Due to the variation of cantilever types and vendors, the position of the laser on the cantilever needs to be optimized for each tip. Figure 4-16 Laser alignment Keysight 5500 SPM User’s Guide 5-15...
Page 90 Place a white piece of paper or business card on the table below the microscope. If using a 980 nm IR scanner, use an IR sensor card in Keysight 5500 SPM User’s Guide 5-16...
Page 91 (Figure 4-18). Figure 4-18 Aligning laser spot over white paper. The laser alignment knobs are located on the top of the scanner (Figure 4-19). The front-to-back knob moves the laser spot toward the Keysight 5500 SPM User’s Guide 5-17...
Page 92 (Diagram B in Figure 4-20). When the laser reaches the chip it will be blocked and will no longer be visible on the paper. You should only need to turn the knob a few rotations. Keysight 5500 SPM User’s Guide 5-18...
Page 93 (and the spot reappears on the paper) (Diagram E in Figure 4-20). Turn the front-to-back knob clockwise slightly to position the laser just on the cantilever tip (Diagram F in Figure 4-20). The spot will reappear on the ground glass. Keysight 5500 SPM User’s Guide 5-19...
Page 94 The easiest way to recover is to roughly center both controls again, moving Keysight 5500 SPM User’s Guide 5-20...
Page 95 Preparing for Imaging the laser back to the center of its travel in both directions. Doing so should make the laser spot reappear. Figure 4-22 Laser alignment control when far out of alignment Keysight 5500 SPM User’s Guide 5-21...
Page 96: Inserting And Aligning The Detector
(lateral, or friction), and SUM signals. Figure 4-23 Photodiode detector operation To install the photodiode detector, insert it into the scanner until it stops (Figure 4-24). Plug the detector cable into the Detector socket on the Keysight 5500 SPM User’s Guide 5-22...
Page 97 Detector alignment is completed through the PicoView software: Launch PicoView. The Laser Alignment window (as well as other windows) will open, displaying the position of the laser spot on the Keysight 5500 SPM User’s Guide 5-23...
Page 98 If the laser spot is off the detector, the SUM signal will be close to 0 V and the solid laser spot in the Laser Alignment window will be displayed as an unfilled circle. Take the detector out of the scanner Keysight 5500 SPM User’s Guide 5-24...
Page 99 For Contact Mode, the dotted yellow line (Figure 4-26) shows the recommended vertical alignment of the laser prior to approaching the sample. Figure 4-26 Align spot to yellow, dotted line for Contact Mode Keysight 5500 SPM User’s Guide 5-25...
Page 100: Mounting The Sample
Preparing for Imaging Mounting the Sample The Keysight 5500 SPM accepts a wide variety of sample plates, including specialized plates for imaging in liquid, in controlled temperature, etc. To use a sample plate: Mount the sample to the sample plate.
Page 101 Place the second alignment tab over the alignment pin as in image B Figure 4-27. Keep the sample plate at an angle so as not to bring the tip into contact with the plate inadvertently. Keysight 5500 SPM User’s Guide 5-27...
Page 102 The 3-pin EC cable provides bias to the sample. The 3-pin MAC connector provides signal to the magnetic coil for MAC Mode. Figure 4-28 EC/MAC cable Keysight 5500 SPM User’s Guide 5-28...
Page 103: Using The Video System
Preparing for Imaging Using the Video System The Keysight 5500 SPM includes a USB-based video system for viewing the tip and sample. The optics of the video system and optics in the scanner together provide optical magnification of up to 150x, depending on the zoom setting of the video lens, on the computer monitor.
Page 104 (Figure 4-31). Turn the front knob clockwise to move the field-of-view backward, and counterclockwise to move it forward. Turn the side knob Keysight 5500 SPM User’s Guide 5-30...
Page 105 Figure 4-31 Adjusting lateral position of the video system Twist the Zoom control (Figure 4-32) to the left to increase the zoom, or to the right to decrease zoom. Figure 4-32 Adjusting zoom Keysight 5500 SPM User’s Guide 5-31...
Page 106 Preparing for Imaging Choose Controls > CameraView to view the video output from the camera (Figure 4-33). Figure 4-33 Camera View window showing tip and sample. Keysight 5500 SPM User’s Guide 5-32...
Page 107: Contact Mode Imaging
Additional factors may affect the quality of images produced in Contact Mode. To understand more about these factors please be sure to read the PicoView software documentation and Keysight training materials. This chapter references material in Chapter 4, “Preparing for Imaging".
Page 108: Setting Up For Contact Mode Imaging
Viewing the video window, bring the tip and sample very close to contact: Adjust the focus and x-y alignment of the video system such that the tip is in sharp focus (Figure 5-1). Keysight 5500 SPM User’s Guide...
Page 109 The tip should now be just above the sample surface. Raise the sample slowly and carefully to avoid collision with the C A U T I ON sample. Hard contact between the tip and the sample can damage either or both. Keysight 5500 SPM User’s Guide...
Page 110 Open the Scan and Z controls window. In the Scan and Z Controls Servo tab (Figure 5-4), enter a Setpoint value slightly more positive than the current Deflection reading. This sets the deflection that the feedback loop will achieve and maintain. Keysight 5500 SPM User’s Guide...
Page 111 Setpoint is maintained. A yellow bar will show the position of the piezo within its available range of motion. The center of the range is defined as “zero,” with positive values indicating piezo displacement away from the sample, and negative Keysight 5500 SPM User’s Guide...
Page 112 In the Scan Controls section of the Scan and Z Controls window, select the Scan tab (Figure 5-5). Figure 5-5 Scan and Z Controls window: Scan tab Figure 5-6 Scan Controls section of Scan and Z Controls window Keysight 5500 SPM User’s Guide...
Page 113 Click the Up blue arrow to initiate the scan from the bottom up (Figure 5-6). The image maps will begin to be displayed in the Realtime Images window. Keysight 5500 SPM User’s Guide...
Page 114 Depending on the Frames setting in the Scan and Motor window, the system will either scan once and stop, or it will scan infinitely, overwriting the previous scan each time. You can also choose to scan for Keysight 5500 SPM User’s Guide...
Page 115: Constant Height Mode
Higher force can place undue wear on the tip and, in the extreme, can damage the tip or sample. The optimal Setpoint value, which will vary per sample and per probe, places enough force on the tip to accurately trace the topography Keysight 5500 SPM User’s Guide...
Page 116: Gains
Increase the I Gain until oscillations appear in the scan lines, then decrease until the oscillations cease. Adjust the P Gain to increase image quality. P Gain is typically close to the same value as the I Gain. Keysight 5500 SPM User’s Guide 5-10...
Page 117: Scan Settings
After completing the large scan, use the Offset and Size values in the Scan and Motor window to adjust the scan to cover the region of interest. Increase the Resolution, decrease the Speed, and re-scan the zoomed region. Keysight 5500 SPM User’s Guide 5-11...
Page 118 Keysight 5500 SPM User’s Guide AC Modes Acoustic AC Mode (AAC) AAC Mode Constant Height Mode Magnetic AC (MAC) Mode Standard MAC Mode 6-10 Top MAC Mode 6-12 Q Control 6-13 In AC Mode, introduced in “Intermittent Contact AFM" on page 9, a sinusoidal voltage is applied to a piezo element or magnetic coil in the nose assembly or sample plate.
Page 119: Ac Modes
Controls > Setup from the main PicoView menu or click the Setup button in the main toolbar. Open the System Components tab and verify that the Serial Port AC Mode Controller check box is selected. Keysight 5500 SPM User’s Guide...
Page 120: Acoustic Ac Mode (Aac)
Use the Close switch on the HEB to bring the tip close to the sample (within 1-2 mm). In PicoView choose Mode > ACAFM. Keysight 5500 SPM User’s Guide...
Page 121 Auto or Manual Tune. In most cases the Auto Tune procedure will be used and is the procedure that will be discussed here. In the ACAFM tab of the AC Tune window, set the Drive Mechanism to AAC. See Figure 6-3. Keysight 5500 SPM User’s Guide...
Page 122 If the resonance frequency range is known more exactly, a smaller range can be used to speed the tuning process. Keysight 5500 SPM User’s Guide...
Page 123 Rotate the video system focus knob very slightly towards you such that the tip goes just out of focus (the focal plane is just below the tip now). Press the Close switch to raise the sample until the sample comes into focus. Keysight 5500 SPM User’s Guide...
Page 124 Chapter In the Scan tab, enter the Size (in microns) and X Offset and/or Y Offset values to set the size and center of the scan. You can also click Keysight 5500 SPM User’s Guide...
Page 125: Constant Height Mode
Constant Height Mode should only be used for very flat samples. To image in Constant Height mode, in the Servo window set the I and P gains to 0.1 %. This system will only very slowly adjust the z-piezo in Keysight 5500 SPM User’s Guide...
Page 126: Magnetic Ac (Mac) Mode
MAC Mode requires either a MAC Mode or MAC Mode III Module, both of which offer the lock-in amplifier required to precisely drive the MAC coil (the MAC Mode III offers additional lock-in amplifiers for Keysight 5500 SPM User’s Guide...
Page 127: Standard Mac Mode
Standard MAC Mode In standard MAC Mode, the coil is located in the sample plate (Figure 6-6). A Contact Mode or AC Mode nose assembly can be used. Figure 6-6 MAC Mode sample plate Keysight 5500 SPM User’s Guide 5-10...
Page 128 Connect the MAC cable connector (blue and green wires) of the EC/MAC cable to the 3-pin connector on the MAC cable (Figure 6-7). Connect the MAC cable to the 6-pin connector on the sample plate as shown in Figure 6-8 on page 12. Keysight 5500 SPM User’s Guide 5-11...
Page 129: Top Mac Mode
Top MAC Mode In Top MAC Mode AFM, the driver coil is located in the nose assembly (Figure 6-9). This configuration provides better tip response when imaging thick samples which can lessen the magnetic field oscillating Keysight 5500 SPM User’s Guide 5-12...
Page 130: Q Control
Q Control is a method that reduces damping of the system, increasing the quality factor of the oscillating cantilever. Enhanced resonance allows imaging with very low force and high phase sensitivity. The Keysight 5500 SPM User’s Guide 5-13...
Page 131 This will set the optimal Q Control Drive (%) value in the lower section of the ACAFM Controls window as shown on the left in Figure 6-11 page 15. The optimized Drive (%) and Phase Shift will also show in the Keysight 5500 SPM User’s Guide 5-14...
Page 132 Figure 6-11 ACAFM Controls and Other tab after Q control optimization Note that negative numbers can be used for the Q Control Drive (%) to lower the Q Control drive amplitude. However the standard AC Mode Drive (%) must be a positive number. Keysight 5500 SPM User’s Guide 5-15...
Page 133 Q Control optimization. Figure 6-12 below shows the change in the amplitude resonance peak before (top) and after (bottom) applying Q Control. Figure 6-12 Amplitude resonance peak before (top) and after (bottom) optimizing Q Control Keysight 5500 SPM User’s Guide 5-16...
Page 134 AC Modes Note the phase curve will also show a steeper slope as shown below in Figure 6-13. Figure 6-13 Phase before (top) and after (bottom) optimizing Q Control Keysight 5500 SPM User’s Guide 5-17...
Page 135: Additional Imaging Modes
7-36 Volume Spectroscopy 7-41 One of the primary advantages of the Keysight 5500 SPM is that it allows you to perform many different imaging modes with the same basic hardware. Most of the modes presented in this chapter are based...
Page 136 STM remarkably high lateral resolution. Keysight STM tips are pre-cut or chemically etched lengths of 0.25 mm OD, 80 % platinum - 20 % iridium wire. If the wire tip is damaged it can be trimmed and used again.
Page 137: Stm Gain And Preamp Settings
The preamp stage uses a fixed preamp board module as shown in Figure 7-4. It can be replaced with different sensitivity settings as noted Table 3. The standard scanner has the module with 10 nA/V Keysight 5500 SPM User’s Guide...
Page 138 Pull out the preamp module carefully. Hold on to the 4-pin connector and unplug the module from the cable. Replace the module and plug it back onto the 4-pin connector. Tighten the module back onto the scanner. Keysight 5500 SPM User’s Guide...
Page 139 Additional Imaging Modes Figure 7-5 Hold the connector while unplugging the preamp module Keysight 5500 SPM User’s Guide...
Page 140: Stm Imaging Procedure
The particular mounting arrangement will depend on the sample type and size. Attach an electrode from the sample plate to the sample. Lift the spring-loaded electrode clip on the sample plate and insert the Keysight 5500 SPM User’s Guide...
Page 141 In the Servo window enter the Bias Voltage (Figure 7-8). Typical values are 50-200 millivolts (0.05-0.200 V). A positive bias indicates current flow from the tip to the sample, and vice versa for negative bias. Keysight 5500 SPM User’s Guide...
Page 142 Then increase the Setpoint until the indicator in the Servo window just turns green. For rougher surfaces you may need to increase the setpoint current slightly more. In the Scan and Motor window, click the Up or Down arrows to begin the scan. Keysight 5500 SPM User’s Guide...
Page 143: Current Sensing Afm (Csafm)
(especially a moisture layer on the sample surface) can reduce the clarity of imaging, it is strongly recommended that CSAFM be completed in a controlled, low humidity environment. The Keysight multi-purpose scanner can be used with the CSAFM nose assembly (Figure 7-10) for CSAFM imaging.
Page 144 Lift the spring-loaded electrode clip on the sample plate and insert the electrode under it (Figure 7-7 on page 7). Connect the electrode to the sample. Check Keysight 5500 SPM User’s Guide 5-10...
Page 145 X Offset and/or Y Offset values to set the location of the scan center. Press the Close switch on the HEB to raise the sample until the tip is close to, but not touching, the sample. Keysight 5500 SPM User’s Guide 5-11...
Page 146 The amplitude of the current signal is strongly dependent upon the condition of the cantilever tip and sample surface, as well as the force applied to the surface. Using known good tips, a controlled environment and low tip force will improve imaging. Keysight 5500 SPM User’s Guide 5-12...
Page 147: Lateral Force Microscopy (Lfm)
Figure 7-11 Display Trace and Retrace Friction images It is important in LFM that the LFM signal on the Head Electronics Box N OT E be carefully set as close to zero as possible. Keysight 5500 SPM User’s Guide 5-13...
Page 148: Dynamic Lateral Force Microscopy (Dlfm)
Insert and align the detector. In PicoView choose Mode > DLFM. Choose Controls > AC Mode to open the ACAFM Controls window. Set the Drive Mechanism to AAC. Set the Drive % to 10 %. Keysight 5500 SPM User’s Guide 5-14...
Page 149 In the Servo window, set the I Gain and P Gain to 5 %. Keysight 5500 SPM User’s Guide 5-15...
Page 150: Force Modulation Microscopy (Fmm)
The multi-purpose scanner and AAC nose assembly are used for FM Mode. A specific Force Modulation cantilever is available through Keysight; however, the best choice of cantilever is often experimentally determined. A MAC Mode or MAC III controller is also required.
Page 151 Now set up the additional AC oscillation: Choose Controls > AC Mode to open the ACAFM Controls window. Set the Drive Mechanism to AAC. Set the Drive % to 10 %. Set the Frequency to 20-50 kHz. Keysight 5500 SPM User’s Guide 5-17...
Page 152 HEB Aux (the Amplitude signal via the HEB). If using a MAC III controller, select Aux 1 and Aux 2. In the Scan and Motor window, click the Up or Down blue arrows to initiate a scan. Keysight 5500 SPM User’s Guide 5-18...
Page 153: Magnetic Force Microscopy
X direction (trace and retrace), measuring topography, then raises the cantilever above the surface and scans the same line again (trace and retrace). This interlacing of scans on a line-by-line basis is called an Keysight 5500 SPM User’s Guide 5-19...
Page 154 Turn the video system focus knob toward you such that the tip goes just out of focus (the focal plane is just below the tip now). Repeat this iteratively (steps a-c) until both the tip and sample are in focus (i.e., they are nearly touching). Keysight 5500 SPM User’s Guide 5-20...
Page 155 The Trace/Retrace window inputs are NOT dependent on the settings in the Realtime Imaging window. The scan modes should be set to Main in the Trace/Retrace window when Interleave scanning is completed if changed during MFM imaging. Keysight 5500 SPM User’s Guide 5-21...
Page 156 Enter the Drive (%) value from the ACAFM Controls dialog box into the Interleave Drive (%) (Figure 7-13) for MFM imaging. Re-set the Drive (%) in the the ACAFM Controls dialog box to its original value. Keysight 5500 SPM User’s Guide 5-22...
Page 157 In the Scan and Motor window’s Scan tab, enter: Scan Speed of 1-2 ln/s. Resolution of 512. Scan Size (in microns). X Offset and/or Y Offset values to set the center of the scan. Keysight 5500 SPM User’s Guide 5-23...
Page 158 In the Servo window Main tab and the Scan and Motor window Scan tab, adjust the Gain, Scan Speed, Resolution, etc., to optimize the topography image. In the Interleave tab, adjust the Gain, Stop At and Pull Away parameters to optimize the MFM phase image. Keysight 5500 SPM User’s Guide 5-24...
Page 159: Electrostatic Force Microscopy (Efm)
Plug the 3-pin EC connector of the EC/MAC cable into the 3-pin socket on the sample plate. Plug the other end of the cable into the EC/MAC socket on the microscope. Choose Mode > EFM. Keysight 5500 SPM User’s Guide 5-25...
Page 160 The AC signal oscillation will be set to this value plus the specified Offset. Q Control can be used with EFM Mode to improve the resonance peak N OT E and image quality. See Chapter 6 for more on Q-Control. Keysight 5500 SPM User’s Guide 5-26...
Page 161 Set the Gain, which multiplies the output of the lock-in by the selected factor. Use a larger multiplier to improve signal-to-noise ratio for a small signal. Ensure that the gain will not result in an Keysight 5500 SPM User’s Guide 5-27...
Page 162 The Aux 1 map will show changes in the electrostatic force as they differ from the force at the touch-down location. Adjust the Gain, Scan Speed, Resolution, etc., to optimize the topography image. For more on advanced options for EFM Mode see Chapter Keysight 5500 SPM User’s Guide 5-28...
Page 163: Kelvin Force Microscopy (Kfm)
Figure 7-15 Advanced AC Mode Controls Other tab Set the I and P gains for the Servo to 1 %. In the Realtime Images window, choose to display images for Topography, Phase and SP (the output from the servo). Keysight 5500 SPM User’s Guide 5-29...
Page 164 SP servo and typically has a value of less than 0.05. The servo values should now be optimized. Stop the Spectroscopy. On the Lock-in 2 tab, select the From Servo check box. For more on advanced options for KFM Mode see Chapter Keysight 5500 SPM User’s Guide 5-30...
Page 165: Force Spectroscopy
Contact vs AC Mode. The choice of scanning prior to taking force measurements also is user-dependent. If AC Mode is chosen, note that the Contact Mode Sweep check box in the Spectroscopy window Advanced tab may be used so the imaging Keysight 5500 SPM User’s Guide 5-31...
Page 166: Force Spectroscopy Procedure For Contact Mode
Set the Setpoint to 0 V. Maximize the Range by entering a very large number (ie. 999) and PicoView will adjust to the maximum value for the scanner. Figure 7-17 Initial Servo settings for Force Spectroscopy Keysight 5500 SPM User’s Guide 5-32...
Page 167 In the Spectroscopy window, choose File > Set filename ..In the Save As dialog box, enter a filename for the data set. Note the file type will default to *.mi. Keysight 5500 SPM User’s Guide 5-33...
Page 168 Start the sweep by clicking the Start button. Stop measurements at any time by clicking the Stop button. After the initial sweep has completed, adjust the sweep range as needed using the Start/End parameters in the Spectroscopy Setup tab. Keysight 5500 SPM User’s Guide 5-34...
Page 169 Additional Imaging Modes An example of a closed loop Force vs Distance sweep is shown in Figure 7-19. Figure 7-19 Closed loop force spectroscopy example Keysight 5500 SPM User’s Guide 5-35...
Page 170: Flexgrid Spectroscopy
Set Gains as needed for the sample. Set the Setpoint to 0 V. Maximize the Range by entering a very large number (ie. 999) and PicoView will adjust to the maximum value for the scanner. Keysight 5500 SPM User’s Guide 5-36...
Page 171 Start value (ie 999) and PicoView will adjust to the maximum value for the scanner. Enter a large negative number for the End value (ie. -999) and PicoView will adjust to the minimum value for the scanner. Keysight 5500 SPM User’s Guide 5-37...
Page 172 (as shown in Figure 7-22). Figure 7-22 FlexGrid tab of the Spectroscopy window with specific points in the topographic image selected using the Add Point tool. Keysight 5500 SPM User’s Guide 5-38...
Page 173 (Figure 7-23). To set what each window will display, select the desired spectroscopy and math plug-in inputs from the pull down menus. The lists will vary depending on the imaging mode. Keysight 5500 SPM User’s Guide 5-39...
Page 174 Additional Imaging Modes Figure 7-23 Plug-in Images window Keysight 5500 SPM User’s Guide 5-40...
Page 175: Volume Spectroscopy
Set Gains as needed for the sample. Set the Setpoint to 0 V. Maximize the Range by entering a very large number (ie. 999) and PicoView will adjust to the maximum value for the scanner. Keysight 5500 SPM User’s Guide 5-41...
Page 176 Start value (ie 999) and PicoView will adjust to the maximum value for the scanner. Enter a large negative number for the End value (ie. -999) and PicoView will adjust to the minimum value for the scanner. Keysight 5500 SPM User’s Guide 5-42...
Page 177 Start the sweep of the selected area by clicking the Scan Up or Scan Down buttons. Stop measurements at any time by clicking the Stop button. After the initial sweep has completed, adjust the sweep range as needed using the Start/End parameters in the Spectroscopy Setup tab. Keysight 5500 SPM User’s Guide 5-43...
Page 178 In the Plug-in Images window, click the “+” button to add to add up to eight windows. To set what each window will display, select the desired spectroscopy and math plug-in inputs from the pull down menus. The lists will vary depending on the imaging mode. Keysight 5500 SPM User’s Guide 5-44...
Page 179 Figure 7-27 Volume spectroscopy plug-in windows with inputs selected The results of volume spectroscopy plug-in analysis and two dimensional maps of material properties are shown in Figure 7-28. Figure 7-28 Output of volume spectroscopy plug-in window analysis Keysight 5500 SPM User’s Guide 5-45...
Page 180: Scanner Maintenance And Calibration
Keysight 5500 SPM User’s Guide Scanner Maintenance and Calibration Care and Handling of the Probes and Scanner Probes Nose Assembly Two-Piece Nose Cone Cleaning Scanner Scanner Characteristics Non-Linearity Sensitivity Other Characteristics Cross Coupling Aging Creep Calibrating the Multi-Purpose Scanner X Calibration...
Page 181 Scanner Maintenance and Calibration Keysight scanners are designed for years of consistent, worry-free operation. However, scanners contain extremely delicate components and must be treated with care to maintain their high level of operation. This chapter discusses regular maintenance of the scanner, nose assemblies and probes, as well as regular calibration procedures for the multi-purpose, open-loop scanner.
Page 182: Care And Handling Of The Probes And Scanner
(dry, wetted with water, or with ethanol). The glass is glued to the nose assembly with chemically resistive epoxy, so if the window breaks there is no easy way to replace it and the entire Keysight 5500 SPM User’s Guide...
Page 183: Scanner
Keysight recommends that scanners be stored in a desiccator. Use care when moving the scanner on its assembly stand as it is not secured to the stand and can be damaged if dropped.
Page 184: Non-Linearity
Though they are explained separately for simplicity, they may not be independent of each other. All Keysight scanners are calibrated before shipment and installation. A unique calibration file is provided with each system, as is a “generic” calibration file, which is not scanner-specific.
Page 185: Other Characteristics
(Z). Systems using tube scanners are more susceptible to geometric cross coupling because a single four-quadrant tube provides motion in all the three axes. The larger Keysight multi-purpose scanners, with 90 micron X/Y scan range, use separate piezoelectric elements for X/Y movement and for Z movement.
Page 186: Creep
Creep appears as elongation of the feature in the direction of the offset because of this slow movement (Figure 8-3). Figure 8-3 Scanner creep Keysight 5500 SPM User’s Guide...
Page 187: Calibrating The Multi-Purpose Scanner
Scanner Maintenance and Calibration Calibrating the Multi-Purpose Scanner Regular calibration ensures that Keysight multi-purpose scanners will provide high performance imaging for many years of service. The following calibration procedure is recommended once or twice per year, if the system is moved, and before critical measurements.
Page 188: Calibration
Scanner Maintenance and Calibration X Calibration In the Realtime Images window, set up two Topography images, one for Trace and one for Retrace (Figure 8-4). Figure 8-4 Images of calibration target during Trace and Retrace Keysight 5500 SPM User’s Guide...
Page 189: Non-Linearity
Section. Use markers to report the dimensions between sets of features at either end of the scan range (Figure 8-6). Figure 8-6 Horizontal cross-section tool used to check non-linearity. Two sets of cursors are shown. Keysight 5500 SPM User’s Guide 5-10...
Page 190: Hysteresis
Trace and Retrace scans. X Hysteresis Place a vertical cursor at the same location in the Trace and Retrace images. The cursor should cross the same features in both images. If this Keysight 5500 SPM User’s Guide 5-11...
Page 191 Scanner Maintenance and Calibration is not the case, as in Figure 8-8, increase the X Hysteresis value and re-scan. Figure 8-8 Misalignment between trace and retrace Keysight 5500 SPM User’s Guide 5-12...
Page 192: Sensitivity
X Sensitivity Using the Cross Section tool from the Realtime Images window, measure the length of a set of features across the scan (Figure 8-10). Figure 8-10 Cross-section of several features to check X Sensitivity Keysight 5500 SPM User’s Guide 5-13...
Page 193: Y Calibration
Obtain an image of the calibration target. Using the Cross Section tool, set markers at the uppermost and bottommost feature along a vertical cross section (Figure 8-11). Figure 8-11 Cross-section in Y direction showing non-linearity Keysight 5500 SPM User’s Guide 5-14...
Page 194: Y Hysteresis
Trace and Retrace scans. Y Hysteresis The next step will be to adjust the Y Hysteresis term. Assign one data channel to display a single frame of the calibration target and place a Keysight 5500 SPM User’s Guide 5-15...
Page 195: Y Sensitivity
Using the Vertical Cross Section tool in the Realtime Images window (from the Tools menu or Toolbar), measure the top-to-bottom distance of a set of features across the scan (Figure 8-14). Figure 8-14 Cross-section of several features to check Y sensitivity Keysight 5500 SPM User’s Guide 5-16...
Page 196: Non-Orthogonality
Figure 8-15 Angle measurement for calibrating Non-orthogonality Adjust the Non-orthogonality term in the Open Loop tab of the Scanner Setup dialog box until the angle measures as close to 90 ° as possible for Keysight 5500 SPM User’s Guide 5-17...
Page 197: Z Calibration
Figure 8-17 Cross-section checking feature height for Z sensitivity It is important to correctly position the markers for the Z feature measurement. Place them in the center of the scan range. It may also be Keysight 5500 SPM User’s Guide 5-18...
Page 198: Servo Gain Multiplier
15 and 20 works well for most scanners. Archive the Calibration Files Copy the newly created calibration files to a disk for archive. Label the file with the scanner model, serial number and calibration date. Keysight 5500 SPM User’s Guide 5-19...
Page 199: Closed-Loop Scanners
Scanner Types Two types of closed-loop scanners are available for the Keysight 5500 SPM: Z-axis closed-loop, and X/Y/Z closed-loop. Z-Axis Closed-Loop Scanner The Z-axis closed-loop scanner provides exceptional Z-axis positioning for very linear vertical positioning.
Page 200: Calibration
Calibration Keysight recommends calibrating the Gains, Offset and Sensitivity settings in the Closed Loop tab of the Scanner Setup dialog box prior to each use of the closed-loop scanner. Begin by calibrating the scanner...
Page 201: And Y Sensor Calibration
Choose Controls > Setup > Microscope to confirm the appropriate microscope definition file. Verify that the correct scanner calibration file is selected in the Scanner menu. Choose Scanner > Edit to open the Scanner Setup dialog box. Select the Closed Loop tab. Keysight 5500 SPM User’s Guide...
Page 202 Gain are typical. Ensure that the Reverse check boxes are selected for X and Z Sensors. If not, contact Keysight support. Note that the scanner values will be different for each scanner. Verify that the Default CL Scan check box is cleared as shown above.
Page 203 For one image display Trace and for the other display Retrace. • Set both buffers to Main scan mode. Choose Tools > Realtime Cross Section so the individual scan lines will be displayed in the Cross Section window. Set the range to ±10 V. Keysight 5500 SPM User’s Guide...
Page 204 Click the Up or Down blue arrows in the Scan and Motor window to initiate a scan.When the scan is first started, the graph will probably look similar to that in Figure 9-4. Keysight 5500 SPM User’s Guide...
Page 205 Closed-Loop Scanners Figure 9-4 Initial plot before closed-loop scanner calibration Keysight 5500 SPM User’s Guide...
Page 206 Adjust the Offset to shift the line up or down until the left end is close to -10 V. Adjust the Gain to adjust the slope until the right end of the line is close to +10 V. Keysight 5500 SPM User’s Guide...
Page 207 Figure 9-5 Cross Section and Trace/Retrace windows after Offset and Gain values optimized In the Realtime Images window, change two image buffers to Y Sensor. Use the Vertical Cross Section tool to display a Y cross-section. Keysight 5500 SPM User’s Guide...
Page 208 The sensitivity ratio is the ratio of the closed loop sensor sensitivity to the open loop sensor sensitivity, and affects the forward correction feature. Open loop calibration can be performed for a small scan range Keysight 5500 SPM User’s Guide 5-10...
Page 209: Z Sensor Calibration
Save the Scanner Setup parameters. Z Sensor Calibration To calibrate the Z sensor, the output of the sensor will be plotted while the piezo is being moved through its entire range. Since only the motion Keysight 5500 SPM User’s Guide 5-11...
Page 210 Z Sensor: go to the Data Channel for the plot and select from the drop-down menu as shown below in Figure 9-6 on page 13. Set the units to V from the drop-down menu in the plot window. Keysight 5500 SPM User’s Guide 5-12...
Page 211 Figure 9-6 Select Z Sensor and units for Z sensor calibration Click the blue triangle to start a continuous sweep of the Z piezo. A warning message will be displayed. Click Yes to proceed with the calibration procedure. Keysight 5500 SPM User’s Guide 5-13...
Page 212 Offset to change the vertical position of the lines until their left edge is as close to -9.8 V as possible. Adjust the Gain to change the slope of the lines until they meet in the upper right corner. Keysight 5500 SPM User’s Guide 5-14...
Page 213 Figure 9-8: Figure 9-8 Spectroscopy sweep with closed loop On In the Scanner Setup Closed Loop tab, adjust the Z Range setting to maximize the range. A typical starting value is 19 V. Keysight 5500 SPM User’s Guide 5-15...
Page 214 Enter the new Z Sensitivity value into the Scanner Setup dialog box. Image the same pit again and check that the depth is now measured at 200 nm. If not, repeat the previous steps until the value is measured correctly. Keysight 5500 SPM User’s Guide 5-16...
Page 215 Closed-Loop Scanners Save the calibration file. X/Y/Z calibration is now complete. Keysight 5500 SPM User’s Guide 5-17...
Page 216: Mac Mode
Keysight 5500 SPM User’s Guide MAC Mode List of MAC Mode Components 10-1 Connections 10-2 Hardware and Sample Setup 10-4 The MAC Mode controller provides high precision AC signal control for AAC and MAC modes. The MAC controller uses a lock-in amplifier to generate the AC signal.
Page 217 MAC Mode Please contact Keysight if any of these items are missing. Connections The MAC Mode controller is shown in Figure 10-1. The rear panel is shown in Figure 10-2. Figure 10-1 Front panel of the MAC Mode controller Figure 10-2 MAC Mode controller rear panel The connectors are as follows: MAC drive output.
Page 218 Connect the MAC cable connector of the EC/MAC cable (Figure 6-7 on page 11) to the 6-pin connector on the sample plate using the MAC cable (Figure 6-8 Keysight 5500 SPM User’s Guide...
Page 219 MAC Mode controller, through the HEB to the microscope. Upon startup, the software may instruct you to update the system’s firmware. Follow the on-screen instructions to do so. Keysight 5500 SPM User’s Guide...
Page 220: Mac Iii
The MAC III controller adds imaging modes, routing capabilities and other experimental controls for applications requiring additional flexibility in experiment design. MAC III works with the Keysight 5500 SPM as either an option or an upgrade. It offers the best control available for oscillating probe technology, providing, among other things, far better resolution in fluids than other techniques.
Page 221: Initial Setup
• RS-232 (serial) cable. • MAC and/or AAC probes. • Top MAC option (includes Top MAC nose assembly and standard sample plate) or MAC option (includes MAC mode sample plate and 3-6 pin MAC cable). Keysight 5500 SPM User’s Guide...
Page 222: Connections
MAC III Please contact Keysight if any of these items are missing. Connections The MAC III controller is shown in Figure 11-1. The rear panel is shown in Figure 11-2. Figure 11-1 Front panel of the MAC III Controller. Figure 11-2 Rear panel of the MAC III Controller.
Page 223 MICROSCOPE connection on the MAC III controller to the CONTROLLER connector on the Head Electronics box (HEB). The HEB is meant to be placed on top of the MAC III box. Use a DB44 Keysight 5500 SPM User’s Guide...
Page 224 AUX The AUX connector has the drive output from each lock-in, a drive-in that can be summed into each lock-in, and an auxiliary input to each lock-in. The pin-out diagram is shown in Figure 11-3: Figure 11-3 AUX Connector pin-out diagram Keysight 5500 SPM User’s Guide...
Page 225: Hardware And Sample Setup
The Auxiliary Signal Access Box (ASAB) can be used in the development of novel capabilities for the examination of local mechanical and electromagnetic properties. The box is shown in Figure 11-4 and described in Table 4. Specific examples Keysight 5500 SPM User’s Guide...
Page 226 To enable summing of this external drive input to any of the lock-in drive outputs, open the Advanced AC Mode Controls window, select the appropriate tab of the lock-in amplifier and select the Sum External Drive check box. Keysight 5500 SPM User’s Guide...
Page 227 The output is nominally in the range of ±10 V. A DC bias can Drive Output also be added by entering a voltage for the Drive Offset in the Lock-in 3 tab in the Advanced AC Mode Controls window. Keysight 5500 SPM User’s Guide...
Page 228 For applying EFM and KFM FM modes, Lock-in 1 is used for the Z servo, Lock-in 2 is drives the tip or sample bias, and Lock-in 3 can be used to monitor second or third harmonics for the Lock-in 2 frequency. Figure 11-5 Wiring diagram for FM-KFM mode Keysight 5500 SPM User’s Guide...
Page 229 III Aux connector to the MAC/AACIII Aux Connector. This is shown as the red line in Figure 11-6 on page 11. Next connect a 6 foot BNC cable from ASAB Lock-in Amplifier 2 Drive Output to the sample plate connector adapter, as shown by the Keysight 5500 SPM User’s Guide 5-10...
Page 230: Mac Iii Software Controls
The procedures and descriptions in this User Guide are for PicoView N OT E 1.10x and higher. Keysight 5500 SPM User’s Guide 5-11...
Page 231: Simplified Software Control Options
To use the MAC III controller as the AC source choose Controls > Setup > Components, then select the Serial Port AC Mode Controller check box. The system will now use the drive signal from the MAC III controller, through the HEB to the microscope. Whenever Keysight 5500 SPM User’s Guide 5-12...
Page 232 The amplitude of the lock-in drive signal, stated as a percentage (0-100 %) of the maximum available 10 V. Frequency (kHz) Displays the frequency of the lock-in signal. From the AC Tune window you can sweep the Keysight 5500 SPM User’s Guide 5-13...
Page 233 When you initiate the approach, the Amplitude 1 and Phase 1 signals will be routed through the Deflection and Friction channels, respectively, to the main controller. During the laser and detector alignment procedure the Pass Through check boxes will be selected to Keysight 5500 SPM User’s Guide 5-14...
Page 234: Stm
DLFM should never be used for imaging in liquid. Choose Mode > DLFM, then choose Controls > AC Mode to open the DLFM Controls window: Figure 11-8 DLFM Controls window Keysight 5500 SPM User’s Guide 5-15...
Page 235: Fmm
These signals can be viewed by selecting Aux 1 or Aux 2 from the drop-down list in the Realtime Images window. In Force Modulation Mode, Lock-in 1 provides the oscillating signal driving the cantilever. The amplitude of cantilever modulation that Keysight 5500 SPM User’s Guide 5-16...
Page 236 Multiplies the output of the lock-in by the selected factor. Use a larger multiplier to improve the signal-to-noise ratio for a small signal. Ensure that the gain will not result in an amplitude exceeding Keysight 5500 SPM User’s Guide 5-17...
Page 237: Efm
Deflection channel as its Input. The actual Deflection input during scanning is the oscillation amplitude. For EFM mode, the Bias switch on the back of the Head Electronics N OT E Box must be set to Tip. Keysight 5500 SPM User’s Guide 5-18...
Page 238 Multiplies the output of the lock-in by the selected factor. Use a larger multiplier to improve the signal-to-noise ratio for a small signal. Ensure that the gain will not result in an amplitude exceeding Keysight 5500 SPM User’s Guide 5-19...
Page 239 Two rules typically apply: • The frequency should not be an integral factor of the Lock-in 1 frequency. • The frequency should not be close (within 10-20 kHz) to the Lock-in 1 frequency. Keysight 5500 SPM User’s Guide 5-20...
Page 240: Kfm
Deflection channel as its Input. A DC bias is provided by an internal servo mechanism to counter electrostatic forces on the tip. For KFM mode, the Bias switch on the back of the Head Electronics N OT E Box must be set to Tip. Keysight 5500 SPM User’s Guide 5-21...
Page 241 (0-100 %) of the maximum available 10 V. Frequency (kHz) Displays the frequency of the Lock-in 1 signal. From the AC Tune window you can sweep the frequency of Lock-in 1, to determine the Keysight 5500 SPM User’s Guide 5-22...
Page 242 As mentioned, Lock-in 2 is used as the source for the AC tip bias. You will typically need to sweep the frequency of Lock-in 2 to ensure that the electrical response of the cantilever does not interfere with the Keysight 5500 SPM User’s Guide 5-23...
Page 243: Advanced Software Control Options
Advanced Software Control Options The Advanced AC Mode property sheet gives you more signal routing and control options than the simplified options described above. To view the AC Mode settings, choose Controls > Advanced > AC Mode. Keysight 5500 SPM User’s Guide 5-24...
Page 244: Lock-In Tabs
The amplitude of the Lock-in 1 drive signal, stated as a percentage (0-100 %) of the maximum available 10 V. Frequency (kHz) Displays the frequency of the Lock-in 1 signal. From the AC Tune window you can Keysight 5500 SPM User’s Guide 5-25...
Page 245 1. Drive Offset Applies an offset, in volts, to the drive signal. The default value is 0. Select the From Servo check box to add the output from the MAC III internal servo loop Keysight 5500 SPM User’s Guide 5-26...
Page 246 Y Component from AUX Select this check box to replace the Y signal with the AUX input. This option essentially converts the lock-in to an A/D converter, providing a quick method for measuring an Keysight 5500 SPM User’s Guide 5-27...
Page 247: Outputs Tab
Routes the output from one of the three lock-in signals to the circuit controlling oscillation of the cantilever (either AAC or MAC, depending on your setup). Set this option to GND to turn off the output Keysight 5500 SPM User’s Guide 5-28...
Page 248 These are the default settings. Ref Set Ref Set is the set point for the electrochemistry potentiostat. First, select the Lock-in. Select the Sum check box to add the Lock-in signal to the Ref Set value; clear Keysight 5500 SPM User’s Guide 5-29...
Page 249 In KFM Mode, the SP (Surface Potential) channel is set to Servo Output N OT E and the Pass Through check box is cleared. The Servo Output is the DC bias produced by the servo to counteract the sample bias. Keysight 5500 SPM User’s Guide 5-30...
Page 250: Other Tab
Routes the Amplitude, Phase, X Component or Y Component from the three lock-in signals to the MAC III servo input. This is the signal that the servo will maintain at the selected Setpoint. Selecting Keysight 5500 SPM User’s Guide 5-31...
Page 251 AC Tune window. Only one lock-in can be swept at a time. Reverts to Lock-in 1 when AutoTune is selected in the AC Tune window. Use Manual Tune to sweep the other lock-ins. Keysight 5500 SPM User’s Guide 5-32...
Page 252: Amplitude And Frequency Modulation Techniques
The ASAB can be used in the development of novel capabilities for the examination of local mechanical and electromagnetic properties. This Keysight 5500 SPM User’s Guide 5-33...
Page 253 The routing of AUX input channels of the second lock-in amplifier and third lock-in amplifier to the BNC2 connector is used for most of the EFM and KFM applications. Typically, this configuration is used for the hardware setup (connections detailed in “Connections for ASAB" Keysight 5500 SPM User’s Guide 5-34...
Page 254 For tuning a KFM probe, Autotune can be performed from the KFM mode environment. For AM mode, it is generally beneficial to tune the cantilever below the resonant frequency. For FM mode, better results are achieved tuning the cantilever 200–300 Hz above the resonant Keysight 5500 SPM User’s Guide 5-35...
Page 255: Setting Parameters For Am Mode Operation
Parameters for FM Mode Operation" on page 40. Setting Parameters for Tracking Surface Topography The Lock-in 1 parameters should be the same for all applications. These settings will yield measurements in the intermittent contact regime. This Keysight 5500 SPM User’s Guide 5-36...
Page 256 This will turn on the AC bias to the tip. If the Amplitude 2 parameter (in the lower portion of the KFM tab) is less than 0.100 V, increase the Drive (%) or Gain 2. Keysight 5500 SPM User’s Guide 5-37...
Page 257 It may be necessary to adjust topography I and P gains if the KFM servo affects topography imaging. Often lowering the Amplitude Setpoint helps to stabilize the topography. Slower imaging speeds are recommended when using KFM. Keysight 5500 SPM User’s Guide 5-38...
Page 258 Servo Setpoint slowly until it is horizontal. Figure 11-19 shows the SP sweep before and after the KFM Servo Setpoint has been adjusted. Note the difference in the vertical scale between before and after. Keysight 5500 SPM User’s Guide 5-39...
Page 259: Setting Parameters For Fm Mode Operation
(ASAB). Connect the ASAB to the controller as shown in Figure 11-5 on page 9. The ASAB is connected to the auxiliary serial port on the back of the MAC III. A BNC cable should connect the Keysight 5500 SPM User’s Guide 5-40...
Page 260 KFM Controls window can be used to optimize the KFM parameters. The default parameters for FM are shown in Figure 11-20. Figure 11-20 KFM tab initial settings for FM mode operation Keysight 5500 SPM User’s Guide 5-41...
Page 261 It may be necessary to adjust topography I and P gains if the KFM servo affects topography imaging. Often lowering the Amplitude Setpoint helps to stabilize the topography. Slower imaging speeds are recommended when using KFM. Keysight 5500 SPM User’s Guide 5-42...
Page 262: Piezoresponse Force Microscopy
DC bias or the frequency of the AC signal applied to the sample via the tip. This technique can also be used to study hysteretic characteristics of the piezoresponse. Keysight 5500 SPM User’s Guide 5-43...
Page 263: Liquid Cell
Keysight 5500 SPM User’s Guide Liquid Cell Liquid Cell with Standard Sample Plate 12-2 Liquid Cell with MAC Mode 12-4 Flow-Through Liquid Cell 12-4 The liquid cell enables in-situ AFM or STM imaging for better control under realistic environments. The cell is made from chemical-resistant polycarbonate and can be used with a wide variety of liquids.
Page 264: Liquid Cell With Standard Sample Plate
Prepare and place the sample on the sample plate. Place the sample plate on the microscope. Using the Close switch on the Head Electronics Box, and watching the video system, roughly approach the sample such that the tip and Keysight 5500 SPM User’s Guide...
Page 265 If necessary, readjust the photodetector position to account for the change of laser location caused by the liquid. Approach and contact the sample. Keysight 5500 SPM User’s Guide...
Page 266: Liquid Cell With Mac Mode
A liquid cell is also available with connections allowing liquid to flow continuously through the cell. The connections should be made with 1 mm OD Teflon tubing, cut at a sharp angle for insertion into the cell. Keysight 5500 SPM User’s Guide...
Page 267: Cantilevers For Temperature Controlled Imaging
Tips for Temperature Controlled Imaging 13-22 Several temperature control sample plates are available for use with the Keysight 5500 SPM. With temperature control, studies can be done while maintaining physiological temperature, for melting experiments, etc. Cantilevers for Temperature Controlled Imaging Uncoated silicon cantilevers are recommended for imaging under temperature control.
Page 268: High Temperature Sample Plates
(Figure 13-1) provides a temperature range from ambient to 250 C. Figure 13-1 5500 standard hot sample plate The Hot MAC sample plate (Figure 13-2) provides temperatures from ambient to 110 C and enables imaging in MAC Mode.
Page 269 Temperature Control Sample plates from the 7500 and 9500 systems are compatible with the 5500. Figure 13-3 7500/9500 standard hot sample plate Figure 13-4 7500/9500 hot MAC sample plate Keysight 5500 SPM User’s Guide...
Page 270 Lakeshore Control Setup menu should be set to 100W Plat/500. Figure 13-5 Lakeshore temperature controller The ramping rate should be keep below 10 degrees per minute to avoid C A U T I ON damaging the plate. Keysight 5500 SPM User’s Guide...
Page 271: Connections
Figure 13-6 High temperature sample plate cables The Hot MAC sample plate also includes a Y connector for the MAC cable (Figure 13-7). Figure 13-7 Hot MAC sample stage Y cable. Keysight 5500 SPM User’s Guide...
Page 272 Figure 13-11 shows the wiring for the hot MAC sample plate. The connection at the end of Cable 1 enables wiring to the temperature stages through a port in the environmental chamber. Fold the straight Keysight 5500 SPM User’s Guide...
Page 273 Then screw the round connector into the port to make a tight seal. Figure 13-9 5500 hot sample plate wiring diagram Keysight 5500 SPM User’s Guide...
Page 274 Temperature Control Figure 13-10 7500/9500 hot sample plate wiring diagram Keysight 5500 SPM User’s Guide...
Page 275 Temperature Control Figure 13-11 5500 hot MAC sample plate wiring diagram Keysight 5500 SPM User’s Guide...
Page 276 Temperature Control Figure 13-12 7500/9500 hot MAC sample plate wiring diagram Keysight 5500 SPM User’s Guide 5-10...
Page 277: Imaging
Set the Ramp Rate to no more than 10 degrees per minute (5 degrees/minute is a typical ramp rate). Press the Heater Range button and select Low, Medium or High. Keysight 5500 SPM User’s Guide 5-11...
Page 278 Image as usual. Imaging during temperature ramp is possible provided care is taken to compensate for sample thermal expansion. Monitor the Z-piezo position as the temperature increases to determine if/when it goes out of range. Keysight 5500 SPM User’s Guide 5-12...
Page 279: Peltier (Cold Mac) Sample Plate
-5 to 40 C. Figure 13-14 Peltier (Cold MAC) sample plate. Sample plates from the 7500 and 9500 systems are compatible with the 5500 system. Figure 13-15 7500/9500 Peltier (Cold MAC) sample plate (bottom view) Keysight 5500 SPM User’s Guide 5-13...
Page 280 13-16) is used to drive the Peltier sample plate temperature. The booster includes a safety device that shuts off the power if the reverse side of the Peltier becomes excessively hot. Figure 13-16 Current booster Keysight 5500 SPM User’s Guide 5-14...
Page 281: Connections
Peltier sample plate: Figure 13-17 Peltier sample plate cables The Peltier sample plate also connects to MAC cables for use with MAC Mode (Figure 13-18). Figure 13-18 MAC cable for Peltier sample plate Keysight 5500 SPM User’s Guide 5-15...
Page 282 Figure 13-19 Y cable for use with 7500/9500 sample plates Figure 13-20 shows the required wiring for the Peltier sample plate. MAC Mode is optional and the figure below shows the setup with the Keysight 5500 SPM User’s Guide 5-16...
Page 283 MAC Mode option. The connection at the end of Cable 1 enables wiring to the temperature stages through a port in the environmental chamber. Figure 13-20 5500 Peltier (Cold MAC) sample plate wiring diagram Keysight 5500 SPM User’s Guide 5-17...
Page 284 Temperature Control Figure 13-21 5500 Peltier (Cold) sample plate wiring diagram Keysight 5500 SPM User’s Guide 5-18...
Page 285 Temperature Control Figure 13-22 7500/9500 Peltier (Cold MAC) sample plate wiring diagram Keysight 5500 SPM User’s Guide 5-19...
Page 286: Water Cooling
-30 C. Connect the water-cooling system and test for leaks before making any C A U T I ON electronic connections or turning on any components. Keysight 5500 SPM User’s Guide 5-20...
Page 287: Imaging
Setting the temperature to ambient avoids this problem. Set the Ramp Rate to no more than 10 degrees per minute (5 degrees/minute is a typical ramp rate). Turn the Range control on the current booster to maximum (fully clockwise). Keysight 5500 SPM User’s Guide 5-21...
Page 288: Tips For Temperature Controlled Imaging
Purging the environmental cell with a dry gas such as nitrogen will help control the sample environment if condensation from cooling to below the dew point becomes an issue. Keysight 5500 SPM User’s Guide 5-22...
Page 289 Keysight 5500 SPM User’s Guide Thermal K Thermal K Calibration 14-3 Thermal K Setup 14-3 Spring Constant Calibration 14-4 It is sometimes necessary to know the spring constant of an AFM probe. This chapter reviews the calibration method using Thermal K to determine spring constants.
Page 290 Consequently, in order to accurately quantify material compliance or molecular interactions with the AFM, the spring constant for each probe should be determined by empirical or semi-empirical methods. Keysight 5500 SPM User’s Guide...
Page 291: Thermal K Calibration
Thermal K Thermal K Calibration Thermal K is an option for the Keysight AFM that allows the user to quickly and easily calculate the spring constant of an AFM probe. The Keysight Thermal K method calculates AFM probe spring constants by...
Page 292: Spring Constant Calibration
In the Spectroscopy window, confirm Force vs Distance for the plot type (Figure 14-2). In the Spectroscopy Basic tab, click on the 1 button to do a single sweep. Figure 14-2 Spectroscopy window showing Force vs Distance selected Keysight 5500 SPM User’s Guide...
Page 293 Right-click on the ruler after the end points are set and select Deflection Sensitivity (Figure 14-4) to update the value in the Advanced tab. Figure 14-4 Advanced tab in the Spectroscopy window Click the Thermal K... button in the Advanced tab of the Spectroscopy window. Keysight 5500 SPM User’s Guide...
Page 294 Averages to 10. Chose the correct cantilever shape from the drop-down menu. Temperature to the correct ambient temperature in Celsius. Click the Full button on the right side of the Thermal K window. Click the Plot button. Keysight 5500 SPM User’s Guide...
Page 295 The Thermal K window will refresh, showing the PSD across the frequency range, and a best fit curve in red. The area under the curve is integrated Keysight 5500 SPM User’s Guide...
Page 296 The Force Constant should now be updated in the Spectroscopy Advanced tab. Change the plot window to display Force units if needed: In the Spectroscopy plot window, click on the units and select nN from the drop-down menu as shown in Figure 14-8: Keysight 5500 SPM User’s Guide...
Page 297 Thermal K Figure 14-8 Select units after calibrating the Force Constant Keysight 5500 SPM User’s Guide...
Page 298 Thermal K Once the units have been selected, measurements can be taken on subsequent force curves as shown in Figure 14-9: Figure 14-9 Force curve with calibrated measurements Keysight 5500 SPM User’s Guide 5-10...
Page 299: Environmental Chamber Glove Box
Keysight 5500 SPM User’s Guide Environmental Control Environmental Chamber 15-1 Glove Box 15-3 In addition to the vibration isolation chamber mentioned earlier in this User’s Guide, two other options are available to let you control the atmosphere for sample preparation and/or imaging.
Page 300 Several types of screw-in fittings are available from Keysight for wires, liquids or 3 mm (1/8 in) inner diameter gas tubing. The ports can be used in any combination. For example, one gas port may be used to introduce a gas while another simultaneously vents the chamber (i.e., when the gas cannot be safely...
Page 301 Glove Box The glove box lets you create a controlled environment for both sample preparation and imaging. As with the environmental chamber, the glove box includes eight ports for introducing gases, liquids or wires into the Keysight 5500 SPM User’s Guide...
Page 302 0C. The gloves are heavy duty, 15 mil Latex. Figure 15-3 Glove Box The 5500 SPM mounts directly to the top of the box’s stainless steel mounting plate, with the stage motor screws and sample plate extending into the box.
Page 303 Keysight 5500 SPM User’s Guide Electrochemistry Equipment 16-3 Liquid Cell 16-3 Electrodes 16-3 Working Electrode and Pogo Electrode 16-4 Reference Electrode 16-4 Counter Electrode 16-4 Cleaning 16-5 Liquid Cell Cleaning 16-5 Non-Critical Applications 16-5 Critical Applications 16-6 Electrode Cleaning 16-6...
Page 304 Figure 16-1 shows a typical electrochemistry setup, while Figure 16-2 shows that same setup created with the 5500 SPM liquid cell. Note that electrochemistry experiments can be conducted using either AFM Modes or STM Mode. Figure 16-1 Electrochemistry experiment schematic...
Page 305: Equipment
Electrodes Three electrodes are typically required for electrochemistry experiments. The experiment being performed will determine the type of wire to be used for the reference and counter electrodes. The type of Keysight 5500 SPM User’s Guide...
Page 306: Working Electrode And Pogo Electrode
Electrochemistry wire will affect the voltage readings. Prepared electrodes may be purchased from Keysight Technologies, or wires may be formed into appropriate electrodes using the following approximate dimensions. Working Electrode and Pogo Electrode Contact between the working electrode (WE) on the sample plate and...
Page 307: Cleaning
The liquid cell should be cleaned prior to every use according to these instructions: Non-Critical Applications Sonicate the liquid cell in laboratory detergent. Rinse in 18 MW/cm water. Rinse in methanol. Blow dry under argon or nitrogen gas. Keysight 5500 SPM User’s Guide...
Page 308: Electrode Cleaning
Place a clean substrate onto the sample plate. Push the liquid cell onto the spring-loaded pins on the sample plate. Verify that the O-ring is in contact with the substrate at all points. Keysight 5500 SPM User’s Guide...
Page 309 Connect the sample plate to the microscope using the 3-pin EC cable connector of the EC/MAC Cable. Load the sample plate onto the microscope. Approach the sample. Keysight 5500 SPM User’s Guide...
Page 310: Troubleshooting
Sample Potential = Sample Bias + Probe Potential. The only two independently-controlled potentials are WE and VEC = WE - RE IEC = Current into or out of the working electrode. Positive is flowing into the working electrode. Keysight 5500 SPM User’s Guide...
Page 311: Software Controls
PicoView User Guide. Choose Controls > Electrochemistry from the PicoView main window, or click on the Electrochemistry icon from the toolbar button to open the Electrochemistry window (Figure 16-6). Figure 16-6 Electrochemistry window overview Keysight 5500 SPM User’s Guide...
Page 312: Guidelines For Electochemistry
In the Electrochemistry window, choose File > Set filename ..In the Save As dialog box, enter a filename for the data set. Note the file type will default to *.mi. Keysight 5500 SPM User’s Guide 5-10...
Page 313 Auto Save is on, circled in red in Figure 16-8. It will also be indicated by a check mark next to Auto Save in the Electrochemisty File menu. Figure 16-8 Auto Save turned on for Electrochemistry experiments Keysight 5500 SPM User’s Guide 5-11...
Page 314: Secm - Scanning Electrochemical Microscopy
Electrochemistry SECM - Scanning Electrochemical Microscopy Scanning Electrochemical Microscopy (SECM) is an optional addition to the electrochemical capabilities of the Keysight 5500 (and 7500) AFM systems. Figure 16-9 Block diagram of combined AFM-SECM system. The control of the sample potential is optional. If necessary it can be controlled using the built in bipotentiostat as illustrated.
Page 315 HEB with the standard 44-pin cable. Figure 16-10 SECM Adapter (left) and adapter connected to AFM Base (right). Assemble the 5500 SECM nose cone (details below). Insert assembled nose cone into scanner. Mount the scanner in the base and align the laser to the cantilever and detector in air, again, just as in standard Contact mode.
Page 316: Assembling The Secm Nose Cone
Assembling the SECM Nose Cone The SECM probe comes pre-mounted on a cartridge for easy placement into the 5500 nose cone. Figure 16-11 SECM nose cone and probe cartridge The procedure to assembly the SECM nose cone is as follows.
Page 317 SECM experiments. Position the end of the wire between the base contact and set screw in the nose cone as seen in Figure 16-13. Figure 16-13 Arrow indicates point of contact for probe wire. Keysight 5500 SPM User’s Guide 5-15...
Page 318 Use the supplied Allen key to tighten the set screw from the bottom of the nose cone, ensuring that secure contact is made with the wire. Figure 16-14 Using Allen key to secure wire to contact in nose cone. Keysight 5500 SPM User’s Guide 5-16...
Page 319: Secm Software Interface
The sample potential, however, can be either floating or controlled by the potentiostat. A typical experiment would be to sweep the tip potential, run CV on the electrode then set the tip potential to a proper Keysight 5500 SPM User’s Guide 5-17...
Page 320 For such experiment, the sweep potential in the control window above should be set to “tip” and the fixed potential should be set to “Sample”. Keysight 5500 SPM User’s Guide 5-18...
Page 321 Keysight 5500 SPM with MAC Mode, Force Modulation Imaging Keysight 5500 SPM with MAC III Option Keysight 5500 SPM with MAC III Option and Closed Loop Scanner The following pages contain wiring diagrams for several common configurations of the Keysight 5500 SPM.
Page 322: Keysight 5500 Spm Standard Wiring Diagram
Wiring Diagrams Keysight 5500 SPM Standard Wiring Diagram Figure A-1 Wiring diagram for Keysight 5500 standard configuration Keysight 5500 SPM User’s Guide...
Page 323: Keysight 5500 Spm With Mac Mode Controller
Wiring Diagrams Keysight 5500 SPM with MAC Mode Controller Figure A-2 Wiring diagram for Keysight 5500 SPM with MAC Mode Option Keysight 5500 SPM User’s Guide...
Page 324: Keysight 5500 Spm With Mac Mode, Force Modulation Imaging
Wiring Diagrams Keysight 5500 SPM with MAC Mode, Force Modulation Imaging Figure A-3 Wiring diagram for Keysight 5500 SPM with MAC Mode Option, Force Modulation imaging mode Keysight 5500 SPM User’s Guide...
Page 325: Keysight 5500 Spm With Mac Iii Option
Wiring Diagrams Keysight 5500 SPM with MAC III Option Figure A-4 Wiring diagram for Keysight 5500 SPM with MAC III Option Keysight 5500 SPM User’s Guide...
Page 326: Keysight 5500 Spm With Mac Iii Option And Closed Loop Scanner
Wiring Diagrams Keysight 5500 SPM with MAC III Option and Closed Loop Scanner Figure A-5 Wiring diagram for Keysight 5500 SPM with MAC III Option and Closed Loop Scanner option Keysight 5500 SPM User’s Guide...
Page 327 Waals, Creep, Force Modulation Microscopy, 1-13, 7-16 Cross coupling, Force Spectroscopy, 7-31 CSAFM Mode, 1-12, Friction, 1-14, 5-8, 7-13 Current booster, 13-14 Friction Force Microscopy, 1-14 Current Sensing AFM, 1-12, Friction signal, 4-24 Keysight 5500 SPM User’s Guide...
Page 328 Advanced software controls, 11-24 Components, 11-2 MAC Mode, 1-11, 6-1, 6-10, 6-14, 10-1 Cables, 10-2 Q Control, 6-13, 7-26, 7-39, 7-44 Components, 10-1 MAC option, 10-1 Sample setup, 10-4 Top MAC option, 10-1 With liquid cell, 12-4 Keysight 5500 SPM User’s Guide...
Page 329 Sensitivity, 8-5, 8-13, 8-16, 8-18 Servo Gain Multiplier, 8-19 STM scanner, STM scanner, inserting a tip, Scanning Probe Microscopy, Scanning Tunneling Microscopy, 1-5, Wiring, 3-12, 4-13, 7-16 Sensitivity, 8-5, 8-13, 8-16, 8-18, Working electrode, 16-4, 16-7, 16-8 Servo, Keysight 5500 SPM User’s Guide...

Keysight 5500 User Manual

Table of Contents

Specifications

Power Supply

1 Introduction to the Keysight 5500

Overview of Keysight SPM System

SPM Basics

SPM Techniques

2 Keysight 5500 Spm Components

2 Keysight 5500 SPM Components

Microscope

Probes

Nose Assembly

Scanner

Detector

Sample Plates

Video System

Head Electronics Box (HEB)

AFM Controller

Vibration Isolation Chamber

Software

System Options

3 Setting up the Keysight 5500 Spm

Component and Facility Dimensions

Facility Requirements

Assembling the Vibration Isolation Chamber

Connecting the Components

Guidelines for Moving the System

Care and Handling of the Probes and Scanner

4 Preparing for Imaging

Setting up the Scanner Assembly

Aligning the Laser

Mounting the Sample

Using the Video System

5 Contact Mode Imaging

6 AC Modes

6 AC Modes

Acoustic AC Mode (AAC)

Magnetic AC (MAC) Mode

Q Control

7 Additional Imaging Modes

Scanning Tunneling Microscopy (STM)

Current Sensing AFM (CSAFM)

Lateral Force Microscopy (LFM)

Dynamic Lateral Force Microscopy (DLFM)

Force Modulation Microscopy (FMM)

Magnetic Force Microscopy

Electrostatic Force Microscopy (EFM)

Kelvin Force Microscopy (KFM)

Force Spectroscopy

Flexgrid Spectroscopy

Volume Spectroscopy

8 Scanner Maintenance and Calibration

Care and Handling of the Probes and Scanner

Scanner Characteristics

Calibrating the Multi-Purpose Scanner

Archive the Calibration Files

Servo Gain Multiplier

Scanner Types Z-Axis Closed-Loop Scanner X/Y/Z Closed-Loop Scanner

9 Closed-Loop Scanners

Calibration

List of MAC Mode Components

List of MAC Mode Components Connections Hardware and Sample Setup

10 MAC Mode

Mac III

Initial Setup

MAC III Software Controls

Amplitude and Frequency Modulation Techniques

Piezoresponse Force Microscopy

12 Liquid Cell

13 Temperature Control

Cantilevers for Temperature Controlled Imaging

High Temperature Sample Plates

Peltier (Cold MAC) Sample Plate

Tips for Temperature Controlled Imaging

Thermal K Calibration

Environmental Chamber Glove Box

16 Electrochemistry

Equipment

Cleaning