Keysight 5500 User manual

Keysight 5500 Scanning Probe
Microscope
User’s Guide

Notices
© Keysight Technologies 2015
No part of this manual may be reproduced
in any form or by any means (including
electronic storage and retrieval or transla-
tion into a foreign language) without prior
agreement and written consent from Key-
sight Technologies as governed by United
States and international copyright laws.
Manual Part Number
N9410-90001
Edition
Rev H, December 2015
Printed in USA
Keysight Technologies
5301 Stevens Creek Blvd.
Santa Clara, CA 95051
Warranty
The material contained in this doc-
ument is provided “as is,” and is
subject to being changed, without
notice, in future editions. Further,
to the maximum extent permitted
by applicable law, Keysight dis-
claims all warranties, either
express or implied, with regard to
this manual and any information
contained herein, including but not
limited to the implied warranties of
merchantability and fitness for a
particular purpose. Keysight shall
not be liable for errors or for inci-
dental or consequential damages in
connection with the furnishing, use,
or performance of this document or
of any information contained
herein. Should Keysight and the
user have a separate written agree-
ment with warranty terms covering
the material in this document that
conflict with these terms, the war-
ranty terms in the separate agree-
ment shall control.
Technology Licenses
The hardware and/or software described
in this document are furnished under a
license and may be used or copied only in
accordance with the terms of such license.
Restricted Rights Legend
If software is for use in the performance
of a U.S. Government prime contract or
subcontract, Software is delivered and
licensed as “Commercial computer soft-
ware” as defined in DFAR 252.227-7014
(June 1995), or as a “commercial item” as
defined in FAR 2.101(a) or as “Restricted
computer software” as defined in FAR
52.227-19 (June 1987) or any equivalent
agency regulation or contract clause. Use,
duplication or disclosure of Software is
subject to Keysight Technologies’ stan-
dard commercial license terms, and
non-DOD Departments and Agencies of
the U.S. Government will receive no
greater than Restricted Rights as defined
in FAR 52.227-19(c)(1-2) (June 1987).
U.S. Government users will receive no
greater than Limited Rights as defined in
FAR 52.227-14 (June 1987) or DFAR
252.227-7015 (b)(2) (November 1995), as
applicable in any technical data.
Safety Notices
CAUTION
A CAUTION notice denotes a
hazard. It calls attention to an
operating procedure, practice, or
the like that, if not correctly per-
formed or adhered to, could result
in damage to the product or loss of
important data. Do not proceed
beyond a CAUTION notice until
the indicated conditions are fully
understood and met.
WARNING
A WARNING notice denotes a
hazard. It calls attention to an
operating procedure, practice,
or the like that, if not correctly
performed or adhered to, could
result in personal injury or
death. Do not proceed beyond a
WARNING notice until the indi-
cated conditions are fully
understood and met.

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N9410-90001 Keysight 5500 SPM User’s Guide iv
Read This First
Warranty
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. Replacement products may be
either new or like-new.
Keysight warrants that Keysight software will not fail to execute its
programming instructions for the period specified above due to defects
in material and workmanship when properly installed and used. If
Keysight receives notice of such defects during the warranty period,
Keysight will replace software media which does not execute its
programming instructions due to such defects. For detailed warranty
information, see back matter.
Safety Considerations
• General - This product and related documentation must be reviewed
for familiarization with these safety markings and instructions before
operation.
This product is a safety Class I instrument (provided with a
protective earth terminal).
• Before Applying Power - Verify that the product is set to match the
available line voltage and the correct fuse is installed. Refer to
instructions in “Facility Requirements" on page 4 of the manual.
• Before Cleaning - Disconnect the product from operating power
before cleaning.
• Safety Earth Ground - An uninterrupted safety earth ground must
be provided from the main power source to the product input wiring
terminals or supplied power cable.

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N9410-90001 Keysight 5500 SPM User’s Guide v
Specifications
Environmental Conditions
Temperature (Operating): 5 to 40 °C
Temperature (Non-operating): -40 to 70 °C
Relative Humidity (Operating): 15 to 95 % non-condensing
Altitude: 2000 m
Power Requirements
100/120/220/240 VAC, 50/60 Hz
Mains supply voltage fluctuations are not to exceed 10 % of the nominal
supply voltage.
Equipment Class I, Pollution Degree 2, Installation Category II.
This equipment is for indoor use only.
When the product is subjected to 8 kV air discharge or 4 kV contact
discharge in accordance with IEC 61000-4-2, interruption of the laser
output may occur.
If this happens, laser power must be re-cycled in order to resume normal
operation. CAUT
NOTE These specifications apply to the Keysight 5500 system, and do not
guarantee the function of an experiment (including the cantilever) in
these conditions.
CAUTION Stop using the scanner if the scanner cable insulation is damaged in
order to avoid electrical shock. Have it repaired or replaced by the
factory.

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N9410-90001 Keysight 5500 SPM User’s Guide vi
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. The aperture in the AFM scanning head is labeled with the
logotype (shown below). DO NOT stare directly into the laser beam. To
ensure safe operation, the scanner must be operated and maintained in
accordance with the instructions included with the laser. The laser must
only be powered by a controller that includes an on/off switch, such as
the Keysight SPM Controller. DO NOT attempt to make any
adjustments to the laser, the laser’s electronics, or optics. If laser
malfunction is suspected, immediately return the scanner to Keysight
Technologies for repair or replacement; there are no user-serviceable
parts. WA
RN
WARNING Use of controls or adjustments or performance of procedures other
than those specified herein may result in hazardous light exposure.
Furthermore, the use of optical instruments with this product may
increase eye hazard.

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N9410-90001 Keysight 5500 SPM User’s Guide vii
In accordance with federal FDA requirements, one of the following
laser precautions is affixed to the scanner:
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.
Procedure for Changing Input Voltage
1Unplug the power cord from the Keysight AFM Controller.
2Remove the fuse holder located on the back of the controller.
3Underneath where the fuse holder was located is the input voltage
control switch. Pull out the switch and rotate it to the desired input
voltage 100/120/220/240 V.
4Reinsert the voltage switch with the desired voltage.
5Replace the fuse holder.
Piezo Scanner Precautions
Piezo scanners are, by nature, very FRAGILE pieces of equipment. The
piezo material that does the scanning is a ceramic and is consequently
quite easily broken. Dropping a piezo scanner will result in damage to
the scanner that can only be repaired by completely replacing the
scanner piezo core. This can be an expensive and time-consuming
process and so it is advised that the utmost care is used when handling
the scanners. Keysight Technologies recommends that the scanners be
stored in the padded scanner case that was supplied with the scanner and
that the scanner be kept in a dry environment when not in use. Piezo
scanners also perform better with consistent use. If a scanner is not used
for some time it may require a short period of use before the scan range
is stable and the calibration is correct. It may also be necessary to
re-calibrate the scanner from time to time. The calibration can be

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N9410-90001 Keysight 5500 SPM User’s Guide viii
verified using a calibration standard, and adjustments can be made using
the calibration tools.
General Care Requirements
SPM equipment is sensitive scientific equipment. Care must be used
when handling all parts. When removing scanners from the microscope
ensure that all cable connections to the scanner are disconnected. This
includes cables for photo-diode detectors. Also, the photo-diode
detector should be removed from the scanner prior to the removal of the
scanner from the microscope. All equipment, especially the sample
plates and scanner nose modules should be kept clean and free from
contamination when not in use. It is recommended, to prolong the life of
these items, that after use all sample plates and noses are cleaned
thoroughly and dried off prior to storage. Cleaning can be done using an
organic solvent. Please refer to the appropriate sections of the manual
for further information regarding the proper cleaning of equipment.
Disclaimers
This User’s Guide, as well as the hardware herein described, is licensed
and can only be used in compliance with such terms and agreements as
entered in by Keysight Technologies. Users of these products
understand, except where permission is given by Keysight Technologies
by said license, no part of this manual may be copied, transmitted,
stored in a general retrieval system, in any form or means, electronic, or
mechanical, without prior written permission of Keysight Technologies.
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.

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N9410-90001 Keysight 5500 SPM User’s Guide ix
Declaration of Conformity

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N9410-90001 Keysight 5500 SPM User’s Guide x
Contact Information
Keysight Technologies
5301 Stevens Creek Blvd., Santa Clara, CA 95051 U.S.A.
Tel: [phone] Fax: [phone]
E-mail: [email protected] Web: www.keysight.com
Customer Technical Support
Tel: [phone]
Fax: [phone]
E-mail: [email protected]
Technical Sales
Tel: [phone]
Fax: [phone]
E-mail: [email protected]
Distributors and Account Representatives
Please visit our web site for up-to-date information:
www.keysight.com/find/nano

Contents
N9410-90001 Keysight 5500 SPM User’s Guide 1
Table of Contents
I Read This First
Specifications I-v
Voltage and Laser Safety Information I-vi
Power Supply I-vii
Piezo Scanner Precautions I-vii
General Care Requirements I-viii
Disclaimers I-viii
Declaration of Conformity I-ix
Contact Information I-x
II Table of Contents
1 Introduction to the Keysight 5500
Overview of Keysight SPM System 1-2
SPM Basics 1-3
SPM Techniques 1-5
Scanning Tunneling Microscopy (STM) 1-5
Atomic Force Microscopy (AFM) 1-6
Contact Mode AFM 1-8
Intermittent Contact AFM 1-9
Current Sensing Mode (CSAFM) 1-12
Force Modulation Microscopy (FMM) 1-13
Lateral Force Microscopy (LFM) 1-14
Dynamic Lateral Force Microscopy (DLFM) 1-14
Magnetic Force Microscopy (MFM) 1-15
Electrostatic Force Microscopy (EFM) 1-15
Kelvin Force Microscopy (KFM) 1-15

Contents
N9410-90001 Keysight 5500 SPM User’s Guide 2
2 Keysight 5500 SPM Components
Microscope 2-3
Probes 2-4
Nose Assembly 2-5
One-Piece Nose Assemblies 2-5
Two-Piece Nose Assemblies 2-6
Scanner 2-7
Detector 2-9
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 2-21
Software 2-22
System Options 2-23
MAC Mode 2-23
MAC III Mode 2-23
Liquid Cell 2-23
Temperature Control 2-24
Thermal K 2-24
Environmental Chamber 2-24
Glove Box 2-25
Electrochemistry 2-26
PicoTREC 2-26
PicoLITH 2-26
3 Setting Up the Keysight 5500 SPM
Component and Facility Dimensions 3-1
Facility Requirements 3-4
Utilities 3-5
Noise and Facility Specifications 3-5
Assembling the Vibration Isolation Chamber 3-7
Switching Door Orientation 3-9

Contents
N9410-90001 Keysight 5500 SPM User’s Guide 3
Managing Cables 3-10
Connecting the Components 3-12
Guidelines for Moving the System 3-13
Care and Handling of the Probes and Scanner 3-14
Probes 3-14
Nose Assembly 3-14
Scanner 3-14
4 Preparing for Imaging
Setting Up the Scanner Assembly 4-1
One-Piece Nose Assembly 4-2
Two-Piece Nose Assembly 4-9
Inserting the Scanner and Connecting Cables 4-12
Aligning the Laser 4-14
Inserting and Aligning the Detector 4-22
Mounting the Sample 4-26
Using the Video System 4-29
5 Contact Mode Imaging
Setting Up for Contact Mode Imaging 5-2
Constant Force Mode 5-2
Constant Height Mode 5-9
Fine-Tuning the Image 5-9
6 AC Modes
Acoustic AC Mode (AAC) 6-3
AAC Mode 6-3
Constant Height Mode 6-8
Magnetic AC (MAC) Mode 6-9
Standard MAC Mode 6-10
Top MAC Mode 6-12
Q Control 6-13

Contents
N9410-90001 Keysight 5500 SPM User’s Guide 4
7 Additional Imaging Modes
Scanning Tunneling Microscopy (STM) 7-1
STM Gain and Preamp Settings 7-3
STM Imaging Procedure 7-6
Current Sensing AFM (CSAFM) 7-9
Lateral Force Microscopy (LFM) 7-13
Dynamic Lateral Force Microscopy (DLFM) 7-14
Force Modulation Microscopy (FMM) 7-16
Magnetic Force Microscopy 7-19
Electrostatic Force Microscopy (EFM) 7-25
Kelvin Force Microscopy (KFM) 7-29
Force Spectroscopy 7-31
Force Spectroscopy Procedure for Contact Mode 7-32
FlexGrid Spectroscopy 7-36
FlexGrid Spectroscopy Procedure for Contact Mode 7-36
Volume Spectroscopy 7-41
Volume Spectroscopy Procedure for Contact Mode 7-41
8 Scanner Maintenance and Calibration
Care and Handling of the Probes and Scanner 8-3
Probes 8-3
Nose Assembly 8-3
Scanner 8-4
Scanner Characteristics 8-4
Non-Linearity 8-5
Sensitivity 8-5
Hysteresis 8-5
Other Characteristics 8-6
Calibrating the Multi-Purpose Scanner 8-8
X Calibration 8-9
Y Calibration 8-14
Non-Orthogonality 8-17
Z Calibration 8-18
Servo Gain Multiplier 8-19

Contents
N9410-90001 Keysight 5500 SPM User’s Guide 5
Archive the Calibration Files 8-19
9 Closed-Loop Scanners
Scanner Types 9-1
Z-Axis Closed-Loop Scanner 9-1
X/Y/Z Closed-Loop Scanner 9-2
Calibration 9-2
X and Y Sensor Calibration 9-3
Z Sensor Calibration 9-11
10 MAC Mode
List of MAC Mode Components 10-1
Connections 10-2
Hardware and Sample Setup 10-4
11 MAC III
Initial Setup 11-2
List of MAC III Components 11-2
Hardware and Sample Setup 11-6
Auxiliary Signal Access Box 11-6
MAC III Software Controls 11-11
Simplified Software Control Options 11-12
Advanced Software Control Options 11-24
Amplitude and Frequency Modulation Techniques 11-33
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

Contents
N9410-90001 Keysight 5500 SPM User’s Guide 6
13 Temperature Control
Cantilevers for Temperature Controlled Imaging 13-1
High Temperature Sample Plates 13-2
Connections 13-5
Imaging 13-11
Peltier (Cold MAC) Sample Plate 13-13
Connections 13-15
Water Cooling 13-20
Imaging 13-21
Tips for Temperature Controlled Imaging 13-22
14 Thermal K
Thermal K Calibration 14-3
Thermal K Setup 14-3
Spring Constant Calibration 14-4
15 Environmental Control
Environmental Chamber 15-1
Glove Box 15-3
16 Electrochemistry
Equipment 16-3
Liquid Cell 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

Contents
N9410-90001 Keysight 5500 SPM User’s Guide 7
Guidelines for Electochemistry 16-10
SECM - Scanning Electrochemical Microscopy 16-12
SECM System Setup 16-12
Assembling the SECM Nose Cone 16-14
SECM Software Interface 16-17
A Wiring Diagrams
Keysight 5500 SPM Standard Wiring Diagram A-2
Keysight 5500 SPM with MAC Mode Controller A-3
Keysight 5500 SPM with MAC Mode, Force Modulation
Imaging A-4
Keysight 5500 SPM with MAC III Option A-5
Keysight 5500 SPM with MAC III Option and Closed Loop
Scanner A-6
Index

Keysight 5500 SPM
User’s Guide
1
Introduction to the Keysight 5500
Overview of Keysight SPM System 1-2
SPM Basics 1-3
SPM Techniques 1-5
Scanning Tunneling Microscopy (STM) 1-5
Atomic Force Microscopy (AFM) 1-6
Intermittent Contact AFM 1-9
Acoustic AC (AAC) AFM 1-10
Magnetic AC (MAC) Mode 1-11
Top MAC Mode 1-12
Current Sensing Mode (CSAFM) 1-12
Force Modulation Microscopy (FMM) 1-13
Lateral Force Microscopy (LFM) 1-14
Dynamic Lateral Force Microscopy (DLFM) 1-14
Magnetic Force Microscopy (MFM) 1-15
Electrostatic Force Microscopy (EFM) 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.
The Keysight 5500 SPM offers features and software for research in
materials science, polymers, nanolithography and general surface
characterization. With excellent ease of use, the 5500 SPM also affords
educators an unprecedented opportunity to introduce students to AFM
technology.

Introduction to the Keysight 5500 5
Keysight 5500 SPM User’s Guide 5-2
Overview of Keysight SPM System
The main component of the Keysight 5500 SPM system is the
microscope (Figure 1-1), which includes the X/Y motion controls,
scanner, high-resolution probe/tip, and detector. The control system for
the microscope includes, at minimum, a high-speed computer, AFM
controller and Head Electronics Box. Optional components include
additional electronics, specialized scanners and probes for particular
SPM techniques, and an environmental enclosure to control acoustic
and vibration noise.
Figure 1-1 The Keysight 5500 SPM microscope, shown with optional
environmental chamber
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.

Introduction to the Keysight 5500 5
Keysight 5500 SPM User’s Guide 5-3
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
curvature typically in the nanometers or tens of nanometers) that is in
near-contact, intermittent contact, or perpetual contact with the sample
surface.
An SPM is used to investigate sample properties at or near the sample
surface; that is, immediately beneath the surface (typically several
nanometers deep) and immediately above the surface (typically several
tens of nanometers high).
In SPM techniques, the sharp probe (tip) is scanned across a sample
surface, or the surface is scanned beneath the tip (Figure 1-2).
Interactions between the tip and sample are detected and mapped.
Different techniques sense different interactions, which can be used to
describe surface topography, adhesion, elasticity, electrostatic charge,
etc.
Figure 1-2 Scanning Probe Microscopy diagram
The small size of the probe tip is key to the SPM’s high resolution.
However, its small size also means that the tip must be scanned in order
to image a significant area of the sample. SPM techniques use “raster
scanning,” in which high resolution actuators, usually made of
piezoelectric materials, move the probe across the sample and back over
each line of the image area. For each X/Y coordinate pair, the
interaction of the tip and sample is recorded as one data point. The