9500 Scanning Microwave Microscopy Mode Users Manual

Keysight Scanning Microwave
Microscopy Mode
User’s Guide
Read This First
Keysight SMM Mode User’s Guide i

Notices
© Keysight Technologies 2013, 2014 Manual Part Number “Commercial computer software” as defined
in DFAR 252.227-7014 (June 1995), or as a
No part of this manual may be reproduced in N9546-90002 “commercial item” as defined in FAR
any form or by any means (including elec-
2.101(a) or as “Restricted computer soft-
tronic storage and retrieval or translation
into a foreign language) without prior agree- Edition ware” as defined in FAR 52.227-19 (June
1987) or any equivalent agency regulation or
ment and written consent from Keysight Edition C, May 2017 contract clause. Use, duplication or disclo-
Technologies as governed by United States
sure of Software is subject to Keysight Tech-
and international copyright laws. Printed in USA
nologies’ standard commercial license
Keysight Technologies terms, and non-DOD Departments and
1400 Fountaingrove Parkway Agencies of the U.S. Government will receive
Santa Rosa, CA 95403 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
Warranty than Limited Rights as defined in FAR
The material contained in this docu- 52.227-14 (June 1987) or DFAR
252.227-7015 (b)(2) (November 1995), as
ment is provided “as is,” and is subject
applicable in any technical data.
to being changed, without notice, in
future editions. Further, to the maxi-
mum extent permitted by applicable Safety Notices
law, Keysight disclaims all warranties,
either express or implied, with regard CAUTION
to this manual and any information A CAUTION notice denotes a
contained herein, including but not lim-
hazard. It calls attention to an
ited to the implied warranties of mer-
chantability and fitness for a particular
operating procedure, practice,
purpose. Keysight shall not be liable for or the like that, if not correctly
errors or for incidental or consequential performed or adhered to, could
damages in connection with the fur- result in damage to the product
nishing, use, or performance of this or loss of important data. Do
document or of any information con- not proceed beyond a
tained herein. Should Keysight and the CAUTION notice until the
user have a separate written agree- indicated conditions are fully
ment with warranty terms covering the understood and met.
material in this document that conflict
with these terms, the warranty terms in
the separate agreement shall control. WARNING
A WARNING notice denotes a
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hazard. It calls attention to an
The hardware and/or software operating procedure, practice,
described in this document are fur- or the like that, if not correctly
nished under a license and may be performed or adhered to, could
used or copied only in accordance with result in personal injury or
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a WARNING notice until the
Restricted Rights Legend indicated conditions are fully
If software is for use in the performance of a understood and met.
U.S. Government prime contract or subcon-
tract, Software is delivered and licensed as
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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 Chapter 3 for Facility Requirements in the
instrument’s User’s Guide 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.
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
Keysight SMM Mode User’s Guide iii

Read This First
Power Requirements
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 5420, 5500 and 5600LS

NOTE
systems, and do not guarantee the function of an experiment
(including the cantilever) in these conditions.
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
Stop using the scanner if the scanner cable insulation is damaged

WA R N IN G
in order to avoid electrical shock. Have it repaired or replaced by
the factory.
Keysight SMM Mode User’s Guide iv

Read This First
Voltage and Laser Safety Information

The SPM instrumentation 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 diode laser with

an output of up to 1 mW of visible radiation at 670 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
Use of controls or adjustments or performance of procedures
WA R N IN G
other than those specified herein may result in hazardous light
exposure. Furthermore, the use of optical instruments with this
product may increase eye hazard.
Keysight SMM Mode User’s Guide v

Read This First
In accordance with federal FDA requirements, the following laser

precaution 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

1 Unplug the power cord from the Keysight AFM Controller.
2 Remove the fuse holder located on the back of the controller.
3 Underneath 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.
4 Reinsert the voltage switch with the desired voltage.
5 Replace 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
Keysight SMM Mode User’s Guide vi

Read This First
calibration can be verified using a calibration standard, and

adjustments can be made using the calibration procedures
described in the “Scanner Maintenance and Calibration” chapter
of the instrument’s User’s Guide Manual.
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.
The Declaration of Conformity (DoC) included in this document

NOTE
(page viii) may not contain the most recent information.
For the most up to date DoC, please refer to
http://regulations.products.keysight.com/DoC/search.htm.
Keysight SMM Mode User’s Guide vii

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Declaration of Conformity
Keysight SMM Mode User’s Guide viii

Read This First
Contact Information
Keysight Technologies
4330 W. Chandler Blvd., Chandler, Arizona 85226-4965 U.S.A.
Tel: +1.480-756-5900 Fax: +1.480-756-5950
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:
http://nano.tm.keysight.com/index.cgi?CONTENT_ID=253
Keysight SMM Mode User’s Guide ix

I Read This First
Specifications ................................................................................................... iii
Voltage and Laser Safety Information ............................................................. v
Power Supply ................................................................................................... vi
Piezo Scanner Precautions .............................................................................. vi
General Care Requirements ............................................................................. vii
Disclaimers ....................................................................................................... vii
Declaration of Conformity ................................................................................ viii
Contact Information ......................................................................................... ix
1 Introduction to Scanning Microwave Microscopy Mode

Overview of Keysight Scanning Microwave Microscopy (SMM) Mode ........... 2
Scanning Impedance Microscopy .............................................................. 3
Scanning Capacitance Microscopy ............................................................ 4
Vector Network Analyzer............................................................................ 5
Mechanical Design ..................................................................................... 5
Scanning Microwave Microscopy Mode .................................................... 6
Spectroscopy with Scanning Microwave Microscopy Mode ..................... 7
2 Keysight SMM Mode Components and Setup

Probes............................................................................................................... 9
Nose Cone Assembly........................................................................................ 10
Vector Network Analyzer ................................................................................. 11
SMM Hardware and Software Installation Guidelines .................................... 12
Parts List for Installation............................................................................. 12
Cabling Configuration................................................................................. 13
SMM Mode Setup ....................................................................................... 14
3 Sample Preparation for Dopant Profiling

Equipment, Chemicals and Supplies ............................................................... 18
Polishing ........................................................................................................... 18
Polishing Procedure.................................................................................... 19
Oxidation........................................................................................................... 21
Final Finish........................................................................................................ 21
4 Imaging in SMM Mode

Setting Up the Scanner Assembly ................................................................... 23
Inserting the Universal Nose Cone............................................................. 24
Removing the Universal Nose Cone ........................................................... 26
Inserting a Probe in the Universal Nose Cone ........................................... 28
Inserting the Scanner and Connecting Cables .......................................... 29
Setup for Optional dC/dV Controller Module (DPMM) .............................. 34
Software Setup for SMM Mode ....................................................................... 36
Determine Frequency for Microwave Signal .............................................. 36
Settings for Optional dC/dV Controller Module......................................... 39
Troubleshooting ............................................................................................... 42
5 Calibrated Imaging with SMM Mode

Capacitance Calibration ................................................................................... 44
Capacitance Calibration Standard ............................................................. 44
SMM Imaging of the Calibration Standard ................................................ 45
Calculating the Capacitance Signal ........................................................... 50
Calibrating the Capacitance Measurement ............................................... 53
Cleaning the Capacitance Standards......................................................... 55
Dopant Profile Calibration................................................................................ 56
Dopant Profile Calibration Standards ........................................................ 56
SMM dC/dV Imaging of the Calibration Standard ..................................... 57
Calibrating the Dopant Measurement........................................................ 70
Applying the Calibration to Unknown Samples ......................................... 73
Cleaning the Dopant Profiling Standards................................................... 73
A Capacitance Standard Specifications

Specifications ................................................................................................... 77
I Index
Keysight Scanning Microwave Microscopy Mode
User’s Guide
1
Introduction to Scanning Microwave
Microscopy Mode
Overview of Keysight Scanning Microwave Microscopy (SMM)
Mode 2
Scanning Impedance Microscopy 3
Scanning Capacitance Microscopy 4
Vector Network Analyzer 5
Mechanical Design 5
Scanning Microwave Microscopy Mode 6
Spectroscopy with Scanning Microwave Microscopy
Mode 7
Scanning Microwave Microscopy (SMM) Mode is a specialized

technique that combines the electromagnetic measurement
capabilities of a microwave Power Network Analyzer (PNA) with
the nanometer-resolution and Angstrom-scale positioning
capabilities of an Atomic Force Microscope (AFM). The Keysight
SMM Mode is compatible with the Keysight 9500, 7500, 5420,
5500 and 5600LS Scanning Probe Microscope (SPM) systems.
This User’s Guide deals specifically with the 9500 SPM.
In this User’s Guide, it is assumed that the reader is already
proficient in Contact Mode Scanning Probe Microscopy
techniques. The chapters that follow will show you how to
assemble the microscope, prepare for and image using the new
SMM Mode.
Keysight Technologies offers high-precision, modular SPM
solutions for research, industry, and education. Exceptional
worldwide support is provided by experienced application
scientists and technical service personnel. Keysight's
leading-edge R&D laboratories ensure the continued, timely
introduction and optimization of innovative, easy-to-use SPM
technologies.
Introduction to Scanning Microwave Microscopy Mode 1
Overview of Keysight Scanning Microwave Microscopy (SMM) Mode

Mapping materials physical properties, such as impedance,
capacitance, dielectric constants, and dopant density, at the
nanoscale is of great interest to both materials and
semiconductor industries. Such mapping, however, usually is not
as straightforward as topography imaging because, in many
cases, these properties are related to buried structures not shown
directly on the surface. It takes innovative approaches to measure
subsurface properties nondestructively with sufficient sensitivity
and resolution.
With the invention of scanning tunneling microscopy (STM) and
atomic force microscopy (AFM), a number of STM and AFM based
techniques have been developed to probe materials properties.
While each method has different advantages, SMM and scanning
capacitance microscopy (SCM) have shown the most potential in
this field for both industrial applications and scientific research.
A new technique, scanning microwave microscopy or SMM Mode,
is introduced here. It integrates network analysis for microwave
frequency communications with high resolution AFM imaging. It is
capable of mapping not only impedance, capacitance, dielectric
constants of a variety of different materials, like what SMM does,
but also dopant density of semiconductors like SCM. With a
specially designed matched resonant circuit, its sensitivity and
signal to noise ratio is significantly enhanced.
Measuring electromagnetic properties of materials can provide
insight into applications in many areas of science and technology,
and increasingly, these properties need to be evaluated at the
nanometer scale. Since electromagnetic properties, such as the
dielectric constant, are ultimately related to a material’s
molecular structure, correlating the detailed physical structure of
a material with its electromagnetic properties is frequently more
valuable than the knowledge of either alone.
The scanning microwave microscope consists of an AFM
interfaced with a VNA, as shown in Figure 1. A microwave signal is
sent directly from the network analyzer and transmitted through a
resonant circuit to a conductive AFM probe that is in contact with
a sample being scanned. The probe also serves as a receiver to
capture the reflected microwave signal from the contact point. By
directly measuring the complex reflection coefficient from the
network analyzer, the impedance of the sample at each scanned
point can then be mapped simultaneously with the surface
topography. A half wavelength impedance transformer placed
directly across a 50 W load forms a matched resonance circuit.
Combined with enhanced peak detection, this circuit significantly
Keysight SMM Mode User’s Guide 2

increases the dynamic range and sensitivity of the impedance

measurement. With a superimposed low-frequency modulation,
changes of the capacitance as a result of depletion of carriers in a
semiconductor sample, or dC/dV, can also be obtained at the
same time with an AC mode controller containing digital lock-in
amplifiers.
Figure 1 Overview of SMM Mode with Keysight’s VNA (left), and

9500 AFM (right)
Scanning Impedance Microscopy

One of the most common applications of network analysis is
measuring the impedance of a component, so as to evaluate if it
matches the impedance of the other components with which it
must interface in a network. Impedance measurement techniques
in network analyzers have become quite advanced and refined.
The SMM Mode uses the VNA in reflection mode for measuring
the impedance of the “network” that includes the tip-sample
interface. In the SMM Mode, the device under test (DUT) for the
VNA consists of the AFM probe and the region of the sample
immediately beneath the metal-coated AFM tip. One application
of impedance measurement with SMM Mode is scanning
capacitance microscopy (SCM) of semiconductors. In this
situation, the AFM tip and the semiconductor sample form a
metaloxide-semiconductor (MOS) capacitor.

The incident microwave signal travels through a series of

components before it reaches the tip-sample interface by means
of a transmission line. The impedance mismatch between the
transmission line and the DUT causes the incident microwave
signal to partially reflect from the tip-sample interface back
towards the stimulus signal source inside the VNA; this reflected
signal is proportional to the impedance mismatch. The incident
microwave signal and the reflected microwave signal together
contain information about the impedance of the DUT.
Scanning Capacitance Microscopy

Measuring the capacitance-to-ground (C) of the tip-sample
interface, and its derivative (dC/dV) with an applied AC bias is an
important extension of AFM for the electrical characterization of
semiconductors. It enables a two dimensional mapping of the
carrier density across different regions of a semiconductor, with
applications in the failure analysis, characterization, modeling and
simulation of device performance, and also in the development of
the semiconductor fabrication process. Traditionally, a resonant
capacitive sensor-based scanning capacitance microscopy (SCM)
technique has been used to implement this type of AFM technique
with some success. One of the main shortcomings of traditional
SCM is the difficulty of making absolute measurements of the
strength of the tip-sample electrical interaction; therefore, SCM
images remain maps of the relative difference in carrier densities
across the scanned area. For this reason, accomplishing the
much-coveted task of using SCM to reliably and repeatably
extract numerical estimates for carrier densities in semiconductor
devices remains elusive.
Keysight VNA hardware includes precision components for the
calibration and performance verification of the instrument,
thereby extending its applications to those that require calibrated,
traceable, and absolute measurements of, for example,
capacitance. Keysight’s VNA measurements are calibrated with
Keysight’s “ECal,” the electronic calibration kits for fast, simple,
accurate calibration of the instrument, including phase
measurements. The instrument’s firmware makes the calibration a
routine push-button task that completes within seconds.

Vector Network Analyzer

Keysight vector network analyzers (VNA) are mature, highly
sophisticated characterization instruments that make extremely
accurate, calibrated measurements of complex-valued ratios on
electromagnetic signals. The ratios are:
reflected signal transmitted signal

R =  ------------------------------------ and T =  -------------------------------------------
 incident signal   incident signal 
The incident signal is generated and controlled inside the VNA. As

a result, the ratios R and T are not merely relative, but referenced
to the well-known, accurately quantified incident signal.
SMM Mode uses Keysight’s VNA microwave vector network
analyzer. The main difference between a scalar network analyzer
and a VNA is the ability of the VNA to make phase measurements.
Like all network analyzers, this VNA is a stimulus-response
instrument, optimized for accurate and repeatable measurement
of the response of a network or a DUT to a known stimulus signal.
This is in contradistinction to instruments such as the spectrum
analyzer, which are usually configured as a receiver (only) of an
unknown signal, and which do not include a source for a stimulus
to be applied to the DUT.
A VNA has two operational modes: transmission and reflection. In
the reflection (alternatively, transmission) mode, the VNA
measures the magnitude and phase characteristics of the DUT by
comparing the signal that reflects off (alternatively, transmits
through) the device with the stimulus signal. In some older model
network analyzers, the stimulus signal was taken from a separate
source. In Keysight’s VNA, the knowledge of the stimulus signal is
excellent, because the microwave signal is generated inside the
VNA with high resolution and stability of both the amplitude and
the frequency.
Each mode enables measurement of several useful parameters. In
the reflection mode, the VNA can measure, among other things,
the impedance of the DUT. Impedance is the total resistance that
a DUT presents to the flow of an AC signal at a given frequency.
Scanning Impedance Microscopy is a major application of the
SMM.
Mechanical Design
To take full advantage of the VNA-based measurement scheme,
Keysight’s SMM Mode incorporates several innovations into the
AFM hardware. These include a sophisticated microwave shielding

to improve the instrument’s electromagnetic compatibility with its

surroundings, and minimize the effect of stray capacitances,
which are inevitable with the movement of the probe during the
raster scanning. The innovation of this design is implemented in
such a way as to minimize the impact on the performance of the
AFM scanner, where the cantilever holder attaches to the rest of
the AFM.
Figure 2 9500 SMM Mode nose assembly and associated

cabling
Scanning Microwave Microscopy Mode

Keysight’s SMM Mode makes high-resolution, calibrated
measurements of the capacitance-to-ground between an AFM tip
and a semiconductor sample. This ushers the way for the reliable,
repeatable extraction of numerical values of the carrier densities
in a semiconductor. The SMM Mode typically operates at
microwave frequencies of 1.5-6 GHz, which is substantially higher
than the frequencies used in traditional SCM of around 900 MHz.
The higher frequencies in SMM Mode lead to better sensitivity and
electrical resolution for measuring the tip-sample capacitance.
The SMM Mode uses a lock-in amplifier for measuring the
in-quadrature and in-phase components of dC/dV, allowing for
the determination of the polarity of the majority carriers in the
semiconductor.

Spectroscopy with Scanning Microwave Microscopy Mode

Spectroscopy with SMM Mode brings the vast measurement
capabilities of the VNA to expand AFM-based spectroscopy
techniques for electromagnetic characterization beyond anything
that has been available in a commercial product so far. For
example, power sweep and frequency sweep capabilities of the
VNA are perfectly suited for characterizing the frequency
response of a given location on a sample. Even the VNA’s most
common methods for representing measurements, such as the
Smith Chart, and the Linear Phase plot, open up a wide range of
possibilities for spectroscopic techniques with AFM. In addition,
the VNA supports and operates, directly on the instrument,
numerous material characterization software packages from
Keysight; these allow, for example, the measurement of the
complex permittivity of a material.
Spectroscopic techniques in AFM are conducted by disabling the
AFM’s raster scanning, and investigating the sample at the
location of the AFM tip while sweeping a parameter across a
range of its values; for example, the amplitude or the frequency of
a signal applied to the tip or to the sample. For more information,
please visit:
http://literature.cdn.keysight.com/litweb/pdf/5989-8215EN.pdf

User’s Guide
2
Keysight SMM Mode Components
and Setup
Probes 9
Nose Cone Assembly 10
Vector Network Analyzer 11
SMM Hardware and Software Installation Guidelines 12
Parts List for Installation 12
Cabling Configuration 13
SMM Mode Setup 14
PnaSvr Application Installation 14
NanoNavigator Software Configuration 15
Advanced PNA Settings 15
Software Troubleshooting 16
Scanning Microwave Microscopy Mode is a specialized technique

that combines the electromagnetic measurement capabilities of a
microwave vector network analyzer (VNA) with the
nanometer-resolution and Angstrom-scale positioning capabilities
of an Atomic Force Microscope.
The Keysight SMM Mode is compatible with the Keysight 9500,
7500. 5420, 5500 and 5600LS Scanning Probe Microscope
systems. In addition to a microscope, SMM Mode requires a
Keysight scanner with an SMM Mode nose assembly and probes.
A Keysight VNA and associated cabling is also required. Additional
computer and software requirements are discussed in more detail
in this chapter.
The SMM technique is capable of mapping the capacitance and
impedance properties of a sample. It is also possible to measure
the dopant profile of a semiconductor material. This option
requires the Keysight dC/dV Controller Module, referred to as the
DPMM Module, dC/dV power supply and associated cabling. The
setup for dC/dV measurements is described in Chapter 4,
"Imaging in SMM Mode".
Keysight SMM Mode Components and Setup 2
In this User’s Guide, it is assumed that the reader is already

proficient in Contact Mode AFM techniques. This chapter will
explain the differences in the nose cone and cantilevers (probes)
used for SMM Mode compared to standard Contact Mode
imaging. It will also cover the hardware and software setup.
Figure 3 Components of Scanning Microwave Microscopy Mode

showing Keysight’s Vector Network Analyzer (left) and
Keysight 9500 SPM (right)
The procedures in this manual are for NanoNavigator1.8 and

NOTE
higher.
Probes
The SPM measurements for imaging are accomplished using a tip
at the free end of a cantilever (a “probe”). Typically, AFM
cantilevers are fabricated from silicon or silicon nitride with an
integrated sharp tip at the end. The selection of probe and tip
geometry, cantilever spring constant, and cantilever resonance
frequencies will vary depending on application, type of sample
surface, imaging environment, and type of image being
generated. Tip geometry may be tetrahedral, pyramidal or conical.
Tip sharpness, defined by radius of curvature and sidewall angles,
greatly affects the resolution available with the probe.

Conductive cantilevers are required for SMM Mode. One type of

cantilever uses platinum-iridium (Pt-Ir) wire for the tip and has a
gold contact pad on the back to carry the microwave signal. This
wire tip design will provide a longer tip service life than a standard
cantilever.
Nose Cone Assembly

The nose assembly retains the cantilever and enables its motion
(Figure 4). A spring clip on the nose cone assembly secures the
probe in place. The nose cone assembly is held securely in the
scanner by an O-ring.
The SMM nose cone assembly is designed to simplify the process
of inserting a cantilever. It also helps prevent damage to the
scanner during installation of the nose cone assembly. Currently,
the SMM nose cone assembly is only available for Contact Mode
imaging.
The SMM nose cone cannot be heated above 180 degrees Celsius.
C A U T IO N
To take full advantage of the VNA-based measurement scheme,

Keysight's SMM incorporates several innovations into the AFM
hardware. These include a sophisticated microwave shielding to
improve the instrument's electromagnetic compatibility with its
surroundings, and to minimize the effect of stray capacitances
which are inevitable with the movement of the probe during the
raster scanning. The innovation of this design is implemented in
such a way as to minimize the impact on the performance of the
AFM scanner, where the cantilever holder attaches to the rest of
the AFM.

Figure 4 SMM Mode Nose Assembly detail
Vector Network Analyzer

The SMM Mode technique requires a vector network analyzer
(VNA) to measure the electronic properties. SMM Mode uses
Keysight’s microwave performance network analyzer (PNA)
instrument. Like all network analyzers, this VNA is a
stimulus-response instrument, optimized for accurate and
repeatable measurement of the response of a network or a device
under test (DUT) to a known stimulus signal. This is in
contradistinction to instruments such as the spectrum analyzer,
which are usually configured as only a receiver of an unknown
signal, and which do not include a source for a stimulus to be
applied to the DUT.
A VNA has two operational modes: transmission and reflection. In
the reflection mode, the VNA measures the magnitude and phase
characteristics of the DUT by comparing the signal that reflects
off the device with the stimulus signal. In the transmission mode,
the VNA measures the characteristics of the DUT by comparing
the signal that transmits through the device with the stimulus
signal.
In Keysight’s VNA instrumentation, the knowledge of the stimulus
signal is excellent, because it is a microwave signal generated
inside the VNA with high resolution and stability of both the
amplitude and the frequency. Each mode enables measurement of
several useful parameters such as impedance and capacitance.

Figure 5 Keysight PNA
SMM Hardware and Software Installation Guidelines

This section discusses the hardware, cabling and software
necessary for SMM Mode.
Parts List for Installation

The following parts are needed to begin installation:
Hardware:
• Keysight 9500 SPM system.
• Metrology scanner with SMM Mode nose assembly and
specialized tip.
Vector Network Analyzer:
• Keysight PNA and associated cabling.
• Keyboard and mouse attached.
Host PC:
• Dedicated computer system as supplied with SPM system.
Network:

• Host PC and VNA need to be connected to the same

network.
Software:
• NanoNavigator software (rev 1.8 or later).
These notes assume the VNA is running Windows XP SP2 and the
NOTE
User has Administrator privileges. Other operating systems could
require different procedures.
Cabling Configuration
The diagram in Figure 6 shows the cabling configuration needed
for SMM Mode installation. This cabling is in addition to standard
SPM system configuration.
- The router connection uses standard Cat5 or better Ethernet
cables connected to a common router. The router may be
uplinked to company network for wider access. The router is
connected to the computer and PNA Ethernet ports. Any of the
ports 1 through 4 may be used.
- The microwave connection uses the cable with SMA
connectors (Keysight PN N9546-60201 or Rosenberger PN
70B-32S1-32S1-01829).
Figure 6 SMM Mode Cabling Configuration

SMM Mode Setup

There are two steps for the SMM Mode setup:
1 Install the PnaSvr application on the VNA.
2 Configure the NanoNavigator software.
PnaSvr Application Installation

1 Log in to the VNA as an Administrator. Keysight VNA
instruments are shipped from the factory with the default user
name PNA-Admin and the password keysight.
2 If connected to the network, run the AgileUpdate now to check
for updated firmware revisions.
a This prompt could come up automatically, or
b This update can be found in the Network Analyzer
application menu under System > Service > AgileUpdate.
c When firmware update finishes, choose Easy Connection
option.
3 If the Network Analyzer application is not running, start it, then
locate the Application Code (firmware) Version number found
under Help > About and note it for future use: _______________
4 Close the Network Analyzer application.
The PNASvr is preinstalled if the VNA is shipped directly from the
factory. If not, copy the PNASVR Setup installation file from the
PicoView folder and copy it to a USB flash drive.
5 Insert the USB flash drive containing the PnaSvr installer in
one of the USB ports on the PNA.
6 The PnaSvr installer may start automatically. If not, launch
setup.exe on the flash drive.
7 Follow the instructions provided by the installer which might
also be installing the .NET framework on the PNA.
8 After the installation PnaSvr will be running and ready for a
connection from PicoView.
9 Click on the PnaSvr icon in the System Tray and note the
numbers shown for IP address and Port: ______ . ______ .
______ . ______ : __________
The PnaSvr application on the VNA must be run by PNA-Admin or

NOTE
a user with administrative rights.

NanoNavigator Software Configuration

1 Start NanoNavigator.
2 In the main menu toolbar, go to the Components tab of the
Setup window (Controls > Setup, or use the Setup button in
the main toolbar) and type the IP Address and port number
recorded above from step 9 in the PNA Address text field.
3 In the System Components dialog box, select the Keysight PNA
check box.
a If the connection to the PNA is successful, the PNA display
will change from one to two windows for amplitude and
phase.
b If an error is detected, see the "Software Troubleshooting"
section below.
4 To avoid future connection errors when starting
NanoNavigator, either start the PNA first or clear the Keysight
PNA check box before exiting NanoNavigator.
5 Choose Controls > PNA to open the PNA Sweep window.
Advanced PNA Settings

There are additional settings for the PNA. These are optional and
should be set for advanced applications when needed.
1 Choose Controls > Setup > Preferences.
2 Select the PNA tab.
3 In the Parameter drop-down menu:
a Select S11 (default) for reflection mode.
b Select S12 for transmission mode.
4 In the Trigger drop-down menu:
a Select BNC (default setting).
b AUX is used for some older PNA modes.
c Consult the PNA manual if necessary
5 If the Load PNA Calibration File When Connecting check box is
selected, a PNA calibration file saved on the local drive of the
PNA by the user will be loaded for PNA Signal connection. The
file name needs to be entered into the PNA calibration file text
field. By default, this feature is not selected and it will not
affect the regular SMM operation

Software Troubleshooting
If NanoNavigator cannot establish communication with the PNA,
the following steps may prove useful.
1 Make sure the PNA is turned on and it is on the network.
2 Verify the IP address and port number recorded in step 9 of
"PnaSvr Application Installation" and entered in step 2 of
"NanoNavigator Software Configuration".
3 Make sure the PnaSvr application on the VNA is run by a user
with administrative rights.
4 The following reference may also be of use:
http://na.tm.keysight.com/pna/help/PNAWebHelp/Programm
ing/Learning_about_COM/Configure_for_COM-DCOM_Progra
mming.htm
If additional assistance is needed, please contact
afm-support@keysight.com.

User’s Guide
3
Sample Preparation for Dopant
Profiling
Equipment, Chemicals and Supplies 18
Polishing 18
Polishing Procedure 19
Polishing 18
Oxidation 21
Final Finish 21
Silicon surfaces need to be clean, smooth and thinly oxidized to

produce the best dopant profiling results using Scanning
Capacitance Microscopy (SCM) or Scanning Microwave
Microscopy (SMM). The goal is to produce a near-atomically
smooth surface with a thin, robust oxide layer that distinguishes
the scanned probe tip from the semiconductor material. This
chapter describes one method used to prepare such samples at
Keysight Technologies. Other procedures are possible. There are
more detailed papers on sample preparation for dopant profiling in
the literature.*
For cross-sectional samples with dopant profiles near one surface,
it is recommended that the sample be bonded to another piece of
silicon with an epoxy which is stable up to 300 °C. The sample
surface closest to the dopant profiles of interest should be bonded
to the other surface. Although bonding to the other piece of
silicon is not required, it results in a sample with minimal rounding
due to the polishing. It also provides a substrate to prevent the
SPM tip from falling off the sample near a region of interest.
* 1.Pawlik, M., "Spreading Resistance: A Quantitative Tool for Process Control and
Development," J. Vac. Sci. Technol. B 10 388-396 (1992).
2.Zavyalov, V.V., McMurray, J.S., and Williams C.C., "Advances in Experimental
Technique for Quantitative Two Dimensional Dopant Profiling by Scanning
Capacitance Microscopy," Rev. Sci. Inst., 70 (1), 158 (1999).
3.Stangoni, M. V., "Scanning Probe Techniques for Dopant Profile
Characterization," Ph.D. Thesis, ETH, Zürich, iss. number 16024 (2005).
Sample Preparation for Dopant Profiling 3
Equipment, Chemicals and Supplies

The following items will be needed to prepare the cross-sectional
samples:
1 Polishing plate capable of spinning 10 to 50 rpm with
deionized (DI) water flow
2 Non-adhesive diamond lapping films with 30, 15, 6, 1, 0.3, and
0.1 μm diamond particle sizes
3 Non-adhesive alumina lapping film with 0.05 μm particles
4 Rubber squeegee
5 FibrMet polishing cloth
6 Colloidal silica 0.02 μm
7 Deionized water
8 Binocular microscope to view polished surface in between the
polishing steps
9 Rinse solution consisting of H2O:H2O2:NH3OH (ratio 10:1:1),
with enough added KOH pellets to raise the pH to 11.
10 Q-tips or texwipes
11 UV-Ozone chamber with hot-chuck capable of 300 °C
temperature
12 CO2 snow-jet cleaning nozzle*
Ensure all chemicals are properly handled and stored.

WA R N IN G
Polishing
Polishing is only necessary for dopant profiling on cross-sections
or beveled samples. If top surface imaging is needed, the sample
may already be smooth enough for measurements. However, if
the top surface has a thick oxide or a poor oxide, it may be
necessary to remove it and reoxidize the surface for optimal
imaging.
The oxide may be removed by dipping the sample in a buffered HF
(BHF or BOE) solution such as 10:1 DI H20:BHF. BHF/BOE is
available from any chemical vendor serving the microelectronics
industry. Etch rates will depend on the type of oxide being etched.
For thermal oxides, 10:1 BHF etches at approximately 90 to
* http://www.co2clean.com/afm.htm

120 nm/min at room temperature. It can then be reoxidized using

the UV-Ozone method described below. For cross-sectional or
beveled surfaces, the “Polishing” and “Oxidation” procedure is
described below. Polishing at an angle other than 90 degrees can
be achieved by mounting the sample at the desired angle in the
polishing chuck.
Polishing is performed on a standard polishing wheel, using
non-adhesive lapping films of decreasing grit size, with the final
polishing step performed with a colloidal silica slurry on a
polishing cloth, and a final rinse with a diluted hydrogen peroxide
oxiding solution. The polishing procedure (excluding the oxidation
step) is the same as is used in high quality sample preparation for
failure analysis and characterization of silicon integrated circuits.
Customers with little or no experience with polishing should
consult with polishing equipment vendors or companies with
expertise in silicon sample preparation.
It is useful to use a sample holder that can be used for sample
preparation and imaging without removing the sample. This
allows one to iterate between cleaning/polishing and imaging
quickly while maintaining the exact same polishing surface.
Polishing Procedure
Wet the wheel surface with some water and place the lapping film
on the polishing wheel. Use the rubber squeegee to squeeze out
the water underneath the lapping film. This will leave a very thin
layer of water to hold the lapping film in place.
Place the silicon sample in the sample holder, attach the sample
holder to the polishing chuck, and place it over the polishing
wheel. Typical total polishing times for each step is from tens of
seconds to about a minute using a ~85 gm polishing chuck on a
~2 mm x 2 mm sample.
1 Lower the chuck onto the surface of the 30 μm diamond
lapping film while rotating at 50 rpm under DI water flow.
Polish deep enough to produce a flattened surface over the
entire region of interest. Remove the chuck, and rinse the
sample with DI water to remove any polishing grit. Check the
result with the optical microscope.When satisfied, remove the
lapping film and replace it with a film with a 15 μm particle
size, then go to step 2.
2 Lower the chuck onto the surface of the 15 μm diamond
lapping film at 50 rpm under DI water flow rotated by 10

degrees about the polishing chuck axis relative to the previous

polish.
a Polish the sample for a couple of minutes; time is
determined by sample area, pressure on sample and grit
size.
b Remove the sample, rinse with DI water until all grit has
been removed, and look at it under the optical microscope.
Continue to polish until the 30 μm striations are no longer
seen.
The change in axial angle will allow a clear differentiation between
the new polishing grooves (15 μm grit) and those produced by the
30 μm grit size. It is important to view the sample under the
optical microscope at various angles (rotating through 360
degrees), as the polishing grooves often cannot be seen until a
certain angle is reached.
3 Replace the lapping film with the next smaller grit size.
4 Repeat the procedure described in step 1 and step 2 using the
6 μm, 1 μm, 0.3 μm, 0.1 μm and 0.05 μm grit sizes. Each
polishing step needs to be long enough to completely
eliminate the grooves and polishing damage done by the
previous polishing step.
5 Remove the lapping film, and replace it with the polishing
cloth. The polishing cloth is usually attached to the polishing
wheel with an adhesive backing.
6 Apply a small amount of the 0.02 μm colloidal silica slurry on
the polishing cloth and adjust the rotation rate to 10 rpm.
Lower the sample into the slurry for 10 seconds at a fixed
angle. Then rotate the sample by 90 degrees and polish for
another 10 seconds. Repeat until the sample has been rotated
through 360 degrees. Then rotate the sample clockwise while it
is in contact with the colloidal slurry for 10 seconds, then
reverse direction (counter clockwise) and rotate for another 10
seconds.
7 Turn the rotation speed up to 50 rpm and immediately spray
the oxidizing rinse solution (H2O:H2O2:NH3OH) on the sample
for 5 seconds while it is still in contact with the pad.
8 Flood the surface with DI water for a minute to flush out the
colloidal solution.
9 Remove the sample and rinse it directly with DI water. Let the
DI water in the polishing machine flood the polishing pad to
flush it out for the next use.

After any polishing step, one may wet the sample surface with DI
water and rub it with a Q-tip or texwipe to remove any diamond
particles that might have dislodged from the lapping film. This will
insure the next polishing step with a finer grit will not have
residual diamond particles that could scratch the surface.
Also, note that if you are looking at a large area of devices,
occasional large scratches need not be removed, as there are
many locations away from the particular scratch where the
imaging can be performed.
Oxidation
The next step is to improve the oxide layer on the polished
surface, beyond the oxide that was formed during the final rinse
step. For non-polished samples, this oxidation step may be
performed directly after the oxide removal using the 10:1 DI
H20:BHF solution discussed in the “Polishing” section, or after the
oxidizing rinse solution is applied.
Ensure that all process gases are properly vented.

C A U T IO N
A dedicated UV-Ozone oxidation/strip chamber may be utilized

for the oxidation process. A typical process will use 0.5 L/min O2
flow under a UV light source with the sample at 300 °C for 30
minutes. It is also possible to perform the oxidation on a hot plate
at 300 °C in air while exposing the sample to UV radiation. In all
cases, proper venting of process gases is necessary.
The oxide formed from the last step is typically thin, uniform, with
a small amount of oxide charge. At this point one may wipe the
surface of the sample with a texwipe or Q-tip to remove any dirt or
dust that gets on the sample without harming the surface. The
sample is then ready for measurements.
Final Finish
Several researchers have found CO2 snow-jet cleaning to be an
effective way to render consistent samples for SCM and SMM. We
recommend a final clean with such a method, as well as a
touch-up clean if the sample gets dirty or sits in air for several
days or more. The CO2 cleaning uses a specially designed nozzle
fitted to a standard ultra-high purity CO2 tank with about 850 psi

pressure. Adiabatic cooling of the CO2 gas as it exits the nozzle

causes the gas to freeze into small particles, hence the name
“snow-jet”. These CO2 particles can knock off large particles on
the sample surface. The CO2 particles also melt and dissolve
organic materials that may have contaminated the sample. In
order to avoid water condensation during the cleaning, the
sample should be heated.
Use a standard heat gun directed at the sample from about 3
inches away. With the sample sitting on an aluminum chuck, heat
the sample a bit and then start the CO2 cleaning. The sample
must be held firmly in place as the CO2 jet has very high pressure.
If cleaning continues too long and the sample cools enough so
water starts condensing on the surface, let the sample heat up
again, and re-clean.
CO2 snow-jet nozzles may be purchased from a few vendors. One
is Applied Surface Technologies (www.co2clean.com), which also
has useful background information on the technique.
Some researchers have seen large changes in surface potential

NOTE
after snow-jet cleaning. It is worth checking this as SCM/SMM
dopant profiling depends on the surface potential.

User’s Guide
4
Imaging in SMM Mode
Setting Up the Scanner Assembly 23
Inserting the Universal Nose Cone 24
Removing the Universal Nose Cone 26
Inserting a Probe in the Universal Nose Cone 28
Inserting the Scanner and Connecting Cables 29
Setup for Optional dC/dV Controller Module (DPMM) 34
Software Setup for SMM Mode 36
Determine Frequency for Microwave Signal 36
Settings for Optional dC/dV Controller Module 39
Because this is a specialized technique, it is assumed that the

user has experience with Scanning Probe Microscopy and with
using Contact Mode imaging. This chapter will cover the steps
that are specific to SMM Mode imaging preparation procedures.
The procedures in this manual use NanoNavigator 1.8 and higher.

NOTE
Setting Up the Scanner Assembly

The Keysight SMM Mode uses a unique SMM Mode nose
assembly which holds the cantilever at a 12° angle relative to the
horizontal sample surface and contains a contact point to apply
the microwave signal to the probe. Due to the microwave
shielding, extra care is required for inserting and removing the
SMM Mode nose cone on the scanner assembly.
These procedures are specific to SMM Mode and should be
followed by standard contact image procedures.
Imaging in SMM Mode 4
Inserting the Universal Nose Cone

The nose assembly is held in the scanner by an O-ring around its
circumference. To insert the SMM nose assembly, first place the
scanner in the scanner mounting fixture as shown in Figure 7.
Figure 7 Metrology scanner in mounting fixture
Place the SMM nose assembly on the scanner, aligning the

contact pins with the sockets in the scanner. Apply even, steady,
vertical pressure at the edges of the nose cone to settle the pins
into the sockets, as shown in Figure 8.

Figure 8 Carefully insert nose assembly in scanner, aligning the

pins with the sockets in the scanner
Push evenly and straight down when inserting the nose assembly
C A U T IO N
and be sure the pins are aligned with the sockets.
After installation, the SMM Mode nose assembly on the scanner

should appear as shown in Figure 9.
Figure 9 SMM Mode nose assembly mounted in scanner

Removing the Universal Nose Cone
A removal tool is included with your system to limit damaging

lateral forces on the scanner while removing the nose assembly.
The following is the only acceptable procedure for removing the
nose assembly:
Figure 10 Nose assembly removal tool
1 Place the scanner in the scanner mounting fixture.

2 Carefully slide the removal tool onto the nose assembly,
ensuring that the opening seats on both sides of the nose.
3 Position your thumb on the flat surface of the removal tool and
your fingers on BOTH sides of the extraction arm.
4 Gently pull up with your fingers while pushing down with your
thumb (Figure 11).

5 Once the nose assembly is clear of the scanner you can remove
it from the tool.
Figure 11 Using the nose assembly removal tool
Do not use the nose removal tool to insert a nose assembly. It is

C A U T IO N
not designed for this purpose.
DO NOT use tweezers or any other tool to remove the nose

C A U T IO N
assembly. The nose assembly removal tool is the only acceptable
method for extracting the nose from the scanner.

Inserting a Probe in the Universal Nose Cone

Conductive cantilevers are required for SMM Mode. One type of
cantilever uses Pt-Ir wires for the tip and has a gold contact pad
on the back to carry the microwave signal. This design will provide
a longer tip service life than a standard cantilever.
1 Loosen the set screw holding down the probe mounting clip as
shown in Figure 12.
Figure 12 Loosen probe clip. Do not remove set screw.
Do not remove set screw. Only loosen enough to allow probe to fit
C A U T IO N
under clip.
2 Load an SMM mode cantilever in the recessed portion of the

probe holder in the base of the nose assembly (Figure 13),
sliding it under the contact point. If using a cantilever with a
contact pad, ensure that the pad is facing up and touching the

contact point of the nose cone. The contact point is shown in

Figure 13.
Figure 13 SMM probe mounted in nose assembly. Ensure that

probe is below contact pin under probe clip.
3 Tighten the set screw to clamp the probe in place. Do not

over-tighten the set screw.
Inserting the Scanner and Connecting Cables

At this point the probe, nose assembly, and scanner should all be
assembled into one unit.
1 Ensure that there is adequate clearance below the scanner
socket in the middle of the microscope.
2 Position the scanner, with nose assembly already inserted,
above the scanner opening in the microscope. Feed the Nose
Assembly Connector Cable through the opening.
3 Place the scanner assembly into the scanner socket, ensuring
that the connector pins on the scanner align with the socket on
the microscope base.
4 Rotate the two securing clamps so they engage the scanner
and then push them down to the locked position.

5 The magnetic block on the nose assembly cable will be

attached to the sample plate when the sample plate is placed
in position, as shown in Figure 14.
Figure 14 View of sample area.
If the doors of the sample chamber are to be installed during

NOTE
scanning, feed the free end of the Nose Assembly Connector
Cable through the port in the bottom of the chamber before
continuing to the next step.
6 Connect the nose assembly cable to the Low Loss cable, as

seen in Figure 15. Use the supplied torque wrench to tighten
the connection to 8 lb-in.
Figure 15 SMM nose assembly cable shown passing through a

port in sample chamber before being connected to Low Loss
cable.

7 Attach the T Connector into a port in the front of the PNA.

Ensure that the side of the T Connector with a shallow punch is
facing the PNA (Figure 16 and Figure 17).
Figure 16 T Connector with punch mark on one side
Figure 17 T Connector attached to the PNA

8 Plug the free end of the Low Loss Cable from the nose
assembly to the T Connector as shown in Figure 18.
Figure 18 Low Loss Cable connects to the front port of the T

Connector
The other connections are shown schematically in Figure 19
Figure 19 Schematic of SMM cable connections, including

optional DPMM module

The AFM Controller is connected to the T Connector and optional

DPMM module using BNC to female SMB cables. See Figure 20.
9 Connect one BNC-to-SMB cable to the open port on the top of
the T connector. The other end connects to the AFM Controller
front panel BNC labeled Basic Outputs, AUX 1.
10 If using the optional DPMM module, connect the other
BNC-to-SMB cable to the DPMM. The other end connects to
the AFM Controller front panel BNC labeled Basic Inputs, AUX
1.
Figure 20 BNC to SMB cable connections
11 Align the laser on the cantilever as usual.

12 Follow the standard procedure for setting up tip approach.

Setup for Optional dC/dV Controller Module (DPMM)

The SMM Mode technique is capable of mapping the capacitance
and impedance properties. It is also possible to measure the
dopant concentration for a semiconductor material using the
Keysight dC/dV Controller Module, also known as the DPMM
module.
Figure 21 Keysight DPMM Module (left) and dC/dV power supply
Set the voltage on dC/dV power supply FIRST. Set one voltage to
C A U T IO N
5 V and the second voltage to 7 V.
1 Set the dC/dV power supply voltage to 5 V and 7 V.

a For the 5 V (V1) banana plug cables, connect red to the
positive terminal and black to the negative.
b For the 7 V (V2) banana plug cables, connect red to positive
and black to negative.
2 Remove the top two U-shaped brackets from Port 1 of the
PNA.
3 Connect the DPMM to the top 4 connectors (CPLR ARM, RCVR
A IN, SOURCE OUT, and CPLR THRU) with the dC/dV
connection side facing left as shown in Figure 22 and
Figure 23.
4 Using the 4 pin connector, connect the module to the dC/dV
power supply.

5 Connect the signal cable from the DPMM Module to the Basic
Inputs, AUX 1 BNC on the front of the AFM Controller, using the
supplied BNC-to-SMB cable.
.
Figure 22 DPMM with connection on the right
Figure 23 Cabling diagram for DPMM connections

Software Setup for SMM Mode

This setup is to be done after the initial computer and component
setup detailed in Chapter 2, Keysight SMM Mode Components
and Setup.”
1 Launch NanoNavigator software.
2 On any page in NanoNavigator, click on AFM Settings in the
top right corner, select Hardware Settings and open the
Network Analyzer tab (Figure 24).
Figure 24 Select the Present check box to enable communication

between NanoNavigator and the PNA.
Determine Frequency for Microwave Signal

The next few steps describe the procedure for determining the
correct frequency for the microwave signal. This is an iterative
process and will require more than one frequency sweep.
3 Go to the Load page and open the SMM TUNE tab.
4 In the sweep configuration table (Figure 25), set the Start
Frequency to 0.5 GHz.
5 Set the End Frequency to 6.0 GHz.
6 Set the Sweep Points to 256.
a Sweep Points can be increased if greater resolution is
needed.
b Note that the sweep time will increase with larger sweep
points.

Figure 25 Settings for PNA and Sweep parameters, Advanced

panel (Basic is similar)
Different model PNAs will have different frequency ranges. In any

NOTE
case, the idea is to begin with a broad frequency sweep and zoom
into the desired resonant peak in an iterative process, as
described below.
7 Click Begin Sweep. NanoNavigator will display the result of the

initial sweep.
Figure 26 Typical result from initial sweep over a wide frequency

range.

8 Markers can be added to the graph by either using the Tools

menu (hover the cursor over the plot to access the Tools menu)
or clicking directly on the plot. Add two markers and use them
to determine frequencies slightly above and below the peak
with the largest amplitude difference.
Figure 27 Menus used to add markers to the frequency plot and

to read the position of the markers.
9 After the peak position has been defined by the markers, type
the marker positions into the Start and End Frequency text
boxes.
10 Click Begin Sweep to repeat the frequency over this reduced
range. A typical result is shown in Figure 28
Figure 28 Typical result after a reduced frequency range sweep.
11 Repeat the process of placing markers to define the upper and

lower frequency values of the desired peak, this time over a
reduced range. Click Begin Sweep to repeat the sweep over
the reduced range.
12 Repeat this process as many times as needed to obtain a well
defined peak position. A typical result is shown in Figure 29

13 Sweep the frequency again. The Amplitude vs Frequency

display should be similar to that shown in Figure 29.
Figure 29 Amplitude vs Frequency graph for final frequency peak

selection
14 Use one of the markers to determine the location of the

frequency peak as shown in Figure 29. Note the actual selected
frequency can be near the peak on either side.
15 Enter the value into the Scan Frequency (GHz) box in the
Configuration table on the SMM TUNE tab.
Configure the SPM as usual for Contact Mode imaging.
Settings for Optional dC/dV Controller Module

Additional settings are required for using the DPMM Module as
shown in Figure 30.
1 Go to the Measure screen and open the Scan tab in Advanced
mode (The gear icon will be orange in Advanced mode. Click
on the icon if it is not orange).
2 Scroll down to the Secondary Lock-ins, Lock-in 1table. If
necessary, expand the table by clicking the right-pointing
arrow(s).

Figure 30 Secondary Lock-ins parameter table (top) and Aux

Output Selection window (bottom)
3 Set Input to Aux In 1.

4 Set Output to Tip Bias Modulation.
5 Select Enable Drive check box. A typical value for the
Frequency is 10 kHz and a Drive of 2 V.
6 In the Preferences window (AFM Settings > Preferences in
main NanoNavigator window), set Aux Output 1 to Drive 1.
7 Select the appropriate Channels in the Scan tab (Figure 31).

Figure 31 SMM imaging channels
The PNA Amplitude and PNA Phase data contain information

about the impedance at the point where the tip is in contact. This
is a qualitative measurement until calibration control samples are
available. Amplitude 1 and Phase 1 channels are obtained from
the optional DPMM Module and correspond to the dC/dV
measurements. These channels measure the dopant
concentration of a semiconductor dopant sample and are
currently qualitative data. An example of these are shown in
Figure 32 where the capacitance and dC/dV measurements reveal
the underlying dopant structures not shown in the topography
image. Once the SMM measurements have been calibrated as
described in Chapter 5, Calibrated Imaging with SMM Mode, the
PNA Capacitance and PNA Conductance channels will provide
quantitative results.
Amplitude 1 image contrast may be enhanced by changing the
phase offset in the Secondary Lock-ins table (Figure 30 on
page 40). This will reduce the contrast for Phase 1.
Begin scanning and optimize the contact mode image as
described in the 9500 User’s Guide.
Example images of a SiGe transistor device are shown in Figure 32
on page 42.

Figure 32 Examples of simultaneous images of a) topography, b)

capacitance, and c) dC/dV measurements of a SiGe transistor
device
Troubleshooting
- Samples are usually grounded. If it is not grounded and the
image is not stable, try to ground the sample.
- If there does not appear to be good contrast for the PNA or
dC/dV images, try a different peak to determine the frequency
for the microwave signal.

User’s Guide
5
Calibrated Imaging with SMM Mode
Capacitance Calibration 44
Capacitance Calibration Standard 44
SMM Imaging of the Calibration Standard 45
Calculating the Capacitance Signal 50
Calibrating the Capacitance Measurement 53
Cleaning the Capacitance Standards 55
Dopant Profile Calibration 56
Dopant Profile Calibration Standards 56
SMM dC/dV Imaging of the Calibration Standard 57
Calibrating the Dopant Measurement 70
Applying the Calibration to Unknown Samples 73
Cleaning the Dopant Profiling Standards 73
This chapter outlines the steps to calibrate the SMM setup for
quantitative capacitance and dopant imaging. Quantitative
measurements require a calibration standard for capacitance and
two standards, p and n-type, for dopant imaging. These standards
are imaged in SMM mode and are used to calibrate the system.
This chapter references material in Chapter 4, Imaging in SMM

NOTE
Mode and Chapter 5, Contact Mode Imaging with SMM Mode. Be
sure to review and understand Chapter 4 and Chapter 5 before
continuing with the Capacitance and Dopant calibration
procedures.
The procedures in this manual use NanoNavigator 1.8 and higher.

NOTE
Calibrated Imaging with SMM Mode 5
Capacitance Calibration
The capacitance calibration procedure requires SMM imaging of a
calibration standard, data processing using PicoImage to
determine the capacitance signal and background values,
calibrating the capacitance in PicoView, and finally quantitative
SMM capacitance imaging in PicoView.
Capacitance Calibration Standard

A sample with a series of micro-capacitors that vary in lateral
dimension and dielectric thickness is used as a calibration
standard. Four different circular contact pads (gold on top of
titanium) with diameters between 1 and 4 μm were fabricated on
each step of a staircase structure; the height of the silicon dioxide
(SiO2) staircase structure ranges from 50 to 200 nm, with step
sizes of 50 nm. The contact pad and SiO2 thicknesses vary with
standard type. Refer to the sample specification sheet for these
values.
Figure 33 Capacitance calibration standard with the selection of

the region of interest highlighted by red squares
Figure 33 shows overview images of a calibration standard, with

subsequent zooms to the region of interest used for the
calibration procedure. Figure 33a shows the 1x1 cm wide
calibration standard, with the different areas showing different
designs of the micro-capacitors arrangement. The red squares in
b to d show the region of interests for capacitance calibration.
Finally, in Figure 33d, the area that should be used for SMM
imaging is enclosed within the red square.
The specifications for the calibration standard will be included
with the standard and are also described in Appendix A. Nominal
thickness values will be included. However, the step measured

with AFM can be different from the nominal values due to surface
contamination or other unknown reasons. A cross-section of a
calibration standard is shown schematically in Figure 34.
Figure 34 Schematic of calibration standard showing gold (Au)

contacts over SiO2 steps of varying height on a silicon
substrate
SMM Imaging of the Calibration Standard

To begin imaging, follow the steps for image preparation:
1 Insert the nose cone assembly into the scanner.
2 Insert a probe into the nose cone assembly.
3 Place the scanner in the microscope and connect its cables,
including those for the microwave signal.
4 Align the laser on the cantilever.
5 Insert and align the detector.
6 Prepare the calibration standard and mount the sample plate.
7 Connect the sample to the sample bias DAC through the
auxiliary EC cable.
For systems with an optional adapter stand, the standard sample

NOTE
plate with adapter stand configuration cannot be used with the
SMM nose cone due to its size and shape.

8 Position the SMM probe over one of the capacitor structures as

shown in Figure 35.
Figure 35 Camera View window (left) showing probe over

capacitor structures (right) for calibration procedure
After approaching the SMM probe to the sample, the amplitude

and phase frequency curves are acquired using a PNA sweep. The
microwave frequency is adjusted by acquiring an Amplitude [dB]
vs. Frequency [GHz] spectrum.
9 Choose Controls > PNA to open the PNA Sweep window if it is
not already open.
10 In the Sweep section on the right panel, enter a Sweep Start of
1 GHz and a Sweep End of 6 GHz.
11 Click the Sweep button.
Figure 36 Amplitude vs Frequency sweep when the probe has

approached the sample surface

A typical frequency spectrum from 1 to 6 GHz is shown in

Figure 36. From the PNA sweep a minimum is chosen, circled in
red, and the frequency adjusted closely to the minimum of the
resonance. The resulting PNA sweep is shown in Figure 37 on
page 47. Typically a frequency slightly left of the minimum is
selected (linearity of the resonance curve) by adjusting the value
for the Scan Frequency parameter. This can be entered manually
or set by moving the slider on the frequency sweep curve.
Figure 37 PNA sweep after selecting a sharp minimum
After selecting the microwave frequency, the parameters in the

NOTE
PNA Sweep window need to be kept constant. Any change in the
parameters may lead to a change in the calibration factor.
After selecting the microwave frequency, the imaging setpoint

(i.e. imaging force) is adjusted to get optimal electrical tip-sample
contact.

Begin imaging:
1 In the Realtime Images window, choose to display Topography
and PNA Amplitude with 1st order Flatten for each image.
2 Typical Setpoint values are between 1 to 3 V.
3 Set the scan speed from 0.7-1 ln/s.
4 The scan area should be between 50 - 70 μm.
5 In the PNA Sweep window:
a IFBW (Intermediate Frequency bandwidth) is typically set to
500-700 Hz.
b The Power Level is set to ~7 dBm.
A proper electrical tip-sample contact is observed in the PNA

amplitude image when the gold pads of the calibration standard
show continuous and homogeneous PNA amplitude signals, as
shown in Figure 38 on page 48
Figure 38 Topography (left) and SMM PNA Amplitude (right)

images of the calibration standard
In the Topography image (left in Figure 38), the various gold pads
can be observed on the four different steps of the staircase
structure, ranging from 200 nm to 50 nm in height. In the PNA
amplitude image (right on Figure 38), continuous and
homogeneous electrical tip-sample contact is observed on the
gold pads. The various colors indicate different PNA amplitude
values, corresponding to different capacitance values.

The diameter of the gold pads and the step heights of the
NOTE
dielectric staircase structure can vary from sample to sample.
Accordingly they should be measured for each calibration
procedure using the topographical image.
Tips to improve the quality of the PNA amplitude image
1 Increasing the setpoint might lead to an improved electrical

tip-sample contact. Particularly this is important when the
gold pads show inhomogeneous signals and intermittent
contact in the PNA amplitude image, as shown in Figure 39.
Figure 39 PNA amplitude images of the calibration standard with

good electrical tip-sample contact (left image) and with
intermittent electrical contact (right image)
2 Reduce the IFBW to reduce the noise. This also automatically

reduces the scan speed.
3 Select another calibration region of the calibration standard.
There are several identical calibration regions that can be used
for calibration. See Figure 33 on page 44 for illustration.
4 Clean the sample to reduce contamination of the surface.
Several methods are described in Cleaning the Capacitance
Standards on page 55.
5 Change the cantilever and use a different SMM probe. The tip
may not be clean, resulting in intermittent electrical contact
properties as shown in Figure 39.

Calculating the Capacitance Signal
After obtaining a PNA amplitude image of the capacitance

calibration standard with good quality, load the image into
PicoImage to calculate the SiO2 film thickness and the
capacitance signal, i.e., the difference of PNA amplitude between
the Au pad and the surrounding SiO2. To calculate the SiO2 film
thickness, one can calculate the relative step height against the
silicon substrate using a Step Height Measurement procedure.
Calculating the capacitance signal may be more difficult if there is
poor quality of the PNA amplitude image caused by intermittent
electric contact between the tip and the Au pad. There can be
many ways of performing the calculation. The following procedure
is a simple and easy approach, but one can follow more
sophisticated procedures to get more accurate results if
necessary.
1 In PicoImage, select the Zoom function.

2 Zoom (Figure 40) to a rectangular region that includes a row of
Au pads of the same size.
Figure 40 Zoom operation in PicoImage

3 Select the Conversion to a series of profiles operator as shown

in Figure 41 on page 51. This step requires PicoImage
Advanced or Expert version. The image can be line corrected
before the conversion.
Figure 41 Conversion to a series operation in PicoImage
4 Extract (Figure 42 on page 52) the lower envelope profile from

the series of profiles (or the upper envelope profile if the
amplitude signal goes in opposite direction).

Figure 42 Extracting a profile in PicoImage
5 Perform a Step Height Measurement (Figure 43 on page 53)

using the extracted profile. Manually set the background level
for each step if the AUTO step detection introduces obvious
error in the measurement. The background value can be read
out from the profile by switching to absolute scale for the
Y-axis.

Figure 43 Step Height Measurement in PicoImage
6 Note the Background (reference line used by PicoImage to

measure depth) and Signal (mean depth) values for the
capacitance calibration calculation in PicoView.
Calibrating the Capacitance Measurement

Return to the PicoView software.
1 In the PNA section of the PNA Sweep window, click the
Capacitance Calibration... button as shown in Figure 44.
Figure 44 Use the Capacitance Calibration... button to open the

PNA Capacitance Calibration window
This will open the PNA Capacitance Calibration window.

2 In the PNA Capacitance Calibration window, shown in

Figure 45, enter the Au pad area and the thickness of each SiO2
step (using the nominal value if you like) and the
corresponding amplitude Signal measured in PicoImage in
step 6.
A linear regression of the data will be plotted and the coefficient is
calculated from the slope of the linear fit. The capacitance offset
is the average from the background PNA amplitude close to each
pad. In the step height measurement in step 5, the background is
already averaged by PicoImage, giving the common background
value for all pads.
Figure 45 PNA Capacitance Calibration window
3 Click the Apply button to set the Capacitance Coefficient and

Offset values for real time capacitance imaging.

4 Return to the Realtime Images window, add a buffer and select

PNA Capacitance for the data type to image capacitance
quantitatively.
Cleaning the Capacitance Standards

The following methods are recommended for cleaning the
capacitance standard sample. Note that a conductive glue, ie.
silver paint, may need to be reapplied to attach the sample to the
metal sample puck.
The calibration standard is manufactured in a clean environment.
Users should take care to keep it clean and uncontaminated.
Follow the procedure below if needed.

WA R N IN G
1 Use a CO2 snow-jet (described in Chapter 3, Sample

Preparation for Dopant Profiling) cleaning method:
a Use a standard heat gun directed at the sample from about
3 inches away.
b With the sample sitting on an aluminum chuck, heat the
sample a bit and then start the CO2 cleaning. The sample
must be held firmly in place as the CO2 jet is very high
pressure.
c If cleaning continues too long and the sample cools enough
so water starts condensing on the surface, let the sample
heat up again, and re-clean.
2 Use a chemical cleaning solution:
a Put a drop of Piranha cleaning solution (a 3:1 mixture of
concentrated sulfuric acid to 30% hydrogen peroxide
solution) on top of the sample. Since the surface is
hydrophobic in general, the liquid holds as a droplet on the
surface,
b Take care not to spread the liquid over the edge of the
sample as it will attack the epoxy and the metal disc below.
c Rinse thoroughly with DI water after one hour.
d Repeat and heat to ~70 °C if necessary.

3 Use a detergent cleaning solution:

a Sonicate the sample in Alconox solution for 5 min, followed
by sonication in clean Millipore water for 2 min.
b Rinse the sample under flowing Millipore water for 30
seconds. Alconox residue may be left on the surface if not
rinsed sufficiently.
c Dry the sample with compressed N2.
4 Wipe the area of interest with an acetone-dipped Q-tip. Shake
off excessive solvent from the Q-tip and apply a single sweep
with one smooth motion from one side of the sample to the
other. Check under an optical microscope (5x) to see if the
areas of interest are at the center of the tip path and are not
covered by residues from the solvent.
Dopant Profile Calibration

For dopant profiling, the SMM is used in dC/dV mode with the
DPMM (Dopant Profile Measurement Module) attached to the
PNA. For proper installation, please refer to Chapter 4, Imaging in
SMM Mode.
The dopant calibration procedure requires optimizing the SMM
dC/dV imaging of a calibration standard, analyzing the
cross-section to calibrate the dopant profile in PicoView, and
finally quantitive SMM dopant imaging in PicoView.
For dopant profile measurements we recommend RMN (Rocky

NOTE
Mountain Nanotechnology) conductive full metal probes
12Pt400B (spring constant 0.3 N/m, 8 N/m, or 16 N/m). Stiff
levers make better electric contact, but are mostly suited for flat
samples with little topography variation because of larger imaging
force.
Dopant Profile Calibration Standards

There are two standards for the dopant profiling calibration: one
for n-type and one for p-type. If the sample of interest has both
types of dopants, then both standards will needed for calibration.
The dopant profiling reference sample is manufactured by
growing layers of varying dopant concentration onto a Si wafer as
shown in the schematic view in Figure 46 left panel. Layer
thicknesses range from several hundred nanometers to several
microns. The resulting structure is then cleaved and polished to

expose the thin layers side by side in the cross section. The
calibration standard is mounted vertically by gluing it on a
conductive gold plate or putting it in a mini-bench vice as shown
in Figure 46 right panel.
Figure 46 Mounting the calibration sample. Left: Sketch of the

sample. Middle: Reference sample glued vertically on a gold
disc via conductive silver paint. Right : Reference sample
mounted vertically by a mini-bench vice.
For all types of calibration samples the highest dopant

concentrations are located on the edge of the sample nearest to
the highly reflecting side (Figure 46, center panel). The detailed
dopant profiles for the calibration standards are shown on the
specification sheets in Figure 50 on page 63 (for n-type sample)
and in Figure 55 on page 68 (for p-type sample).
SMM dC/dV Imaging of the Calibration Standard

To begin, follow the steps for image preparation:
1 Insert the nose cone assembly into the scanner.
2 Insert a probe into the nose cone assembly.
3 Place the scanner in the microscope and connect its cables,
including those for the microwave signal.
4 Align the laser on the cantilever.
5 Insert and align the detector.
6 Prepare the calibration standard and mount the sample plate.
7 Connect the sample to the sample bias DAC through the
auxiliary EC cable.
8 Connect the dC/dV module (DPMM) as directed in Setup for
Optional dC/dV Controller Module (DPMM) on page 34.
9 Adjust the settings in the Advance AC Mode control window as
described in Settings for Optional dC/dV Controller Module on
page 39.

For systems with an optional adapter stand, the standard sample

NOTE
plate with adapter stand configuration cannot be used with the
SMM nose cone due to its size and shape.
Scan Area Adjustments

The cantilever is approached to the cleaved or polished cross
section face close to the edge of the highly reflecting side of the
sample.
Figure 47 CCD Camera view of the calibration sample and the

cantilever
1 Position the SMM probe over the edge of the sample as shown
in Figure 47.
2 Start scanning with a small scan size.
The n-type standard requires 70 μm scans while for the p-type
standard 5 μm are required.
3 Optimize the scan area according to the specific sample and
approach the tip carefully towards the edge during imaging.

For the 5600 this can be done by changing the X Offset in the
stage controller box (Figure 47, encircled in red). For the 5400 and
5500 bring the tip close to the edge of the sample through a
combination of scan offset and manually moving the sample
plate.
4 Display the edge of the sample on the Topography channel as

shown in Figure 48 on page 59.
Do not scan over the edge of the sample as the tip could be
damaged by colliding with the edge of the sample as shown on
the right, circled in red in Figure 48. It should be mentioned that
the optical CCD camera image and the scan are rotated by 180 °
in the default PicoView setting. The optical view can be rotated in
the Camera Setting window in the Camera View window.
Avoid scanning over the edge to minimize damaged caused by the

NOTE
tip colliding with the sharp edge of the sample.
Figure 48 Topography image (left) and cross-section profile

(right) showing the edge of the sample. Dopant profile
measurements are done close to the edge of the cleaved and
polished surface of the sample, near the highly reflecting side
of the sample.

dC/dV Parameter Settings

While most parameters are set before starting the measurement,
the AC Drive amplitude should be optimized during imaging.
1 Choose Controls > AC Mode Tune to open the Advanced AC
Mode Controls window.
2 Go to the Lock-in 3 tab and set the following:
a AC Drive (100 % = 10 V amplitude): 10-30 %.
b Frequency: 12 kHz (typical values between 10 and 50 kHz)
a Gain: 64 (or 128)
a Input: Aux
3 Go to the Outputs tab and set the following:
a Tip Bias: Drive 3
b Aux 1: Amplitude 3
c Aux 2: Phase 3
d Aux 3: X-Component 3
e Aux 4: Y-Component 3
f Clear the Pass Through check box for Aux 1-4
Minimize the AC Drive amplitude typically to 10 % (corresponding

to 1 V amplitude or 2 V peak-to-peak). If the drive amplitude is set
too high (e.g. 50 % or higher), typically larger dC/dV Amplitude
signals result but are less accurate. Examples of typical settings
for the Advanced AC Mode Controls windows are shown in
Figure 49.

Figure 49 Advanced AC Mode Controls settings for Lock-in 3 (left)

and Outputs (right) tabs
dC/dV Imaging of Dopant Calibration Standards

Up to eight data channels may need to be opened for imaging. In
the Realtime Images window, click the + button to add buffers
until enough image windows are displayed. Select the Input
Channels with the following data types. Note these channels do
not have to be opened simultaneously but selected as needed:
1 Topography
2 Deflection
3 PNA Amplitude (optional)
4 PNA Phase (optional)
5 Aux 1 (dC/dV Amplitude)
6 Aux 2 (dC/dV Phase)
7 Aux 3 (dC/dV X-Component) (optional)
8 Aux 4 (dC/dV Y-Component) (optional)
The Aux settings should correlate with settings in the Advanced
AC Mode Controls Outputs tab.

Optimize Parameters for dC/dV Imaging

Generally there are three relevant parameters for optimizing
dopant profiling by SMM:
- PNA Frequency
- AC Drive (100 % = 10 V amplitude = ±10 V = 20 V peak to
peak range)
- DC Tip Bias
The procedure of parameter optimizing is quite similar for n-type
and p-type standards. Parameter optimization is outlined for the
n-Type Standard sample and the p-Type Standard.
When optimizing the dC/dV imaging parameters for the first time,
do a manual sweep from 1-20 GHz in steps of 100 MHz on the
calibration standard initially.
Once the system is characterized, start with the unknown sample
and find the optimum PNA frequency. Then proceed with the
same frequency on the calibration standard. It is recommended to
start with frequencies around 4 GHz, 11 GHz, and 15 GHz.
n-Type Standard
On the n-type calibration standard, Layer 2 and Layer 3 have
dopant concentrations that are close to each other. It is important
to optimize the parameters such that Layers 2 and 3 show
different dC/dV signals. Layer 3 must have a higher dC/dV signal
than Layer 2 because a lower the dopant density will have a larger
dC/dV signal. Non-optimal parameter settings might result in
non-monotonic behavior of the dC/dV vs dopant concentration
plot. Use the cross-section profile of the dC/dV Amplitude to
check for non-monotonic behavior. For proper calibration,
imaging parameters should be selected in order to show a
monotonic calibration curve.
Table 1 details the dopant density in atoms/cm³ of different layers
for the calibration standards used. The layers are illustrated in the
specification sheet for the n-type standard shown in Figure 50.

Table 1 Dopant density of different layers for calibration

standards.
Sample Layer 4 Layer 3 Layer 2 Layer 1
n-Type 1.05x1016 8.70x1017 1.60x1018 3.65x1019
p-Type 8.80x1016 1.70x1018 1.60x1019 9.10x1019
Figure 50 Specification sheet for the n-doped calibration

standard sample
The specification sheet depicted in Figure 50 gives an overview

about the dopant steps on the n-type calibration sample named
Layer 1 (highest dopant density, 3.65*1019 atoms/cm³) to Layer 4
(lowest dopant density, 1.05*1016 atoms/cm³).
PNA Frequency
After approaching the cantilever to the sample, the PNA
frequency is adjusted using the PNA sweep in the Keysight PNA
Controls window.
1 Sweep the PNA and obtain an Amplitude [dB] vs. Frequency
[GHz] spectrum from 1-20 GHz as depicted in Figure 51 on
page 64 (left).
2 Select a resonance minimum and adjust the PNA frequency at
a point near a resonance minimum (Figure 51, right).

Not all resonances are susceptible for SMM measurements. If no

NOTE
contrast is seen in the dC/dV channels use a different nearby
resonance. Furthermore, it's also possible to make proper dC/dV
images at frequencies where no resonance is found in the PNA
sweep. Select an arbitrary frequency and search locally by
changing the frequency in 2 MHz steps up and down.
Figure 51 Left: PNA sweep from 1-20 GHz (PNA amplitude top
and PNA phase bottom). Right: PNA sweep for selecting a
single resonance minimum (top is PNA amplitude and bottom
is PNA phase).
For n-type samples, the PNA frequency is preferably between

10-20 GHz, showing a better signal intensity compared to lower
frequencies (e.g. 2 GHz).
3 Optimize the PNA frequency in 1-2 MHz steps up and down
during scanning by using Ctrl+Shift+Scroll.
It is also possible to optimize the PNA frequency by scrolling the
mouse wheel while holding Ctr+Shift to move the PNA frequency.
To change frequency in smaller steps, the red frequency line can
be dragged by a mouse click (Figure 51 on page 64, right) during
scanning.
A signal change can then be observed in the dC/dV channels
(Aux 1-4).
4 Choose Tools > Real Time Cross Section to open the Real Time
cross section tool.

In Figure 52 the influence of PNA frequency changes on the

dC/dV Amplitude signal is illustrated. The figure on the left shows
dC/dV Amplitude data at different PNA frequencies applied
during scanning. The cross-section is shown in the figure on the
right for frequency f3 (19.440 GHz-15 MHz).
Figure 52 Left: Three different PNA frequencies around

19.440 GHz applied on the n-type sample. Right:
Corresponding cross-section of the frequency with the highest
dC/dV Amplitude signal f3.
5 Change the frequency in 2 MHz steps upwards and downwards

while monitoring the Real Time cross-section profile to find the
frequency which results in the best dC/dV signal.
For calibrated dopant density measurements the PNA frequency

NOTE
should be the same for the calibration standard and the unknown
sample.
AC Drive
6 Change the AC Drive between 10 % and 30 % while monitoring

the Real Time cross-section profile to find the AC Drive which
results in the best dC/dV signal.
Figure 53 on page 66 contains dC/dV Amplitude data (left) for the

n-type sample at different AC Drives, ranging from 10 to 30 % that
were applied during scanning at a fixed frequency of 17.608 GHz.
The image on the right shows the cross-section profile at 30 %.

Higher AC Drive leads to slightly higher signals in the dC/dV

Amplitude channel, at the cost of averaging over a wider range of
voltages.
Figure 53 dC/dV Amplitude data at different AC Drives (left).

Right: Extracted cross section profile at 30 % AC Drive (3 V
Amplitude). DC Tip Bias: 0 V
For 30 % AC Drive, the cross section profile is extracted on the

right of Figure 53. The lowest dopant stripe (Layer 4) shows the
highest dC/dV Amplitude signal. The signal decreases
monotonically towards the highest doped stripe (Layer 1).
Typically the dC/dV signal is between 30 mV and 500 mV on the
calibration standards, depending on the tip diameter. When the
tip diameter is very large due to a blunt tip, the dC/dV signal
could reach up to1 V.
DC Tip Bias
For n-type samples, positive values of the DC Tip Bias are used
(e.g. 0 V to 3 V), while for p-type samples negative values are
used (e.g. 0 V to -3 V).
7 Be sure that the bias is set to the Tip (and not to sample) in the
Servo dialog box under Advanced tab (Apply bias to tip).
8 Optimize the DC Tip Bias using 0.1 V steps to get good
contrast between different layers of dopant concentrations
best results in the dC/dV signal.
Figure 54 shows the dC/dV Amplitude image at different tip
biases acquired at 17.608 GHz. In this case the tip bias was
changed from 2 V to 3.5 V.

Figure 54 Left: DC Tip Bias varied during scanning from 2 V to

3.5 V. Right: Extracted cross section profile of the highest
signal regime at 3 V DC Tip Bias. AC Drive: 10 %.
For 3 V DC Tip Bias the cross section is displayed on the right of

Figure 54. The cross section of the optimized signal shows a
monotonic behavior with the highest signal at the lowest dopant
(Layer 4) and the lowest signal at the highest dopant density
(Layer 1).
Start with the unknown sample and optimize the DC Tip Bias in
small steps (100 mV steps or less). Then go with the selected DC
Tip Bias on the calibration standard.
For bi-polar doped materials either:
- Work around 0 V DC Tip Bias as proper operating point for
both n-and p-doped regions, or
- Acquire two subsequent images, one being a p-sensitive
image (with optimized DC Tip Bias in the negative voltage
range) and the other one being an n-sensitive image (with
optimized DC Tip Bias in the positive voltage range). Use
those optimized DC Tip Bias voltages then for the p- and
n-doped calibration standards.
p-Type Standard
For the p-type standard sample, a scan area of about 5 μm is
recommended. Figure 55 on page 68 shows the dopant steps on
the p-type standard named Layer 1 (highest dopant density,
9.1x1019 atoms/cm³) to Layer 4 (lowest dopant density,
8.8x1016 atoms/cm³). The dopant values for the layers are given
in Table 1 on page 63.

Figure 55 Left: Specification sheet for p-type calibration

standard. Upper right: dC/dV Amplitude data acquired at
2.2 GHz PNA frequency. Lower right: Corresponding cross
section profile showing a monotonic behavior of dC/dV
Amplitude versus dopant density. AC Drive: 15 %, DC Tip Bias:
-1.4 V.
For calibrated dopant density measurements the PNA frequency

NOTE
should be the same for the calibration standard and the unknown
sample.
The parameter optimization is done similar to the n-type standard.
PNA Frequency

After approaching the cantilever to the sample, the PNA

frequency is adjusted using the PNA sweep in the Keysight PNA
Controls window.
1 Sweep the PNA and obtain an Amplitude [dB] vs. Frequency
[GHz] spectrum from 1-20 GHz.
2 Select a resonance minimum and adjust the PNA frequency at
a point near a resonance minimum.
3 Optimize the PNA frequency in 1-2 MHz steps up and down
during scanning.
4 Choose Tools > Real Time Cross Section to open the Real Time
cross section tool.
5 Change the frequency in 2 MHz steps upwards and downwards
frequency which results in the best dC/dV signal.
AC Drive
6 Change the AC Drive between 10 % and 30 % while monitoring
the Real Time cross-section profile to find the AC Drive which
results in the best dC/dV signal.
DC Tip Bias
For p-type samples, negative values are used (e.g. 0 V to -3 V) for
DC Tip Bias.
7 Be sure that the bias is set to the Tip (and not to sample) in the
Servo dialog box under Advanced tab (Apply bias to tip).
8 Optimize the DC Tip Bias using 0.1 V steps to get good
contrast between different layers of dopant concentrations
best results in the dC/dV signal.
In Figure 55 the dC/dV Amplitude image and the corresponding

cross section of a scan at 2.2 GHz PNA frequency are displayed.
The dopant levels show monotonic steps with the lowest signal at
the highest dopant (Layer 1) and vice versa. Layer 1 with the
highest dopant is located next to the edge while Layer 4 the
lowest dopant is located on the inner side of the sample next to
the bulk. Generally it has to be mentioned that the bulk is difficult
to image with the dC/dV signal dropping significantly and
therefore the bulk is excluded from the calibration procedure.

Similarly as for the n-type standard, the proper setting of PNA

Frequency, AC Drive and DC Tip Bias is essential for p-typed
standards to get a monotonic behavior of the dC/dV Amplitude
signal with the dopant density.
Calibrating the Dopant Measurement

The dC/dV Amplitude image of the dopant calibration standard is
acquired and the cross-section profile analyzed. Note it may be
necessary to acquire data at more than one frequency, depending
upon the unknown sample of interest. At higher PNA frequencies,
the signal-to-noise ratio is improved with respect to lower PNA
frequencies, as observed in the cross-section profiles.
From the cross-section profile, the dC/dV Amplitude voltage
values are taken for the various dopant levels and plotted with
respect to the corresponding dopant concentrations, taken from
the dopant standard specification sheet. The plot of dC/dV
Amplitude versus dopant concentration is henceforth called the
calibration curve.
Thus the calibration curve procedure follows these steps:
a Acquire a dC/dV Amplitude image of the dopant calibration
standard.
b Analyze the image using a Cross Section tool.
c Create a calibration curve with the dC/dV Amplitude data
and known concentrations from the standard

To create a calibration curve in PicoView:

1 In the PNA section of the PNA Sweep window, click the Dopant
Calibration... button as shown in Figure 56 to open the PNA
Dopant Calibration window.
Figure 56 Use the Dopant Calibration button... (circled in red) in

the PNA Sweep window to open the PNA Dopant Calibration
window
2 Calibrate the system using the dC/dV Amplitude and known

concentrations from the standard. Use the + or - buttons to
add or subract rows for the calibration data as shown in
Figure 57. Note the units for Amplitude are in V.
Figure 57 Right panel of PNA Dopant Calibration window with

data for calibration curve

The mean values of the dC/dV Amplitude are plotted with respect
to the dopant levels from the dopant calibration standard
specification sheet. Calibration curves for the n-type and p-type
standard samples are shown in Figure 58.
Figure 58 Dopant profiling calibration curves for n-typed standard

(left, 17.5 GHz) and p-type standard (right, 2.2 GHz).
For proper comparison of dC/dV signals between calibration

standard and unknown sample it is important to keep the imaging
parameters like PNA Frequency, AC Drive and DC Tip Bias
constant. However, there are several additional factors related to
non-uniform sample properties that influence the accuracy of the
calibration procedure. Uncertainties are introduced mainly from
varying quality of tip-sample junctions (e.g. changing
tip-diameter), contamination of the sample surface and changes
of the insulator thickness of the MOS junction.
Every time the SMM hardware is changed (e.g. cantilever change,

NOTE
cables, etc) it is recommended to repeat the calibration
procedure. The absolute dC/dV Amplitude values might vary from
setup to setup.

Applying the Calibration to Unknown Samples

The following steps summarize the procedure for quantitative
dopant imaging:
1 Image the appropriate (p-type or n-type) dopant calibration
standard.
2 Generate the calibration curve.
3 Image the unknown sample, using the same settings and
hardware configuration used for the calibration standard.
4 In the Realtime Images window, select Dopant Concentration
as a data channel to use the dopant calibration data.
Cleaning the Dopant Profiling Standards

The following methods are recommended for cleaning the dopant
profiling standard samples. Note that a conductive glue, e.g.,
silver paint, may need to be reapplied to attach the sample to the
metal sample puck.

WA R N IN G
1 Wipe the interested area with acetone or isopropanol using a

Q-tip. Shake off excessive solvent from the Q-tip and apply a
single sweep with one smooth motion from one side of the
sample to the other. Check under an optical microscope (5x) to
see if the interested areas are at the center of the tip path and
are not covered by residues from the solvent.
2 Use a buffered HF solution to remove thick oxidation layers:
a Put a drop of buffered HF solution on the sample for a few
seconds.
b Take care not to spread the liquid over the edge of the
sample.
c Rinse thoroughly with DI water.
3 Use a standard polishing procedure for a fine polish to avoid
surface roughness.

4 Use a CO2 snow-jet (described in Chapter 3, Sample

Preparation for Dopant Profiling) cleaning method:
a Use a standard heat gun directed at the sample from about
3 inches away.
b With the sample sitting on an aluminum chuck, heat the
sample a bit and then start the CO2 cleaning. The sample
must be held firmly in place as the CO2 jet has very high
pressure.
c If cleaning continues too long and the sample cools enough
so water starts condensing on the surface, let the sample
heat up again, and re-clean.

User’s Guide
Appendix A
Capacitance Standard
Specifications
Specifications 77
A sample with a series of micro-capacitors that vary in lateral

dimension and dielectric thickness is used as a calibration
standard (Figure 59). Four different circular contact pads (gold on
top of titanium) with diameters between 1 and 4 μm were
fabricated on each step of a staircase structure; the height of the
silicon dioxide (SiO2) staircase structure ranges from 50 to
200 nm, with step sizes of 50 nm. The height of the SiO2 steps is
controlled to within ± 10 nm by an applied etching technique. The
exact height of each step can be measured precisely by AFM with
a well-calibrated Z range of the AFM scanner.
The area that should be used for SMM imaging is enclosed within
the red square in the figure below.
Capacitance Standard Specifications A
Figure 59 Capacitance calibration standard
A scanning electron microscope (SEM) image of a contact pad is

shown in Figure 60.
Figure 60 SEM image of a 1 μm-wide contact pad

Capacitance Standard Specifications A
Specifications
The diameter, area and thickness specifications are tabulated
below. The diameters are for the bottom of the contact pad where
the electrical contact is located.
Contact Pad 1 μm 2 μm 3 μm 4 μm
Diameter
Error in diameter ± 0.01 μm ± 0.01 μm ± 0.01 μm ± 0.01 μm
Error in area (μm2) 0.785 ± 4.0 % 3.142 ± 2.0 % 7.069 ± 1.3 % 12.566 ± 1.0 %
Contact Pad Materials Titanium Gold

Thickness 20 nm 200 nm
Error ± 5 nm ± 5 nm
SiO2 Step Size 1 2 3 4

Thickness 50 nm 100 nm 150 nm 200 nm
Error ± 10 nm ± 10 nm ± 10 nm ± 10 nm

Index
Index
A N
Atomic Force Microscope, 1 NanoNavigator, 15
nose assembly, 10
removal, 27
C nose cone, 8
cables, 26
cabling configuration, 13 P
cantilever, see probes
capacitance, 2, 3, 8, 11 performance network analyzer, 11
cleaning, snow-jet, 21 PNA, 11, 15
complex reflection coefficient, 2 settings, 15
Contact Mode, 1 probe, 2, 9
platinum-iridium, 10
D R
dC/dV, 3, 4, 6, 41
Realtime Images window, 48
dC/dV controller module, 8, 34
reflection, 11
device under test (DUT), 3, 11
reflection mode, 5
dielectric constants, 2
router connection, 13
dopant density, 2
DPMM module, 8, 39
DUT, see device under test S
sample preparation, 17
E final finish, 21
oxidation, 21
ECal kit, 4 polishing, 18, 19
electromagnetic properties, 2 supplies, 18
scanning capacitance microscopy, 2, 17
scanning microwave microscopy, 1, 2, 17, 23
I Scanning Probe Microscope, 1
scanning tunneling microscopy, 2
impedance, 2, 3, 5, 8, 11
SCM, see scanning capacitance microscopy
installation
hardware needed, 12 SMM mode, 2, 3, 5, 6, 8
nose assembly, 23
setup, 14
L spectroscopy, 7
SMM, see scanning microwave microscopy
lock-in amplifier, 3, 6 software troubleshooting, 16
M T
microwave frequencies, 6 transmission, 11
microwave shielding, 5, 10, 23 transmission mode, 5

Index
V
vector network analyzer, 11
VNA, 2, 5
VNA, 3, 11
W
wiring, 26

This information is subject to change without notice.
© Keysight Technologies 2013, 2014
Edition C, May 2017
*N9546-90002*
N9546-90002
www.keysight.com

9500 Scanning Microwave Microscopy Mode Users Manual

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Keysight Scanning Microwave

Keysight SMM Mode User’s Guide i

Read This First

Keysight SMM Mode User’s Guide iii

These specifications apply to the Keysight 5420, 5500 and 5600LS

Equipment Class I, Pollution Degree 2, Installation Category II.

Stop using the scanner if the scanner cable insulation is damaged

Keysight SMM Mode User’s Guide iv

Voltage and Laser Safety Information

The following symbol indicates hazardous voltages:

This system is designed to be used with a Class II diode laser with

Keysight SMM Mode User’s Guide v

In accordance with federal FDA requirements, the following laser

Procedure for Changing Input Voltage

Piezo Scanner Precautions

Keysight SMM Mode User’s Guide vi

calibration can be verified using a calibration standard, and

General Care Requirements

The Declaration of Conformity (DoC) included in this document

Keysight SMM Mode User’s Guide vii

Keysight SMM Mode User’s Guide viii

Customer Technical Support

Distributors and Account Representatives

Keysight SMM Mode User’s Guide ix

1 Introduction to Scanning Microwave Microscopy Mode

2 Keysight SMM Mode Components and Setup

3 Sample Preparation for Dopant Profiling

4 Imaging in SMM Mode

5 Calibrated Imaging with SMM Mode

A Capacitance Standard Specifications

Scanning Microwave Microscopy (SMM) Mode is a specialized

Overview of Keysight Scanning Microwave Microscopy (SMM) Mode

Keysight SMM Mode User’s Guide 2

increases the dynamic range and sensitivity of the impedance

Figure 1 Overview of SMM Mode with Keysight’s VNA (left), and

Scanning Impedance Microscopy

Keysight SMM Mode User’s Guide 3

The incident microwave signal travels through a series of

Scanning Capacitance Microscopy

Keysight SMM Mode User’s Guide 4

Vector Network Analyzer

reflected signal transmitted signal

The incident signal is generated and controlled inside the VNA. As

Keysight SMM Mode User’s Guide 5

to improve the instrument’s electromagnetic compatibility with its

Figure 2 9500 SMM Mode nose assembly and associated

Scanning Microwave Microscopy Mode

Keysight SMM Mode User’s Guide 6

Spectroscopy with Scanning Microwave Microscopy Mode

Keysight SMM Mode User’s Guide 7

Scanning Microwave Microscopy Mode is a specialized technique

In this User’s Guide, it is assumed that the reader is already

Figure 3 Components of Scanning Microwave Microscopy Mode

The procedures in this manual are for NanoNavigator1.8 and

Keysight SMM Mode User’s Guide 9

Conductive cantilevers are required for SMM Mode. One type of

Nose Cone Assembly

To take full advantage of the VNA-based measurement scheme,

Keysight SMM Mode User’s Guide 10

Figure 4 SMM Mode Nose Assembly detail

Vector Network Analyzer

Keysight SMM Mode User’s Guide 11

Figure 5 Keysight PNA