Piezo Response Force Microscopy (PFM)

The word “piezo” is derived from the Greek information with correlative surface
word piezein, meaning “to press tightly”. topography. This mode of operation of AFM
Piezoelectricity is the ability of a material to is often termed as Piezo response Force
convert mechanical energy (pressing) into Microscopy (PFM). PFM can measure
electric energy (polarization) and vice deformations in the sub-nanometer regime
versa. The direct piezoelectric effect is the and map ferroelectric domains with a
generation of electric polarization in lateral resolution of a few nanometers.
response to an applied stress. The
directionality and the magnitude of
polarization is proportional to the stress How does it work?
applied, and the polarization can have
components in the parallel and AFM is a surface characterization
perpendicular directions. The opposite technique that rasters a fine needle at the
phenomenon, the inverse piezoelectric free end of a cantilever across the sample
effect, is the generation of a mechanical surface. Light is reflected off the back of the
deformation in response to an applied cantilever onto a position sensitive
electrical field. photodiode that registers the motion of the
cantilever.
Piezoelectric materials are prevalent in our
everyday lives. For example, ferroelectric
materials are a subset of piezoelectric
material that possess an inherent
spontaneous polarization and can be found
in capacitors, nonvolatile memory,
ultrasound imaging, data storage,
thermistors, oscillators, filters, light
deflectors, modulators, and monitors, to
name a few. In fact, atomic force
microscopes (AFM) rely on the inverse
piezoelectric effect in their scanner design.
As components continue to miniaturize in
the electronics industry, piezoelectric thin
films have also become a significant area of
interest (e.g. functionally coated flexible
glass). Thin films exhibit piezoelectric
behavior in distinct regions (often called Figure 1: Schematic of a Piezo-response Force
domains) in the sub-nanometer regime. Microscopy experiment. Voltage is applied to a
Understanding the domain size as well as conductive tip in contact with sample and mechanical
their response under an applied electric deformation of the sample is measured by the
deflection of the laser.
field enables dynamic measurements of
domain switching and local hysteretic
behavior. These material properties allow In PFM mode, AFM is operated in contact
researchers to understand structure mode where the cantilever is continously in
function relationships for material design. contact with the sample at a constant force.
To apply an electrical field over the sample,
AFM can measure the local inverse a sample is mounted on a conductive
piezoelectric response with high fidelity substrate and a conductive cantilever is
and provide high resolution piezoelectric used as the second electrode. Either

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electrode can be used to apply the voltage, If the response observed is purely
though the first generally performs parallel/antiparallel to the field (Figure
better. Figure 1 shows a schematic PFM 2a,b), the out-of-plane amplitude and
setup. phase of the vertical cantilever bending
provides direct information about the
To measure the piezo response, an AC magnitude and polarization (parallel vs.
voltage is applied between the tip and the anti-parallel) of the sample deformation. If
substrate causing a periodic expansion the polarization and electric field are
and/or contraction of the sample. With the perpendicular to one another (Figure c,d),
tip constantly in contact with the sample, inplane movement of the sample results.
the oscillatory movement of the sample
surface induces a periodic cantilever With a purely out-of-plane response, the
bending that is analyzed by the AFM effective piezoelectric coefficient, d33, can
controller’s lock-in amplifier. be calculated from the measured amplitude
(A) of the oscillation and the applied voltage
During PFM imaging, the amplitude and over the sample (VAC):
phase response of the cantilever are
recorded. Phase contrast in PFM provides 𝑑𝑑33=𝐴𝐴/𝑉𝑉𝐴𝐴𝐴𝐴
information about the direction of the
electrical polarization relative to electrical Below the resonance frequency of the
field. The amplitude shows the magnitude cantilever, the amplitude A can be
of the piezo response and can often be used expressed in pm (by converting voltage to
to discern features such as the position of distance using the cantilever deflection
domain walls. sensitivity) and the effective piezoelectric
coefficient can be measured quantitatively.
However, it is not straightforward to
compare d33 measurements obtained by
AFM with other bulk techniques. It is well
known that material properties can vary
significantly on the nanoscale compared to
the bulk, and the piezoelectric effect is no
exception.

In practice, materials can exhibit a

mechanical response in three dimensions.
Movement both in-plane and out-of-plane
Figure 2: Schematics of (a-b) vertical and (c-d)
relative to the sample surface can occur in
lateral PFM mode. The applied electric field (E) and response to the applied voltage. To capture
polarization (P) direc-tions are denoted with arrows. this, vector PFM is used to monitor both
Vector PFM is performed by combining data with a vertical and lateral deflection of the
0° and 90° rotation of the sample to obtain 3D cantilever. Additionally, a sample area is
vector information of the response. measured at two rotational orientations
with respect to the cantilever. The data can
The electrical polarization can have be mathematically reconstructed to
components both parallel/antiparallel as combine both the in-plane and out-of-
well as perpendicular to the applied field, plane vector components to provide a 3D
the AC field will result in out-of-plane and map of the piezo response.
in-plane oscillations of the sample surface,
thus causing vertical and lateral bending of Beyond imaging, AFM can also provide a
the cantilever, as denoted in Figure 2. means to spectroscopy, locally induce
polarization at the tip to understand

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material hysteresis or write domains using prevented, as this will reduce the field
lithography. These topics will be covered in strength over the sample and hence the
more detail below. piezo response.

Conductive cantilevers for PFM have a wide

Experimental setup range of force constants varying from <0.1
N/m to >40 N/m with a resonance
As illustrated in Figure 1, PFM requires an frequency range between 10-
AFM that can perform electrical 400 kHz. Stiffer cantilevers minimize the
measurements with conductive cantilevers. contribution of electrostatic interaction
To measure both the out-of-plane and in- with samples, whereas softer probes are
plane responses, two independent internal less prone to tip wear and sample damage
lock-in amplifiers are required to measure during scanning. While Pt/Ir coated probes
the amplitude and phase of each can be used for performing PFM
component. measurements, studies have shown that
conductive diamond or PtSi coated tips
An additional, essential part for many
have shown improved stability of the PFM
samples is a camera view that allows to view
signal. Another important parameter for
the sample from above to find areas of
measurements is the optical sensitivity,
interest, as illustrated in Figure 3.
which is inversely proportional to the probe
Particularly for 2D materials, the flakes of
length. Therefore, the shorter cantilevers
interest must be located and positioned
provide better signal.
under the cantilever.
Specialized PFM measurements such as
high-voltage PFM (HV-PFM) and dual
frequency response tracking (DFRT)
require additional instrumentation. For
HV-PFM, an additional high-voltage
amplifier is connected to a user output of
the AFM controller and directly controlled
from the AFM software. The user channel is
calibrated so that the user can directly set
the output voltage of the HV-amplifier.
DFRT-PFM will be explained in more detail
later. For this mode, Nanosurf equipment
can be combined with an external lock-in
Figure 3: A top view camera image is essential for amplifier from Zurich Instruments and
most PFM samples. This image shows flakes of 2D signals can be imported via user input
material on a gold substrate. Flakes of different channels. Zurich Instruments' lock-in
thickness appear as different colors in the image.
amplifiers are powerful tools, not only for
PFM, but other advanced AFM modes such
Several practical aspects of PFM are worth as frequency modulated, heterodyne Kelvin
mentioning, including sample preparation Probe Force Microscopy (KPFM), and other
and cantilever choice. While flat samples multi-frequency applications.
are generally suitable for performing PFM
as is, some rougher samples such as
ceramics may require polishing prior to Traditional PFM Applications
imaging. Care must be taken to work
with contamination-free surfaces. A thick Lithium niobate (LiNbO3) is versatile
insulating layer between conductive ferroelectric material and widely used in
substrate and sample should generally be applications ranging from waveguides to

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piezoelectric sensors. A PFM measurement and distinct domains can be more readily
is shown in Figure 4. This sample is observed (Figure 5c, arrow heads).
periodically poled and shows a pure out-of-
plane response with alternating domains
parallel and antiparallel to the applied field.
At ambient conditions, the piezo response
is stable over a large voltage range of the
applied electric field. The topography and
magnitude (amplitude signal) of the piezo
response are not affected by the
polarization, but phase changes by 180°
indicating that the electrical polarization is
switching in the out-of-plane direction.
The amplitude does not change
significantly between the oppositely poled
domains.

Figure 5: Vertical PFM imaging of 2D ferroelectric

CuInP2S6 on Silicon substrate. (a) amplitude (b)
phase and (c) amplitude projection, all
Figure 4: Vertical PFM images of periodically poled represented as a color overlay on the topography.
lithium niobate. (a) Representative topography with Image size: 5x5 µm2 (color scales do not include
phase information color overlaid for a 20x20 µm2 illumination effects from the topography
area showing, (b) horizontal profile of the amplitude visualization).
and (c) phase, showing little influence of amplitude
with polarity and the 180° phase shift as expected. Ferroelectric thin films are easily
Data courtesy: Brian Odermatt, EPFL/Nanosurf. characterized using PFM. Figure 6 shows
the piezoelectric characterization of a
Ferroelectric 2D materials and thin films piezoelectric and high magnetostrictive
are growing in interest with potential thin film that was grown using a sol-gel
applications in energy, electronics and process on a flexible glass substrate. The
optoelectronics. PFM of CuInP2S6 flakes on surface topography reveals "protrusions"
a silicon substrate are shown in Figure 5. with a dome-like morphology that are
The PFM measurement provides the microns across (Figure 6a). The amplitude
magnitude of the vertical deformation projections of the out-of-plane response
(amplitude image, Figure 5a) and the (Figure 6b) and the in-plane response
corresponding polarization direction (Figure 6c) clearly show the differences in
(phase image, Figure 5b). To more easily domain size and structure within individual
distinguish the polarization direction of an dome-like protrusions on the sample.
amplitude, the amplitude and phase
information can be combined by using an
amplitude projection (Figure 5c). By
multiplying the amplitude with the cosine
of the phase, which is 0° or 180° the sign is
consistent to the polarization direction,

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 Figure 7: Schematics showing (a) traditional PFM
measurement in off resonance mode and dual
frequency resonance enhanced PFM mode. (b-d)
DFRT amplitude response upon a change in contact
resonance frequency.

cantilever. Since PFM is performed in

contact mode, the first available resonance
frequency is the contact resonance, where
the cantilever makes a buckling movement
Figure 6: Out-of-plane and in-plane PFM response
recorded on a 800 nm PZT thin film, grown by sol- with both the tip and the base of the
gel method on Pt(111)/Ti/Flexible glass. (a) cantilever fixed. The sample is used
Topography, (b) out-of-plane amplitude projection, as a “shaker piezo”, to oscillate the
(c) in-plane amplitude projection. Image size: cantilever in its (contact) resonance, which
9x9 µm2 (color scales do not include illumination is about 4-5 times higher than the
effects from the topography visualization). Data fundamental resonance frequency of the
courtesy: Dr. Itamar Neckel, Brazilian Center for cantilever that is only fixed at one side.
Research in Energy and Materials – CNPEM, Brazilian
Synchrotron Light Laboratory LNLS. Working at the contact resonace is
susceptible to crosstalk between the PFM
response and other tip sample interactions,
Dual frequency resonance tracking because the contact resonance depends on
(DFRT) PFM the local stiffness of the sample. To avoid
this crosstalk, the DFRT mode was
In a traditional PFM measurement, the introduced. In DFRT mode, an AC voltage is
probe is oscillated at frequencies well applied at two frequencies on either side
below the resonance frequency of the of the contact resonance peak with equal
cantilever ( Figure 7a). A main advantage of amplitude (Figure 7b). When the contact
working at these frequencies is that the resonance shifts, the amplitudes also
deflection can be readily converted into undergoes a shift (Figure 7c) and a feedback
picometers, using the deflection sensitivity algorithm in the lock-in amplifier nullifies
of the cantilever. However, signals are the difference by modulation of the
often small and can be challenging to excitation frequencies. The difference
measure, particularly for thin samples. The ∆f between the two excitation frequencies
piezo response can be enhanced by is kept fixed in feedback (Figure 7d). By
working at a resonance frequency of the applying this method, changes in the

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 Figure 8: PFM measurement at contact resonance
frequency (a) amplitude (arbitrary units), (b) phase (c)
profile In the phase, showing domain widths ~100
nm range. Excitation: VAC=5 V at f=304 kHz,
Cantilever: Pt-coated Si with nominal spring constant
k=1.5 N/m. Image size: 3x3 µm2. Sample courtesy:
Prof. A. Kholkin, University of Aveiro, Portugal, data
Figure 9: Piezo phase response from a thin film
courtesy: Sergei Magonov, SPM labs, AZ
CuInP2S6 grown on a silicon surface imaged with
DFRT PFM showing oppositely polarized
contact resonance frequency are largely domains while applying <1 V of AC modulation.
decoupled from the PFM response.

Contact frequency enhanced PFM can be

Spectroscopy and high-voltage PFM
used to study the piezo-ceramic material -
lead zirconate titanate (PZT). Improvement To look beyond imaging, AFM can also be
of fatigue and retention of PZT can be made used for spectroscopy and to locally "write"
by adding small amounts of donor dopant domains by applying a DC bias to the
like ions of La3+. With signal enhancement sample. In spectroscopy, the amplitude and
at the contact resonance frequency, grain phase of the piezo response are measured
and domain morphology of such samples as a function of an applied bias voltage over
can be successfully examined with PFM, as the sample. One of the main applications
illustrated in Figure 8. for spectroscopy is to determine the
voltage needed for domain reversal. In
As a demonstration of DFRT, the PFM phase
ferroelectric materials, the external voltage
signal of a thin film of CuInP2S6 is shown in
required to reverse a polarization is called
Figure 9. Despite a modualtion amplitude of
the coercive field. To reach the coercive
less than 1V, the amplification by the
filed may require bias voltages exceeding
contact resonance gives improved contrast
±10 V. In such cases a high-voltage amplifier
and makes the borders between oppositely
is connected to a user output and voltages
polarized domains clearer for visualization.
up to ±200 V can be applied. AC voltages
When using DFRT, quantification of the can also be applied via the high-voltage
amplitude of the response is more (HV) amplifier to improve the signal to noise
challenging than when performing ratio of weak piezoelectric properties. To
traditional PFM. The conversion of the perform HV-PFM, the sample must be
amplitude to picometers requires stable under high voltage and to prevent
additional calibration steps, as it depends physical harm to the user or damage to
on the quality factor of the contact electronic equipment, care must be taken
resonance and the deflection sensitivity for that no electronics are exposed when high
the buckling movement. voltages are applied.

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 Figure 10: Schematic diagram of SS-PFM
measurement depicting a train of DC bias pulses
on top of an AC modulation.

However, increasing bias voltage offset

increases the contribution of electrostatic
forces on the cantilever. This electrostatic
contribution may even exceed the PFM
response, obscuring domain reversal. Figure 11: Piezo response hysteresis loop of P(VDF-
Switching spectroscopy PFM (SS-PFM) is a TrFE) thin film (a) amplitude vs applied voltage and
spectroscopy method to reduce the effect (b) phase vs applied volt-age obtained by SS-PFM.
Sample courtesy: Joanneum Research
of electrostatics. Rather than ramping the
Forschungsgesellschaft mbH, Austria.
voltage linearly, a train of voltage pulses is
applied, switching off the voltage difference
in between. During this switching, the AC
voltage is continuously applied to record Polarization and lithography
the PFM response both in the on and off
states of the voltage. This is schematically Once the required voltage to overcome the
depicted in Figure 10. The “on” and “off” coercive field is known, for example from
states refer to the status of the DC bias an SS-PFM experiment, the tip can be used
voltage. While the DC voltage is used to to locally polarize the sample. Lithography
modify the polarization, the AC voltage is can be used to to write single domains,
used to measure the piezoelectric signal at domain arrays, and complex patterns
the same time. without changing the surface topography.
To demonstrate SS-PFM, amplitude and PFM high-voltage lithography on a P(VDF-
phase behavior of a P(VDF-TrFE) thin film is TrFE) thin film is demonstrated in Figure 12.
shown in Figure 11. The data were recorded The tip was biased and scanned in square
during the off phase of an SS-PFM regions to intentionally polarize regions
experiment. Pulses between -40V and +40V and reverse the polarity of a smaller region.
were applied using a HV amplifier. As the First, a 3x3 µm2 area was imaged while
voltage pulses were ramped upward, at applying a bias voltage of +40 V to the
+16 V the polarization switching was sample substrate. The polarization was
observed. This is indicated by the amplitude subsequently reversed by scanning areas of
dropping to zero and the 180° phase shift. 2x2 µm2, and 1x1 µm2 and applying -40 V and
As the voltage was ramped down, the +40 V, respectively. Figure 12 shows a 4x4
polarization switches back at -25 V, µm2 image of the PFM amplitude projection
returning to the starting point.

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 the electromechanical properties of
materials with nanometer spatial resolution
and picometers of sensitivity. Nanosurf
PFM capabilities extend beyond traditional
PFM imaging to improve signal to noise,
measure switching dynamics, perform
lithography, and apply high voltages
according to your experiment needs.

Notes:

1. PFM is available on CoreAFM, FlexAFM

Figure 12: PFM amplitude projection of P(VDF- and DriveAFM from Nanosurf.
TrFE) thin film after applying DC sample bias of 2. AFM and PFM images were processed
40 V, -40 V, and 40 V during consecutive scanning with MountainsSPIP 9.
of 3x3 µm2, 2x2 µm2, and 1x1 µm2 areas
respectively. The AC amplitude amounted to 5 V.
Sample courtesy: Joanneum Research
Forschungsgesellschaft mbH, Austria.

(amplitude multiplied with the cosine of the

phase) on the P(VDF-TrFE) film after these
manipulation steps. Outside the largest
area, the thin film is not polarized, and the
amplitude is consequently small. After
polarization with a positive substrate
voltage, the sample shows zero phase and
high amplitude, denoted by the magenta
color. The 500 nm green region shows Contact information
polarization reversal, with similar
Nanosurf AG
amplitude, but opposite sign, due to the
Gräubernstr. 12-14
180° phase difference. In the magenta inner 4410 Liestal
square represents a 1x1 µm2 region where Switzerland
the polarization was reversed a second [email protected]
time. Interestingly, the shape of the domain www.nanosurf.com
borders between the oppositely polarized
regions extend into the adjacent regions,
indicating collective switching of domains
outside the tip-sample contact area.

Conclusion

Understanding the piezo-responsive

behavior of materials will continue to be
critical for the advancement of a wide range
of technologies. Characterization on the
nanometer scale has emerged, as the
miniaturization of electronics continues.
PFM uniquely enables researchers to study

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