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Characterisation of piezoelectric materials

The reputation of NPL's expertise in functional materials has been built up through years of research and lies in the
characterisation of materials that have some extra function apart from their obvious mechanical or chemical properties.
Often it is a material that will couple one form of energy to another, for instance a piezoelectric will transform electrical
energy into mechanical displacement in an ultrasonic cleaning bath. The group has built up an extensive suite of
characterisation facilities for piezoelectric materials and the following lists some of these.

Polarisation Field (PE loop) analysis

The signature of a true ferroelectric material is the ability to switch electrically between two polarisation states, and this
is characterised using the polarisation loop method. The functional materials group at NPL have over 20 years' experience
in making these measurements and have used in house systems, commercial systems and also installed two in-situ
synchrotron beamline systems at Diamond and ESRF. The current workhorse is a an Aixacct Piezoelectric Evaluation
System (aixPES), which can test bulk samples at voltages up to 10kV, and at temperatures of up to 250C. This also has
an integrated SIOS interferometer system for the simultaneous measurement of piezoelectric displacements. The
software suite enables the automatic characterisation of the functional behaviour as a function of temperature, fatigue,
and coupled with an impedance analyser (HP 4192A) the measurement of C-V behaviour.

Effect of frequency on the polarisation loop response of a soft PZT 5H material

Measurement of the Pyroelectric Effect

Measurement of the pyroelectric coefficient of materials can be measured via two methods. The standard method is Byer Roundy, where the temperature of the
sample is cycled sinusoidally with an amplitude of a few degrees, whilst measuring the charge produced by the sample. This can be done above room temperature
using our Aixacct system, but with addition of a Peltier Element the temperature of the sample can be cooled to below room temperature. A second method is to use
the temperature dependence of PE loops, where the slope of a plot of the remnant polarisation against temperature also gives the pyroelectric coefficient.

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Pyroelectric charge response of a polymer sample excited with a triangular heat profile
using a Peltier element to control the temperature around ambient

Jamin Common Path Interferometer system

The displacements produced by piezoelectric materials under low field conditions can be smaller than is measureable
using a standard Michelson Interferometer set-up such as the SIOS attached to the Aixacct system. For instance,
piezoelectric quartz only displaces 2.3 pm with an applied voltage of 1V. To measure these sorts of displacements and
smaller movements associated with thin film piezoelectrics, NPL has developed a Jamin Common path system. Using a
common path set-up, coupled with lock-in techniques, it enables thermal and acoustic noise sources to be reduced
enabling sub pm displacements to be measured.
In order to measure the piezoelectric coefficient of a thin film material on a substrate, it is necessary to be able to
remove the bending contribution. Traditionally, this has been done using a beam path that interrogates the front and rear
surface of a thin film sample. However, the extended beam path means the size of the interferometer is large and
maintaining path stability over this size is more difficult. NPL has concentrated on design on the stability and registration of the sample holder such that a single sided
interferometer can be used on a thin film sample, measuring the front and rear separately and subtracting the results.

Resonance analysis for low field piezoelectric characterisation

For virtually any kind of finite element modelling of active piezoelectric devices, the first stumbling block people have is where to get all the data to populate the model.
For a model of a typical piezoelectric material with ∞mm symmetry, it requires six separate elastic constants, three piezoelectric coefficients and two dielectric
constants. This is where resonance analysis characterisation comes in. By analysing the resonance modes of four simple shaped samples, these parameters can be
derived. This method is defined in a European standard EN 50324-2 'Piezoelectric properties of ceramic materials and components Part 2: Methods of measurement
Low power'. The Functional Materials Group at NPL were involved in defining this standard, and have written a best practice guide on the method. The method can
also be extended to include losses where all the coefficients now have a real and imaginary part. These values are needed for some FEA codes that predict the loss.

Measurement of the piezoelectric coefficient using a Berlincourt tester

The measurement of the direct piezoelectric coefficient is a simple but effective test used in industry and academia to
characterise the piezoelectric output of samples. Sometimes termed a 'Berlincourt tester', it applies an oscillating force
and measures the resulting charge - the ratio is the piezoelectric coefficient. NPL has several Berlincourt type systems
that can measure the d33, d31 and dh hydrostatic piezoelectric coefficient over a frequency range from 30-300Hz. They
offer a rapid and cost-effective method of assessing the piezoelectric output of bulk materials in a variety of shapes and
forms. NPL has written a best practice guide on the method, and are also developing a MEMS based tool that will
perform a similar function on smaller samples.

LIMM measurement
In the most part ,characterisation of piezoelectric materials uses methods where sample sizes are of the order of
millimetres or larger, and any quantitative results are an average value of these samples. It also assumes that the properties are homogeneous throughout the sample
under test. Presently, the only technique where the spatial variation of the piezoelectric properties can be probed is piezoelectric mode atomic force microscopy, PFM,
but here the technique is limited to use on very small sample sizes.
In the laser intensity modulation method, LIMM - an intensity modulated laser - is used as a periodic heat source which generates a pyroelectric current within the
material that is detected using lock-in techniques. By changing the frequency of the intensity modulation, films can be probed to different depths. NPL has pioneered
the use of this method to characterise piezoelectric materials, and has extended its use into scanning samples. The system has been used to characterise the
polarisation variation of a number of different applications.

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LIMM image of a laser engraved PZT sample. The laser engraved sample must be
graphite coated to ensure an even laser absorption, and the engraved region shows
up as a region of low activity (blue).

Dielectric breakdown testing

The dielectric breakdown strength of materials is important for many dielectric materials applications, but particularly for piezoelectric materials where high fields are
needed to achieve the maximum output from a device. For breakdown tests on bulk materials to standards such as ASTM-149 or BS EN 60243-1, we have a 50kV
Sefelec dielectric breakdown tester. We have also carried out less routine breakdown investigations on piezoelectric materials, for example withstand voltage over
time whilst measuring leakage currents in high humidity.

Evidence of dielectric breakdown on the electrode surface of a piezoelectric

People
Mark Stewart
Markys Cain

Publications

Properties of morphotropic phase boundary Pb(Mg1/3Nb2/3)O3-PbTiO3 films with submicron range thickness on Si based substrates
M. Alguero, M. Stewart, M. G. Cain, P. Ramos, J. Ricote, M. L. Calzada
J. Phys. D.: App. Phys, 43 (20), 205401 (2010)
Spatial characterization of piezoelectric materials using scanning laser intensity modulation method (LIMM)
M. Stewart
J. Am. Ceram. Soc., 91 (7), pages 2176-2181 (2008)
Piezoelectric resonance
M. G. Cain, M. Stewart
Measurement Good Practice Guide No. 33 (2001)
Measuring piezoelectric d33 coefficients using the direct method
M. Stewart, W, Battrick, M. G. Cain
Measurement Good Practice Guide No. 44 (2001)

Last Updated: 23 Jan 2014

Created: 12 Mar 2012

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