Abstract
The ability to reliably measure electromechanical properties is crucial to the advancement of materials design for applications in fields ranging from biology and medicine to energy storage and electronics. With the relentless miniaturization of device technology, the ability to perform this characterization on the nanoscale is paramount. Due to its ability to probe electromechanical properties on the micro- and nano-scales, piezoresponse force microscopy (PFM) has become the premier tool for piezoelectric and ferroelectric characterization of a new generation of smart, functional materials. Despite its widespread use and popularity, PFM is a highly nuanced technique, and measurements on similar samples using different machines and/or in different laboratories often fail to agree. A comprehensive protocol for accurate quantitative measurements has not been presented in the literature, slowing the general uptake of the technique by reducing the ability of research groups to take full advantage of PFM for their characterization needs. Here, we present a procedure for PFM measurements, which outlines the practical aspects of quantitative PFM, from sample preparation to probe choice and use of control samples, and we substantiate these steps with original data on lithium niobate control samples. This quantitative characterization protocol is critical as society looks to smaller, greener alternatives to traditional piezoelectric materials for applications such as drug delivery, bio-microelectromechanical system sensors and actuators, and energy harvesting.
Highlights
Atomic force microscopy (AFM), in particular its voltage modulated variant piezoresponse force microscopy (PFM), has become an indispensable tool for the study of mechanical and electromechanical phenomena in a wide variety of functional materials.[1,2] While traditionally used to investigate piezoelectricity and ferroelectricity in ceramics and polymers, PFM has seen a renaissance in its use to probe biological materials
We present a procedure for PFM measurements, which outlines the practical aspects of quantitative PFM, from sample preparation to probe choice and use of control samples, and we substantiate these steps with original data on lithium niobate control samples
If the sample is not sufficiently fixed to the substrate, low frequency resonances can occur, often in the range used for the conventional PFM (20–40 kHz), which creates an unwanted artificial “piezoresponse.”[29] If the sample has been placed on the substrate through a method such as drop casting and the surrounding solvent has evaporated, the crystals left behind will often be naturally adhered to the substrate
Summary
Atomic force microscopy (AFM), in particular its voltage modulated variant piezoresponse force microscopy (PFM), has become an indispensable tool for the study of mechanical and electromechanical phenomena in a wide variety of functional materials.[1,2] While traditionally used to investigate piezoelectricity (the linear coupling between stress and polarization, or electric field and strain) and ferroelectricity (a spontaneous polarization that can be reversed by the application of an external electric field) in ceramics and polymers, PFM has seen a renaissance in its use to probe biological materials. In PFM, an oscillating electric field between the probe tip and sample results in local deformations of the sample surface, provided the sample is piezoelectric. The probe is placed in contact with the sample and the piezoelectric response of the surface is detected as the first harmonic component, A1ω, of the probe tip deflection A, which is given as
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