A simple experimental method for piezoresponse force microscopy (PFM) measurements for reliable evaluation of piezoelectric surface displacements even on compliant surfaces is proposed based on atomic force microscopy (AFM) operated in frequency-modulation (FM) dynamic mode with constant excitation (CE), by using non-contact mode cantilevers. Surface displacement by piezoelectric effect after application of an electric potential to the conductive AFM probe translates into a likewise variation of the probe oscillation amplitude, while the related electrostatic forces mainly affect the oscillator resonant frequency, and cantilever bending is limited due to their high stiffness. Our non-contact CE-FM-PFM method is shown to reduce electrostatic force contributions as compared to contact-PFM modes. Converse piezoelectric effect mapping is demonstrated on poly(vinylidenefluoride) nanofibers obtained by electrospinning.
Effective converse piezoelectric coefficient (d33,eff) mapping of poly(vinylidene fluoride) (PVDF) nanofibers with ceramic BaTiO3 nanoparticle inclusions obtained by electrospinning was carried out by piezoresponse force microscopy (PFM) in a peculiar dynamic mode, namely constant-excitation frequency-modulation (CE-FM), particularly suitable for the analysis of compliant materials. Mapping of single nanocomposite fibers was carried out to demonstrate the ability of CE-FM-PFM to investigate the nanostructure of semicrystalline polymers well above their glass transition temperature, such as PVDF, by revealing the distribution of piezoelectric activity of the nanofiber, as well as of the embedded nanoparticles employed. A decreased piezoelectric activity at the nanoparticle site compared to the polymeric fiber was found. This evidence can be rationalized in terms of a tradeoff between the dielectric constants and piezoelectric coefficients of the component materials, as well as on the mutual orientation of polar axes.
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