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Register a new userA New Heterodyne Megasonic Piezoresponse Force Microscopy with High-frequency Excitation beyond 100 MHz
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Piezoresponse Force Microscopy (PFM), as a powerful nanoscale characterization technique, has been extensively utilized to elucidate diverse underlying physics of ferroelectricity. However, the intensive study of conventional PFM has revealed a growing number of concerns and limitations which are largely challenging its validity and application. Herein, we developed a new advanced PFM technique, named Heterodyne Megasonic Piezoresponse Force Microscopy (HM-PFM), which uniquely uses 106 to 108 Hz high-frequency excitation and heterodyne method to measure the piezoelectric strain at nanoscale. We report that HM-PFM can unambiguously provide standard ferroelectric domain and hysteresis loop measurements, and an effective domain characterization with excitation frequency up to ~110 MHz has been realized. Most importantly, owing to the high-frequency and heterodyne scheme, the contributions from both electrostatic force and electrochemical strain can be significantly minimized in HM-PFM. Furthermore, a special difference-frequency piezoresponse frequency spectrum (DFPFS) measurement is developed on HM-PFM and a distinct DFPFS characteristic is observed on the materials with piezoelectricity. It is believed that HM-PFM can be an excellent candidate for the piezoelectric or ferroelectric studies where the conventional PFM results are highly controversial.
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Hafnium oxide (HfO2)-based ferroelectrics offer remarkable promise for memory and logic devices in view of their compatibility with traditional silicon CMOS technology, high switchable polarization, good endurance and thickness scalability. These factors have led to steep rise in research on this class of materials over the past number of years. At the same time, only a few reports on the direct sensing of nanoscale ferroelectric properties exist, with many questions remaining regarding the emergence of ferroelectricity in these materials. While piezoresponse force microscopy (PFM) is ideally suited to probe piezo- and ferro-electricity on the nanoscale, it is known to suffer artifacts which complicate quantitative interpretation of results and can even lead to claims of ferroelectricity in materials which are not ferroelectric. In this paper we explore the possibility of using an improved PFM method based on interferometric displacement sensing (IDS) to study nanoscale ferroelectricity in bare Si doped HfO2. Our results indicate a clear difference in the local remnant state of various HfO2 crystallites with reported values for the piezoelectric coupling in range 0.6-1.5 pm/V. In addition, we report unusual ferroelectric polarization switching including possible contributions from electrostriction and Vegard effect, which may indicate oxygen vacancies or interfacial effects influence the emergence of nanoscale ferroelectricity in HfO2.
To achieve quantitative interpretation of Piezoresponse Force Microscopy (PFM), including resolution limits, tip bias- and strain-induced phenomena and spectroscopy, analytical representations for tip-induced electroelastic fields inside the material are derived for the cases of weak and strong indentation. In the weak indentation case, electrostatic field distribution is calculated using image charge model. In the strong indentation case, the solution of the coupled electroelastic problem for piezoelectric indentation is used to obtain the electric field and strain distribution in the ferroelectric material. This establishes a complete continuum mechanics description of the PFM contact mechanics and imaging mechanism. The electroelastic field distribution allows signal generation volume in PFM to be determined. These rigorous solutions are compared with the electrostatic point charge and sphere-plane models, and the applicability limits for asymptotic point charge and point force models are established. The implications of these results for ferroelectric polarization switching processes are analyzed.
We report ionic strength-dependent phase shifts in second harmonic generation (SHG) signals from charged interfaces that verify a recent model in which dispersion between the fundamental and second harmonic beams modulates observed signal intensities. We show how phase information can be used to unambiguously separate the chi(2) and interfacial potential-dependent chi(3) terms that contribute to the total signal and provide a path to test primitive ion models and mean field theories for the electrical double layer with experiments to which theory must conform. Finally, we demonstrate the new method on supported lipid bilayers and comment on the ability of our new instrument to identify hyper-Rayleigh scattering contributions to common homodyne SHG measurements in reflection geometries.
Domains walls and topological defects in ferroelectric materials have emerged as a powerful new paradigm for functional electronic devices including memory and logic. Similarly, wall interactions and dynamics underpin a broad range of mesoscale phenomena ranging from giant electromechanical responses to memory effects. Exploring the functionalities of individual domain walls, their interactions, and controlled modifications of the domain structures is crucial for applications and fundamental physical studies. However, the dynamic nature of these features severely limits studies of their local physics since application of local biases or pressures in piezoresponse force microscopy induce wall displacement as a primary response. Here, we introduce a fundamentally new approach for the control and modification of domain structures based on automated experimentation whereby real space image-based feedback is used to control the tip bias during ferroelectric switching, allowing for modification routes conditioned on domain states under the tip. This automated experiment approach is demonstrated for the exploration of domain wall dynamics and creation of metastable phases with large electromechanical response.
Frequency dependent dynamic behavior in Piezoresponse Force Microscopy (PFM) implemented on a beam-deflection atomic force microscope (AFM) is analyzed using a combination of modeling and experimental measurements. The PFM signal comprises contributions from local electrostatic forces acting on the tip, distributed forces acting on the cantilever, and three components of the electromechanical response vector. These interactions result in the bending and torsion of the cantilever, detected as vertical and lateral PFM signals. The relative magnitudes of these contributions depend on geometric parameters of the system, the stiffness and frictional forces of tip-surface junction, and operation frequencies. The dynamic signal formation mechanism in PFM is analyzed and conditions for optimal PFM imaging are formulated. The experimental approach for probing cantilever dynamics using frequency-bias spectroscopy and deconvolution of electromechanical and electrostatic contrast is implemented.
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