Broadband nanodielectric spectroscopy by means of amplitude modulation electrostatic force microscopy (AM-EFM)

In this work we present a new AFM based approach to measure the local dielectric response of polymer films at the nanoscale by means of Amplitude Modulation Electrostatic Force Microscopy (AM-EFM). The proposed experimental method is based on the measurement of the tip–sample force via the detection of the second harmonic component of the photosensor signal by means of a lock-in amplifier. This approach allows reaching unprecedented broad frequency range (2–3×104 Hz) without restrictions on the sample environment. The method was tested on different poly(vinyl acetate) (PVAc) films at several temperatures. Simple analytical models for describing the electric tip–sample interaction semi-quantitatively account for the dependence of the measured local dielectric response on samples with different thicknesses and at several tip–sample distances

Thermo-magnetic behaviour of AFM–MFM cantilevers

Atomic force microscopy (AFM) experiments were performed to study the behaviour of AFM cantilevers under an external magnetic field B and temperature field produced by a coil with an iron core. Four cantilever types were studied. Forces were measured for different B values and at various coil-to-cantilever separation distances. The results were analysed on the basis of a phenomenological model. This model contains the contribution of two terms, one monopole-monopole interaction at short distance, and one apparent paramagnetic interaction in del B-2 at large distance, which represents the temperature effects. We observe a good agreement between the model and the experimental data

Nanodielectric mapping of a model polystyrene-poly(vinyl acetate) blend by electrostatic force microscopy

We present a simple method to quantitatively image the dielectric permittivity of soft materials at nanoscale using electrostatic force microscopy (EFM) by means of the double pass method. The EFM experiments are based on the measurement of the frequency shifts of the oscillating tip biased at two different voltages. A numerical treatment based on the equivalent charge method allows extracting the values of the dielectric permittivity at each image point. This method can be applied with no restrictions of film thickness and tip radius. This method has been applied to image the morphology and the nanodielectric properties of a model polymer blend of polystyrene and poly(vinyl acetate)

Nanoscale dielectric properties of insulating thin films: From single point measurements to quantitative images

Dielectric relaxation (DR) has shown to be a very useful technique to study dielectric materials like polymers and other glass formers, giving valuable information about the molecular dynamics of the system at different length and time scales. However, the standard DR techniques have a fundamental limitation: they have no spatial resolution. This is of course not a problem when homogeneous and non-structured systems are analyzed but it becomes an important limitation for studying the local properties of heterogeneous and/or nano-structured materials. To overcome this constrain we have developed a novel approach that allows quantitatively measuring the local dielectric permittivity of thin films at the nanoscale by means of Electrostatic Force Microscopy. The proposed experimental method is based on the detection of the local electric force gradient at different values of the tip-sample distance. The value of the dielectric permittivity is then calculated by fitting the experimental points using the Equivalent Charge Method. Even more interesting, we show how this approach can be extended in order to obtain quantitative dielectric images of insulating thin films with an excellent lateral resolution

Magnetic flux distortion in two-phase liquid metal flow: Model experiment

In this paper, we present the model experiments in order to study the magnetic flux distortion of a two-phase liquid metal flow excited by an AC magnetic field in a range of pulsation where Faraday induction and Lorentz force effects are significant. These experiments realized with solid aluminum rods allow to characterize the effects of flow velocity (0 ≲ U≤1 ms−1), void fraction (0≤α≤6.9 %), pulsation of the AC magnetic field (1.5×103≤ω≤12.5×103 rad s−1), and of two different void geometries. The results are analyzed on the basis of a first order expansion of magnetic flux in U and α. Despite the strong coupling between Faraday induction and Lorentz force effects, the results show that the contributions of U and α on a magnetic flux distortion can be well separated at both low magnetic Reynolds number and α values. These results are independent of void geometry

Imaging dielectric relaxation in nanostructured polymers by frequency modulation electrostatic force microscopy

We have developed a method for imaging the temperature-frequency dependence of the dynamics of nanostructured polymer films with spatial resolution. This method provides images with dielectric compositional contrast well decoupled from topography. Using frequency-modulation electrostatic-force-microscopy, we probe the local frequency-dependent (0.1–100 Hz) dielectric response through measurement of the amplitude and phase of the force gradient in response to an oscillating applied electric field. When the phase is imaged at fixed frequency, it reveals the spatial variation in dielectric losses, i.e., the spatial variation in molecular/dipolar dynamics, with 40 nm lateral resolution. This is demonstrated by using as a model system; a phase separated polystyrene/polyvinyl-acetate (PVAc) blend. We show that nanoscale dynamic domains of PVAc are clearly identifiable in phase images as those which light-up in a band of temperature, reflecting the variations in the molecular/dipolar dynamics approaching the glass transition temperature of PVAc

Measuring dielectric properties at the nanoscale using Electrostatic Force Microscopy

Several electrostatic force microscopy (EFM) - based methods have been recently developed to study the nanoscale dielectric properties of thin insulating layers. Some methods allow measuring quantitatively the static dielectric permittivity whereas some others provide qualitative information about the temperature-frequency dependence of dielectric properties. In this chapter, all these methods are described and illustrated by experiments on pure and nanostructured polymer films. A section is dedicated to EFM probe - sample models and especially to the Equivalent Charge Method (ECM)

Dielectric properties of thin insulating layers measured by Electrostatic Force Microscopy

In order to measure the dielectric permittivity of thin insulting layers, we developed a method based on electrostatic force microscopy (EFM) experiments coupled with numerical simulations. This method allows to characterize the dielectric properties of materials without any restrictions of film thickness, tip radius and tip-sample distance. The EFM experiments consist in the detection of the electric force gradient by means of a double pass method. The numerical simulations, based on the equivalent charge method (ECM), model the electric force gradient between an EFM tip and a sample, and thus, determine from the EFM experiments the relative dielectric permittivity by an inverse approach. This method was validated on a thin SiO2 sample and was used to characterize the dielectric permittivity of ultrathin poly(vinyl acetate) and polystyrene films at two temperatures

Caractérisation nanomécanique des parois cellulaires du bois à différents stades de leur différenciation

L’explication de la réorientation des arbres repose sur la compréhension de la différenciation cellulaire lors de la croissance secondaire au niveau du cambium au cours de laquelle la paroi cellulaire va s’épaissir et se rigidifier occasionnant des précontraintes de croissance. Cette étude a pour objectif de mesurer les propriétés mécaniques de la paroi cellulaire par microscopie à force atomique

Mid-IR plasmonic compound with gallium oxide toplayer formed by GaSb oxidation in water

The oxidation of GaSb in aqueous environments has gained interest by the advent of plasmonic antimonide-based compound semiconductors for molecular sensing applications. This work focuses on quantifying the GaSb–water reaction kinetics by studying a model compound system consisting of a 50 nm thick GaSb layer on a 1000 nm thick highly Si-doped epitaxial grown InAsSb layer. Tracing of phonon modes by Raman spectroscopy over 14 h of reaction time shows that within 4 h, the 50 nm of GaSb, opaque for visible light, transforms to a transparent material. Energy-dispersive x-ray spectroscopy shows that the reaction leads to antimony depletion and oxygen incorporation. The final product is a gallium oxide. The good conductivity of the highly Si-doped InAsSb and the absence of conduction states through the oxide are demonstrated by tunneling atomic force microscopy. Measuring the reflectivity of the compound layer structure from 0.3 to 20 μm and fitting of the data by the transfer-matrix method allows us to determine a refractive index value of 1.6 ± 0.1 for the gallium oxide formed in water. The investigated model system demonstrates that corrosion, i.e. antimony depletion and oxygen incorporation, transforms the narrow band gap material GaSb into a gallium oxide transparent in the range from 0.3 to 20 μm