T. Mélin

Surface potential of n- and p-type GaN measured by Kelvin force microscopy

n- and p-type GaN epitaxial layers grown by metal-organic chemical vapor deposition with different doping levels have been characterized by Kelvin probe force microscopy (KFM). To investigate the surface states of GaN beyond instrumental and environmental fluctuations, a KFM calibration procedure using a gold-plated Ohmic contact as a reference has been introduced, and the reproducibility of the KFM measurements has been evaluated. Results show that the Fermi level is pinned for n- and p-type GaN over the available doping ranges, and found 1.34±0.15eV below the conduction band and 1.59±0.18eV above the valence band, respectively.

Charge injection in individual silicon nanoparticles deposited on a conductive substrate

We report on charge injection in individual silicon nanoparticles deposited on conductive substrates. Charges are injected using a metal-plated atomic force microscope tip, and detected by electric force microscopy (EFM). Due to the screening efficiency of the conductive substrate, up to ∼200 positive or negative charges can be stored at moderate (<10 V) tip–substrate injection voltage in ∼40 nm high nanoparticles, with discharging time constants of a few minutes. We propose an analytical model in the plane-capacitor approximation to estimate the nanoparticle charge from EFM data. It falls in quantitative agreement with numerical calculations using realistic tip/nanoparticle/substrate geometries.

Charging and discharging processes of carbon nanotubes probed by electrostatic force microscopy

Electrostatic properties of individually separated single-walled carbon nanotubes (SWCNTs), double-walled carbon nanotubes (DWCNTs), and multiwalled carbon nanotubes (MWCNTs) deposited on insulating layers have been investigated by charge injection and electric force microscopy (EFM) experiments. Delocalized charge patterns are observed along the CNTs upon local injection from the EFM tip, corresponding to (i) charge storage in the nanotubes and to (ii) charge trapping in the oxide layer along the nanotubes. The two effects are dissociated easily for CNTs showing abrupt discharge processes in which the charge stored in the CNT are field emitted back to the EFM tip, while trapped oxide charge can subsequently be imaged by EFM, clearly revealing field-enhancement patterns at the CNT caps. The case of continuous discharge processes of SWCNTs, DWCNTs, and MWCNTs is discussed, as well as the evolution of the discharge time constants with respect to the nanotube diameter.

Numerical simulations for a quantitative analysis of AFM electrostatic nanopatterning on PMMA by Kelvin force microscopy

Electrostatic nanopatterning of electret thin films by atomic force microscopy (AFM) has emerged as an alternative efficient tool for the directed assembly of nano-objects on surfaces. High-resolution charge imaging of such charge patterns can be performed by AFM-based Kelvin force microscopy (KFM). Nevertheless, quantitative analysis of KFM surface potential mappings is not trivial because of side-capacitance effects induced by the tip cone and the cantilever of the scanning probe. In this paper, we developed numerical simulations of KFM measurements taking into account these artifacts, so as to estimate the actual surface charge density of square charge patterns (nominal sizes ranging from 100 nm to 10 microm) written by AFM into polymethylmethacrylate (PMMA) thin films. This work revealed that, under our conditions, such charge patterns exhibit a surface charge density between 1.5 x 10(-3) and 3.8 x 10(-3) C m(-2), depending on the assumed depth of injected charges. These results are crucial to quantify the actual electric field generated by such charge patterns and thus the electrostatic forces responsible for the directed assembly of nano-objects onto these electrostatic traps.

High-Resolution Kelvin Probe Force Microscopy Imaging of Interface Dipoles and Photogenerated Charges in Organic Donor–Acceptor Photovoltaic Blends

We present noncontact atomic force microscopy and Kelvin probe force microscopy studies of nanophase segregated photovoltaic blends based on an oligothiophene-fluorenone oligomer and [6,6]-phenyl C70 butyric acid methyl ester. We carried out a complete analysis of the influence of the tip-surface interaction regime on the topographic, in-dark contact potential and surface photovoltage contrasts. It is demonstrated that an optimal lateral resolution is achieved for all channels below the onset of a contrast in the damping images. With the support of electrostatic simulations, it is shown that in-dark contact potential difference contrasts above subsurface acceptor clusters are consistent with an uneven distribution of permanent charges at the donor-acceptor interfaces. A remarkable dependence of the surface photovoltage magnitude with respect to the tip-surface distance is evidenced and attributed to a local enhancement of the electromagnetic field at the tip apex.

Note: Quantitative (artifact-free) surface potential measurements using Kelvin force microscopy

The measurement of local surface potentials by Kelvin force microscopy (KFM) can be sensitive to external perturbations which lead to artifacts such as strong dependences of experimental results (typically in a ∼1 V range) with KFM internal parameters (cantilever excitation frequency and/or the projection phase of the KFM feedback-loop). We analyze and demonstrate a correction of such effects on a KFM implementation in ambient air. Artifact-free KFM measurements, i.e., truly quantitative surface potential measurements, are obtained with a ∼30 mV accuracy.

Kelvin force microscopy at the second cantilever resonance: An out-of-vacuum crosstalk compensation setup

We investigate the gap-voltage control loop in a Kelvin force microscopy setup with simultaneous non-contact topography imaging. The Kelvin controller electrostatically excites the second resonance of the cantilever at about 6.3 times the first resonance frequency and adjusts the DC component of the gap voltage to cancel the oscillation amplitude at this frequency, while the non-contact topography imaging is based on a frequency control loop that maintains a constant frequency of the mechanically excited first resonance of the cantilever by adjusting the tip-sample separation. Due to the self-excitation of the first resonance in our setup, it has to be considered that the electrostatic excitation at the second resonance frequency is applied to a closed feedback loop and cannot be considered as a simple superposition to the oscillation at the first resonance frequency. In particular, special care has to be taken about internal capacitive crosstalk between the tip bias and the cantilever deflection output signal. It is shown that such a coupling cannot be corrected by subtraction of a constant offset at the demodulator output since the crosstalk is sent into the self-excitation loop and is multiplied by the closed loop transfer function. We present a circuit that actively compensates, outside the vacuum environment, the internal crosstalk by adding to the deflection output a dephased fraction of the electrostatic excitation signal.

Cross-talk artefacts in Kelvin probe force microscopy imaging: A comprehensive study

We provide in this article a comprehensive study of the role of ac cross-talk effects in Kelvin Probe Force Microscopy (KPFM), and their consequences onto KPFM imaging. The dependence of KPFM signals upon internal parameters such as the cantilever excitation frequency and the projection angle of the KPFM feedback loop is reviewed, and compared with an analytical model. We show that ac cross-talks affect the measured KPFM signals as a function of the tip-substrate distance, and thus hamper the measurement of three-dimensional KPFM signals. The influence of ac cross-talks is also demonstrated onto KPFM images, in the form of topography footprints onto KPFM images, especially in the constant distance (lift) imaging mode. Our analysis is applied to unambiguously probe charging effects in tobacco mosaic viruses (TMVs) in ambient air. TMVs are demonstrated to be electrically neutral when deposited on silicon dioxide surfaces, but inhomogeneously negatively charged when deposited on a gold surface.

Calculating Kelvin force microscopy signals from static force fields

We present an analytical formula to achieve numerical simulations of Kelvin force microscopy (KFM) signals from static force fields, which can be employed to describe amplitude-modulation or frequency-modulation KFM, as well as simultaneous topography and KFM modes for which the tip probe exhibits a nonzero oscillation during KFM imaging. This model is shown to account for side-capacitance and nonlinear effects taking place in KFM experiments, and can therefore be used conveniently to extract quantitative information from KFM experiments at the nanoscale.

Charging and emission effects of multiwalled carbon nanotubes probed by electric force microscopy

Electrostatic properties of single-separated multiwalled carbon nanotubes (MWCNTs) deposited on a dielectric layer have been investigated by charge injection and electric force microscopy (EFM) experiments. We found that upon local injection from the biased EFM tip, charges delocalize over the whole nanotube length (i.e., 1–10μm), consistent with a capacitive charging of the MWCNT-substrate capacitance. In addition, the insulating layer supporting the nanotubes is shown to act as a charge-sensitive plate for electrons emitted from the MWCNTs at low electric fields, thus allowing the spatial mapping of MWCNT field-emission patterns.