Tewfik Souier

A method to provide rapid in situ determination of tip radius in dynamic atomic force microscopy

We provide a method to characterize the tip radius of an atomic force microscopy in situ by monitoring the dynamics of the cantilever in ambient conditions. The key concept is that the value of free amplitude for which transitions from the attractive to repulsive force regimes are observed, strongly depends on the curvature of the tip. In practice, the smaller the value of free amplitude required to observe a transition, the sharper the tip. This general behavior is remarkably independent of the properties of the sample and cantilever characteristics and shows the strong dependence of the transitions on the tip radius. The main advantage of this method is rapid in situ characterization. Rapid in situ characterization enables one to continuously monitor the tip size during experiments. Further, we show how to reproducibly shape the tip from a given initial size to any chosen larger size. This approach combined with the in situ tip size monitoring enables quantitative comparison of materials measurements between samples. These methods are set to allow quantitative data acquisition and make direct data comparison readily available in the community.

Mechanical properties of BixSb2−xTe3 nanostructured thermoelectric material

Research on thermoelectric (TE) materials has been focused on their transport properties in order to maximize their overall performance. Mechanical properties, which are crucial for system reliability, are often overlooked. The recent development of a new class of high-performance, low-dimension thermoelectric materials calls for a better understanding of their mechanical behavior to achieve the desired system reliability. In the present study we investigate the mechanical behavior of nanostructure bulk TE material p-type Bi(x)Sb(2-x)Te(3) by means of nanoindentation and 3D finite element analysis. The Youngs modulus of the material was estimated by the Oliver-Pharr (OP) method and by means of numerically assisted nanoindentation analysis yielding comparable values about 40 GPa. Enhanced hardness and yield strength can be predicted for this nanostructured material. Microstructure is studied and correlation with mechanical properties is discussed.

Enhanced electrical properties of vertically aligned carbon nanotube-epoxy nanocomposites with high packing density

During their synthesis, multi-walled carbon nanotubes can be aligned and impregnated in a polymer matrix to form an electrically conductive and flexible nanocomposite with high backing density. The material exhibits the highest reported electrical conductivity of CNT-epoxy composites (350 S/m). Here, we show how conductive atomic force microscopy can be used to study the electrical transport mechanism in order to explain the enhanced electrical properties of the composite. The high spatial resolution and versatility of the technique allows us to further decouple the two main contributions to the electrical transport: (1) the intrinsic resistance of the tube and (2) the tunneling resistance due to nanoscale gaps occurring between the epoxy-coated tubes along the composite. The results show that the material behaves as a conductive polymer, and the electrical transport is governed by electron tunneling at interconnecting CNT-polymer junctions. We also point out the theoretical formulation of the nanoscale electrical transport between the AFM tip and the sample in order to derive both the composite conductivity and the CNT intrinsic properties. The enhanced electrical properties of the composite are attributed to high degree of alignment, the CNT purity, and the large tube diameter which lead to low junction resistance. By controlling the tube diameter and using other polymers, the nanocomposite electrical conductivity can be improved.

Dynamic electrostatic force microscopy technique for the study of electrical properties with improved spatial resolution

The need to resolve the electrical properties of confined structures (CNTs, quantum dots, nanorods, etc) is becoming increasingly important in the field of electronic and optoelectronic devices. Here we propose an approach based on amplitude modulated electrostatic force microscopy to obtain measurements at small tip-sample distances, where highly nonlinear forces are present. We discuss how this improves the lateral resolution of the technique and allows probing of the electrical and surface properties. The complete force field at different tip biases is employed to derive the local work function difference. Then, by appropriately biasing the tip-sample system, short-range forces are reconstructed. The short-range component is then separated from the generic tip-sample force in order to recover the pure electrostatic contribution. This data can be employed to derive the tip-sample capacitance curve and the sample dielectric constant. After presenting a theoretical model that justifies the need for probing the electrical properties of the sample in the vicinity of the surface, the methodology is presented in detail and verified experimentally.

Characterization of multi-walled carbon nanotube–polymer nanocomposites by scanning spreading resistance microscopy

Nanocomposites of aligned multi-walled carbon nanotubes (CNTs) embedded in a polymer matrix yield a unique combination of thermal and electrical properties and mechanical strength. These properties are intimately related to the composite nanostructure and to the growth and processing conditions. The alignment of the tubes, the filling fraction and the contact junction between the nanotubes are key parameters controlling the composite electrical conductivity. For this purpose, a full description of the composite nanostructure is required. Among the non-destructive scanning probe techniques, scanning spreading resistance microscopy is found to be a powerful technique in identifying the carbon nanotubes with true nanometer resolution, thus competing with SEM and TEM imaging. Additionally, the technique provides valuable information about the electrical conduction mechanism within the composite structure. Indeed, by using a controlled contact force and an appropriate model of conduction at the nanoscale, the tip-CNT contact resistance, the CNT intrinsic resistance and the CNT-epoxy-CNT resistance junction are evaluated. This latter is found to be the factor controlling the overall electrical conductivity of the composite.

Disentangling viscosity and hysteretic dissipative components in dynamic nanoscale interactions

The mechanisms through which energy is dissipated in nanoscale dynamic interactions might involve tens or hundreds of atoms and might be diverse. Here, a method is presented that provides the means to disentangle, with the use of common experimental parameters, short and long range viscosity and hysteretic dissipative components. While the approach is general, the experimental study is directed to show the mechanisms of energy dissipation between a silicon atomic force microscope tip and a carbon nanotube and a quartz surface. By stabilizing the tip in situ, quantitative information is found in a reproducible manner where the magnitude of energy dissipated remains constant in experiments thus allowing comparative studies.

Investigation of nanoscale interactions by means of subharmonic excitation

Multifrequency atomic force microscopy holds promise as a method to provide qualitative and quantitative information about samples with high spatial resolution. Here, we provide experimental evidence of the excitation of subharmonics in ambient conditions in the regions where capillary interactions are predicted to be the mechanism of excitation. We also experimentally decouple a second mechanism for subharmonic excitation that is highly independent of environmental conditions such as relative humidity. This implies that material properties could be mapped. Subharmonic excitation could lead to experimental determination of surface water affinity in the nanoscale whenever water interactions are the mechanism of excitation.

Investigating the effect of suspensions nanostructure on the thermophysical properties of nanofluids

The effect of fractal dimensions and Feret diameter of aggregated nanoparticle on predicting the thermophysical properties of nanofluids is demonstrated. The fractal dimensions and Feret diameter distributions of particle agglomerates are quantified from scanning electron and probe microscope imaging of yttria nanofluids. The results are compared with the fractal dimensions calculated by fitting the rheological properties of yttria nanofluids against the modified Krieger-Dougherty model. Nanofluids of less than 1 vol. % particle loading are found to have fractal dimensions of below 1.8, which is typical for diffusion controlled cluster formation. By contrast, an increase in the particle loading increases the fractal dimension to 2.0–2.2. The fractal dimensions obtained from both methods are employed to predict the thermal conductivity of the nanofluids using the modified Maxwell-Garnet (M-G) model. The prediction from rheology is found inadequate and might lead up to 8% error in thermal conductivity for a...

Electrical characteristics of graphene wrinkles extracted by conductive Atomic Force Microscopy and electrical measurements on kelvin structures

One of the key deliverables of using graphene as a channel in transistors is to achieve low source and drain parasitic contact resistance. Careful characterization of the surface of graphene is needed in order to improve understanding of the metal to graphene interface. In this paper, we employ conductive Atomic Force Microscope (C-AFM) to characterize the electrical properties of these wrinkles as a function of the applied force. At low forces, the wrinkles are more conductive than flat regions and at high forces the wrinkles have similar conductance as the flat regions. Graphene devices were fabricated and the total resistance of graphene in these devices was measured to be in the range 2Ω to 10MΩ. Additional research is planned to investigate if the wrinkles impact the electrical contact resistance of large area structures.

Identification and quantification of the dissipative mechanisms involved in the radial permanent deformation of carbon nanotubes

Recent advances in atomic force microscopy (AFM) are used here to determine, decouple and quantify the dissipative processes involved in the interaction between a silicon tip and a carbon nanotube (CNT). The energy dissipated per atom due to hysteretic contact processes on the CNT remains constant with increasing cantilever stored energy. The energy dissipated due to viscoelasticity, however, increases in the order of several eV?nm?2 per nm of free amplitude until the CNT eventually laterally deforms. This trend is general in amplitude modulation AFM and could be used to determine the nature and effects of dissipation for other relevant nanostructures.