Failure analysis and optimization of semiconducting devices request knowledge of their electrical properties. To meet the demands of today’s semiconductor industry, an electrical nanometrology technique is required which provides quantitative information about the doping profile and which enables scans with a lateral resolution in the sub-10 nm range. In the presented work it is shown that Kelvin probe force microscopy (KPFM) is a very promising electrical nanometrology technique to face this challenge. The technical and physical aspects of KPFM measurements on semiconductors required for the correct interpretation of the detected KPFM bias are discussed. A new KPFM model is developed which enables the quantitative correlation between the probed KPFM bias and the dopant concentration in the investigated semiconducting sample. Quantitative dopant profiling by means of the new KPFM model is demonstrated by the example of differently structured, n- and p-type doped silicon. Additionally, the transport of charge carriers during KPFM measurements, in particular in the presence of intrinsic electric fields due to vertical and horizontal pn junctions as well as due to surface space charge regions, is discussed. Detailed investigations show that transport of charge carriers in the semiconducting sample is a crucial aspect and has to be taken into account when aiming for a quantitative evaluation of the probed KPFM bias.

This thesis addresses the fabrication, evaluation, and analysis of the probe tip of a non-vibrating contact potential difference sensor. The non-vibrating contact potential difference (nvCPD) probe measures the work function variation on a conducting surface and recent experiments performed to measure the size of surface features have shown poor correlation between actual and calculated probe tip dimensions. In order to address this deficiency, experiments were done and an analytical model was developed, including fringe electrical fields, that predicts the shape of the nvCPD probe signal as a function of probe tip geometry, work function variation, and experimental parameters. Probe tips were constructed with varying geometric properties and experiments using these probe tips were compared to a model. There was good correlation of the nvCPD probe output for a known work function change and probe tip geometry. The effective area of the probe tip resulting from electrical field fringing is expected to increase with dielectric thickness to a finite value, based on pre-existing electrostatic models for a shielded parallel plate capacitor. The minimum fringe field obtained in these experiments was for a 3.18mm diameter probe tip with a dielectric thickness of 0.20mm. The fringe field diameter was 3.38mm at a fly height of 0.60mm, representing an effective probe tip area increase of 13%.

This work describes two closed-loop atomic force microscopy methods that utilize the heated silicon probe to interrogate surfaces. The first method identifies the softening temperatures of a selected polymer and organic substrate as a function of contact force and surface hardness. Motivation partly stems from nanosampling, which requires knowledge of phase-specific transitions to identify and extract mass from multicomponent systems for chemical analysis. In the second method, the cantilever is implemented as a Kelvin probe to study the effect of temperature on the measured contact potential. The objective is to ascertain whether the probe functions as a capable electrode for scanning Kelvin probe microscopy (SKPM) applications. This was achieved by performing heated force-distance experiments on a biased gold film with the tip operating at various potentials. Both experiments examine the interaction between the tip and substrate and analyze sample effects both induced and sensed by the cantilever.

No description available.

La nanostructure et les propriétés électroniques de matériaux modèles pour le photovoltaïque organique, ont été étudiées en utilisant la Microscopie à Force Atomique en mode non contact sous ultra-vide (NC-AFM) et la Microscopie à sonde de Kelvin (KPFM). En utilisant le mode modulation d'amplitude (AM-KPFM), le potentiel de surface photo- généré dans des mélanges donneur-accepteur présentant une ségrégation de phase optimale a pu être visualisé à l'échelle du nanomètre. Afin de préciser la nature des forces mises en jeu dans le processus d'imagerie KPFM, des oligomères π-conjugués auto-assemblés ont ensuite été étudiés. Une transition entre régimes à longue et à courte portée a ainsi été mise en évidence en combinant l'imagerie en haute résolution aux mesures de spectroscopie en distance. Ces mesures ont également démontré que l'influence des forces électrostatiques à courte portée peut être minimisée en travaillant au seuil du contraste de dissipation. Enfin cette procédure a été utilisée, en combinaison avec les mesures de spectroscopie de photoélectrons UV, pour analyser la fonction de sortie locale d'électrodes transparentes à base de nanotubes de carbone fonctionnalisés. / In this thesis, noncontact atomic force microscopy (NC-AFM) and Kelvin probe force microscopy (KPFM) under ultrahigh vacuum have been applied to investigate the nanostructure and electronic surface properties of model materials for organic photovoltaics. First, it has been demonstrated that the surface photovoltage of nanoscale phase segregated donor-acceptor photovoltaic blends can be finely resolved at the nanometer scale by using amplitude modulation KPFM (AM-KPFM). Next, model self-assembled π-conjugated oligomers have been investigated, in order to obtain a deeper insight into the nature of the tip-surface forces involved in the KPFM imaging process. A crossover between long-range (LR) and short-range (SR) regimes has been evidenced by combining high resolution imaging with distance-spectroscopy measurements. It has also been shown that the influence of the SR electrostatic forces can be minimized by working at the onset of the damping contrast. Finally, using this procedure, the local work function of flexible transparent electrodes, comprised of functionalized carbon nanotubes by metallic nanoparticles, has been investigated, and compared to the averaged value deduced from ultraviolet photoelectron spectroscopy.

Two graphene layers placed in close proximity offer a unique system to investigate interacting electron physics as well as to test novel electronic device concepts. In this system, the interlayer spacing can be reduced to value much smaller than that achievable in semiconductor heterostructures, and the zero energy band-gap allows the realization of coupled hole-hole, electron-hole, and electron-electron two-dimensional systems in the same sample. Leveraging the fabrication technique and electron transport study in dual-gated graphene field-effect transistors, we realize independently contacted graphene double layers separated by an ultra-thin dielectric. We probe the resistance and density of each layer, and quantitatively explain their dependence on the backgate and interlayer bias. We experimentally measure the Coulomb drag between the two graphene layers for the first time, by flowing current in one layer and measuring the voltage drop in the opposite layer. The drag resistivity gauges the momentum transfer between the two layers, which, in turn, probes the interlayer electron-electron scattering rate. The temperature dependence of the Coulomb drag above temperatures of 50 K reveals that the ground state in each layer is a Fermi liquid. Below 50 K we observe mesoscopic fluctuations of the drag resistivity, as a result of the interplay between coherent intralayer transport and interlayer interaction. In addition, we develop a technique to directly measure the Fermi energy in an electron system as a function of carrier density using double layer structure. We demonstrate this method in the double layer graphene structure and probe the Fermi energy in graphene both at zero and in high magnetic fields. Last, we realize dual-gated bilayer graphene devices, where we investigate quantum Hall effects at zero energy as a function of transverse electric field and perpendicular magnetic field. Here we observe a development of v = 0 quantum Hall state at large electric fields and in high magnetic fields, which is explained by broken spin and valley spin symmetry in the zero energy Landau levels. / text

Dans un contexte normatif toujours plus sévère concernant les rejets automobiles polluants, la substitution des aciers par des alliages d’aluminium dans les structures des véhicules est en plein essor. Ce projet de thèse, qui s’inscrit dans un programme de développement de la société Constellium, cible plus précisément les alliages d’aluminium de la série 7xxx (Al-Zn-Mg) qui, malgré leurs propriétés mécaniques élevées, peuvent présenter une sensibilité à la corrosion sous contrainte (CSC) liée au phénomène de fragilisation par l’hydrogène (FPH). La compréhension des mécanismes mis en jeu dans ce type d’endommagement constitue donc une première étape vers une optimisation métallurgique en vue d’une industrialisation future de ces alliages dans le secteur automobile. La première partie de ces travaux est consacrée à l’étude de l’influence de l’état métallurgique de l’alliage 7046 sur son comportement en CSC et à l’identification des mécanismes de dégradation. Un lien direct a pu être mis en évidence entre l’abattement des propriétés mécaniques et les modes de rupture actifs et la quantité d’hydrogène dans l’alliage. Les deux modes d’endommagement observés, intergranulaire-fragile et transgranulaire-fragile, ont respectivement été attribués à un enrichissement en hydrogène aux joints de grains et au piégeage de l’hydrogène au niveau des précipités intragranulaires. Les interactions entre l’hydrogène et les précipités fins d’une part et les dislocations d’autre part, identifiés comme deux hétérogénéités microstructurales critiques vis-à-vis de la FPH, ont été étudiées à une échelle plus locale dans la seconde partie du travail de thèse. Les essais ont été réalisés sur des échantillons modèles, chargés en hydrogène en milieu H2SO4 sous polarisation cathodique et la profondeur de pénétration de l’hydrogène a été évaluée par SKPFM (Scanning Kelvin Probe Force Microscopy). L’ensemble des résultats obtenus met en évidence : 1/ un effet « barrière » des précipités fins et des dislocations sur la diffusion de l’hydrogène en relation avec un abattement des propriétés mécaniques moins important, 2/ un transport possible de l’hydrogène par les dislocations et 3/ l’efficacité du SKPFM pour déterminer précisément des coefficients de diffusion apparents de l’hydrogène. Ces résultats ouvrent ainsi de nouvelles pistes vers la compréhension des mécanismes de CSC dans les alliages Al-Zn-Mg.

This thesis deals with the use of Atomic Force Microscopy (AFM) and Kelvin Probe Force Microscopy (KPFM) in solar cells production. Both techniques measure surface properties using interactions between surface and tip that progressively scans entire surface of the sample. Atomic force microscopy allows three dimensional imaging of surface structure. Kelvin probe force microscopy is used to measure the contact potential difference on the sample surface. There are described experimental measurements of monocrystalline and multicrystalline substrates after various etching processes using AFM. By using KPFM the contact potential difference was measured on dielectric layers PSG, SiOX, SiNX and Al2O3 and on selective emitter structures. All experiments described in this work were carried out at the Solartec Ltd. workplace and they completely correspond with the actual technology of crystalline solar cells production.

Failure analysis and optimization of semiconducting devices request knowledge of their electrical properties. To meet the demands of today’s semiconductor industry, an electrical nanometrology technique is required which provides quantitative information about the doping profile and which enables scans with a lateral resolution in the sub-10 nm range. In the presented work it is shown that Kelvin probe force microscopy (KPFM) is a very promising electrical nanometrology technique to face this challenge. The technical and physical aspects of KPFM measurements on semiconductors required for the correct interpretation of the detected KPFM bias are discussed. A new KPFM model is developed which enables the quantitative correlation between the probed KPFM bias and the dopant concentration in the investigated semiconducting sample. Quantitative dopant profiling by means of the new KPFM model is demonstrated by the example of differently structured, n- and p-type doped silicon. Additionally, the transport of charge carriers during KPFM measurements, in particular in the presence of intrinsic electric fields due to vertical and horizontal pn junctions as well as due to surface space charge regions, is discussed. Detailed investigations show that transport of charge carriers in the semiconducting sample is a crucial aspect and has to be taken into account when aiming for a quantitative evaluation of the probed KPFM bias.

No description available.