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<p>This research presents new calibration techniques for the characterization of atomic force microscopy cantilevers. Atomic force microscopy cantilevers are sensors that detect forces on the order of pico- to nanonewtons and displacements on the order of nano- to micrometers. Several calibration techniques exist with a variety of strengths and weaknesses. This research presents techniques that enable the noncontact calibration of the output sensor voltage-to-displacement sensitivity and the cantilever stiffness through the analysis of the unscaled thermal vibration of a cantilever in a liquid environment.</p><p>A noncontact stiffness calibration method is presented that identifies cantilever characteristics by fitting a dynamic model of the cantilever reaction to a thermal bath according to the fluctuation-dissipation theorem. The fitting algorithm incorporates an assumption of heavy fluid loading, which is present in liquid environments.</p><p>The use of the Lorentzian line function and a variable-slope noise model as an alternate approach to the thermal noise method was found to reduce the difference between calibrations preformed on the same cantilever in air and in water relative to existing techniques. This alternate approach was used in combination with the new stiffness calibration technique to determine the voltage-to-displacement sensitivity without requiring contact loading of the cantilever.</p><p>Additionally, computational techniques are presented in the investigation of alternate cantilever geometries, including V-shaped cantilevers and warped cantilevers. These techniques offer opportunities for future research to further reduce the uncertainty of atomic force microscopy calibration.</p> / Dissertation

The stochastic dynamics of an array of closely spaced micron scale cantilevers in a viscous fluid is considered. The stochastic cantilever dynamics are due to the constant buffeting of fluid particles by Brownian motion and the dynamics of adjacent cantilevers are correlated due to long range effects of fluid dynamics. The measurement sensitivity of an experimental setup is limited by the magnitude of inherent stochastic motion. However, the magnitude of this noise can be decreased using correlated measurements allowing for improved force resolution. A correlated scheme is proposed using two atomic force microscope cantilevers for the purpose of analyzing the dynamics of single molecules in real time, a regime that is difficult to observe using current technologies. Using a recently proposed thermodynamic approach the hydrodynamic coupling of an array of cantilevers is quantified for precise experimental conditions through deterministic numerical simulations. Results are presented for an array of two readily available micron-scale cantilevers yielding the possible force sensitivity and time resolution of correlated measurements. This measurement scheme is capable of achieving a force resolution that is more than three fold more sensitive than that of a single cantilever when the two cantilevers are separated by 200 nm, with a time scale on the order of tens of microseconds. / Master of Science

Single-walled carbon nanotubes (SWNTs) exhibit extraordinary properties: mechanical, thermal, optical and, possibly the most interesting, electrical. These all-carbon cylindrical structures can be metallic or semi-conducting depending on their precise structure. They have the potential to allow faster transistor switching speeds and smaller, more closely-packed interconnects in microelectronics. However, such applications are hindered by the difficulties of positioning the correct type of SWNT in a spatially precise location and orientation. In addition, greater understanding of the fundamental limits of SWNTs, such as the limit of current density, is needed for optimum operation in applications. The primary aim of this project was to increase the understanding of current density limitation by using in situ plasmonically enhanced Raman spectroscopy during electrical transport. The use of plasmonic metal nanostructures to enhance the Raman scattering should allow the acquisition of informative spectra from SWNTs away from their intrinsic resonance conditions. To achieve this aim, SWNTs must be integrated with plasmonic metal structures as well as electrical connections. This thesis presents two approaches for the integration of SWNTs with other nanometre-scaled features, in particular plasmonic nanoparticles. Fountain pen nanolithography uses a hollow nanopipette in place of the probe tip in an atomic force microscope (AFM), through which material can be delivered to a spatially precise position on a surface. Aqueous SWNT dispersion was delivered to chemically-functionalised silicon in this way, through pulled quartz pipettes with aperture diameters of 50 nm, 100 nm and 150 nm. The heights, widths and continuity of lines drawn on the surface by the nanopipette depended on the size, setpoint and lateral speed of the tip. A small bias voltage applied between the SWNT dispersion inside the pipette and the substrate allowed the deposition to be switched on or off depending on the polarity of the voltage, through the action of electroosmotic effects within the quartz capillary. The quality and density of the SWNT dispersion was found to be important for successful deposition to occur, since too low a concentration results in the lines deposited from the pipette being only surfactant but too high a concentration of bundles would quickly block the small tip of the pipette. Polarised Raman spectroscopy on SWNT deposited by fountain pen nanolithography showed that they had a high level of alignment parallel to the direction in which the pipette moved. Spherical gold nanoparticles with plasmonic properties suitable for enhancing Raman scattering were dropped onto samples containing individual SWNTs supported on a Si/SiO2 surface. Nanomanipulation with an atomic force microscope was used to push the gold nanoparticles onto the SWNTs. Raman spectra measured with and without the gold particles showed that the gold nanoparticles gave local enhancement factors of 24 for a single 150 nm nanoshell and 130 for a small cluster of 150 nm nanoshells. Polarised Raman studies on the cluster showed that the angle dependence deviated significantly from that expected of a bare SWNT. Electrical transport experiments with in situ plasmonically enhanced Raman spectroscopy may be performed on samples prepared from the methods described here. Such experiments would increase understanding of the electrical properties of SWNTs and how they relate to the vibrational and optical properties.

We examine the design of a high speed atomic force microscope using an optical pickup from a commercially available compact disc/digital versatile disc drive. An investigation of the commercial optical pickup is done with the goal of determining how it can be used for dimensional measurements on nanometer scale. An evaluation of noise sources, imaging capabilities, and functionality is performed.

Orientador: José Manoel Balthazar / Banca: Átila Madureira Bueno / Banca: Bento Rodrigues de pontes Junior / Resumo: Desde 1986, quando Binnig et al (1986) criaram o microscópio de força atômica (AFM), esse aparelho se tornou um dos mais importantes microscópios de varredura (SPM), sendo usado para análise de DNA, nanotubos, etc. (Rützel et al, 2006). O AFM tem como componente principal uma microviga, com uma ponteira em uma das extremidades, que vibra próximo de sua frequencia de ressonância para mandar sinais a um fotodetector que traduz esse sinal e gera as imagens da superfície da amostra. O modo de operação tapping é o mais usado, e o comportamento caótico é muito comum nesse modo de operação, por esse motivo, AFM se tornou um assunto muito importante no mundo científico. Nesse trabalho, a microviga é modelada com o uso das equações de Bernoulli, as interações entre ela e a amostra são modeladas usando o potencial de Lennard Jones. Simulações numéricas detectam movimento caótico no sistema, a necessidade de estabilizá-lo nos leva a usar os seguintes métodos: Método do Balanço Harmônico, sincronização de Sistemas Não Lineares, Método das Equações de Estado Dependentes de Riccati (SDRE), Método de Realimentação de Sinal Atrasado. Por fim, a aplicação dos métodos se mostra eficiente, com pequeno erro e fácil implementação / Abstract: Since 1986, when Binnig et al (1986) created the atomic force microscope (AFM), this unit became one of the most important scanning probe microscopes (SPM) being used for DNA analysis, nano tubes, etc. (Rutzel et al, 2006). The AFM has as a main component, a micro cantilever, with a tip at its free end, which vibrates near its resonance frequency to send signals to a photo detector that translates the signal and generates images of the sample surface. The tapping mod of operation is the most widely used and chaotic behavior is very common in this mode, therefore, AFM has become a very interesting subject in the scientific world. In this work, the micro cantilever is modeled using Bernoulli's equation and the interactions between the tip and the sample are modeled using the Lennard Jones potential. Numerical simulations detect chaotic motion in the system and the need to stabilize it leads us to use the following methods, Harmonic Balance Method; Synchronization of Nonlinear Systems; the State Dependent Riccati Equation control method (SDRE); the Method of Feedback Delay. Finally, the application of the methods proved to be effective, with small error and easy implementation / Mestre

Metrological data from sample surfaces can be obtained by using a variety of profilometry methods. Atomic Force Microscopy (AFM), which relies on contact inter-atomic forces to extract topographical images of a sample, is one such method that can be used on a wide range of surface types, with possible nanometer range resolution. However, AFM images are commonly distorted by convolution, which reduces metrological accuracy. This type of distortion is more significant when the sample surface contains high aspect ratio features such as lines, steps or sharp edges - structures commonly found in semiconductor devices and applications. Aiming at mitigating these distortions and recovering metrology soundness, we introduce a novel image deconvolution scheme based on the principle of stereo imaging. Multiple images of a sample, taken at different angles, allow for separation of convolution artifacts from true topographic data. As a result, perfect sample reconstruction and probe shape estimation can be achieved in certain cases. Additionally, shadow zones, which are areas of the sample that cannot be probed by the AFM, are greatly reduced. Most importantly, this technique does not require a priori probe characterization. It also reduces the need for slender or sharper probes, which, on one hand, induce less convolution distortion but, on the other hand, are more prone to wear and damage, thus decreasing overall system reliability. / Singapore-MIT Alliance (SMA)

In the past two decades depth-sensing indentation has becomea widely used technique to measure the mechanical properties ofmaterials. This technique is particularly suitable for thecharacterisation of materials at sub-micro or nano scale thoughthere is a tendency to extend its application to the micro ormacro scale. The load-penetration depth curve of depth-sensingindentation is a characteristic of a material and can be usedfor analysing various mechanical properties in addition tohardness. This thesis deals with the mechanicalcharacterisation of bulk materials, thin films and coatings,gradient materials, and composites using depth-sensingindentation. Finite element method has been resorted to as atool to understand the indentation behaviour of materials. The piling-up or sinking-in behaviour of materials plays animportant role in the accurate determination of materialsproperties using depth-sensing indentation. Finite elementsimulations show that the piling-up or sinking-in behaviour isdetermined by the material parameters, namelyE/σyratio and strain hardening exponent orexperimental parameterhe/hmaxratio, and the contact friction. Anempirical model has been proposed to relate the contact area ofindentation to theE/σyratio and thehe/hmaxratio and used to predict thepiling-up orsinking-in of materials. The existence of friction is found toenhance the sinking-in tendency of materials. A generalrelationship between the hardness and the indentationrepresentative stress valid for both soft and hard materialshas been obtained. A possible method to estimate the plasticproperties of bulk materials has been suggested. Measuring the coating-only properties requires theindentation to be done within a critical penetration depthbeyond which substrate effect comes in. The ratio of thecritical penetration depth to the coating thickness determinedby nanoindentation is independent of coating thickness andabout 0.2 for gold / nickel, 0.4 for aluminium / BK7 glass, and0.2 for diamond-like-carbon / M2 steel and alumina / nickel.Finite element simulations show that this ratio is dependent onthe combination of the coating and the substrate and moresensitive to differences in the elastic properties than in theplastic properties of the coating/substrate system. Thedeformation behaviour of coatings, such as, piling-up of thesoft coatings and cracking of the hard coatings, has also beeninvestigated using atomic force microscope. The constraint factors, 2.24 for WC phase and 2.7 for WC-Cocemented carbides, are determined through nanoindentation andfinite element simulations. A modified hardness model of WC-Cocemented carbides has been proposed, which gives a betterestimation than the Lee and Gurland hardness model. Finiteelement method has also been used to investigate theindentation behaviour of WC-Co gradient coatings. Keywords:depth-sensing indentation, nanoindentation,finite element method, atomic force microscope, mechanicalproperties, hardness, deformation, dislocations, cracks,piling-up, sinking-in, indentation size effect, thin coatings,composite, gradient materials, WC-Co, diamond-like-carbon,alumina, gold, aluminium, nickel, BK7 glass, M2 steel.

The fabrication characteristic of etching and deposition of focused ion beam (FIB) on the submicron structure of silica and quartz glass was investigated. FIB has several advantages such as high sensitivity, high material removal rate, and direct fabrication in some selected areas without the use of etching mask, etc. In this study, silicon and quartz glass materials etched by FIB were used for fast fabrication of 3-D submicron structures to investigate the differences between the samples before and after fabrication. The expansion effect of silicon with sputtered platinum on surface is compared with Pyrex glass with sputtered chromium on surface. The result shows the side wall of structure in the center wouldn¡¦t be vertical after etching and trimming on the quartz glass and the silicon substrate. Trenches with different depth and width on the surface of silicon were etched by FIB and measured by Atomic Force Microscope. Lines with different interval were deposited by FIB on the surface of quartz glass and were measured by Atomic Force Microscope.

<p>Nucleic acids are subjected to many different mechanical loadings inside. These loadings could cause large deformations and conformational changes to these molecules. This is why the mechanical properties of nucleic acids are so important to their functions. Here we use a newly designed and built high-performance AFM force spectrometer, supplemented with molecular dynamics simulations and NMR spectroscopy to investigate the relationship between mechanical properties and structure of different nucleic acids.</p><p>To test the mechanical properties of nucleic acids, we successfully designed and purpose-built a single molecule puller, an instrument to physically stretch single molecules, at a fraction of the cost of a commercial AFM instrument. This instrument has similar force noise to hybrid instruments, while also exhibiting significantly lower drift, on the order of five times lower. This instrument allows the measurement of subtle transitions as a molecule is stretched. With the addition of a lock-in amplifier, we possibly could obtain better force resolution, the order of femtonewtons. </p><p>We find that helical structure does indeed have an effect on the mechanical properties of double-stranded DNA. As the A-form double helix has a shorter, wider structure compared to the B-form helix, its force spectra exhibit a shorter initial length before the overstretching force plateau, compared to B-form DNA. Contrarily, the Z-form double helix has a narrower, more extended helical structure than B-form DNA, and we see this fact manifest in the force spectra of Z-DNA, which has a longer initial length before the overstretching force plateau. Also, interestingly, we find that neither A, nor Z-DNA force spectra display the second melting force plateau. Indicating this plateau is not necessarily cause by melting of strands apart, but rather a feature of B-DNA. </p><p>To better understand the forces that stabilized these different structures, specifically base stacking, we also mechanically characterize different single-stranded helical polynucleotides using AFM based force spectroscopy. We expand on previous studies by confirming that single helical polynucleotides undergo a force transition at a force of ~20 pN as they are uncoiled, and also demonstrating, that when stretched beyond this force transition, the molecules behave differently depending on base sequence and backbone sugar. Specifically, the force spectra of poly-adenylic acid possess a linear force region, which persists to ~300 pN, after the force plateau. We also observe that poly-deoxyadenylic acid is comparatively stiffer than other polynucleotides after undergoing two force transitions. By supplementing our force spectroscopic data with MD simulations and NMR spectroscopy, we find that base stacking in adenine is quite strong, persisting above 100 pN. We find that initial helical structure, which is defined by base stacking and backbone sugar, guides the stretching pathway of the polynucleotides. This finding can possibly be extrapolated to the elasticity of double-stranded DNA.</p> / Dissertation