Scanning probe microscopes (SPMs) are the highest resolution imaging instruments available today and are among the most important tools in nanoscience. Conventional SPMs suffer from several drawbacks owing to their large and bulky construction and to the use of piezoelectric materials. Large scanners have low resonant frequencies that limit their achievable imaging bandwidth and render them susceptible to disturbance from ambient vibrations. Array approaches have been used to alleviate the bandwidth bottleneck; however as arrays are scaled upwards, the scanning speed must decline to accommodate larger payloads. In addition, the long mechanical path from the tip to the sample contributes thermal drift. Furthermore, intrinsic properties of piezoelectric materials result in creep and hysteresis, which contribute to image distortion. The tip-sample interaction signals are often measured with optical configurations that require large free-space paths, are cumbersome to align, and add to the high cost of state-of-the-art SPM systems. These shortcomings have stifled the widespread adoption of SPMs by the nanometrology community. Tiny, inexpensive, fast, stable and independent SPMs that do not incur bandwidth penalties upon array scaling would therefore be most welcome. The present research demonstrates, for the first time, that all of the mechanical and electrical components that are required for the SPM to capture an image can be scaled and integrated onto a single CMOS chip. Principles of microsystem design are applied to produce single-chip instruments that acquire images of underlying samples on their own, without the need for off-chip scanners or sensors. Furthermore, it is shown that the instruments enjoy a multitude of performance benefits that stem from CMOS-MEMS integration and volumetric scaling of scanners by a factor of 1 million. This dissertation details the design, fabrication and imaging results of the first single-chip contact-mode AFMs, with integrated piezoresistive strain sensing cantilevers and scanning in three degrees-of-freedom (DOFs). Static AFMs and quasi-static AFMs are both reported. This work also includes the development, fabrication and imaging results of the first single-chip dynamic AFMs, with integrated flexural resonant cantilevers and 3 DOF scanning. Single-chip Amplitude Modulation AFMs (AM-AFMs) and Frequency Modulation AFMs (FM-AFMs) are both shown to be capable of imaging samples without the need for any off-chip sensors or actuators. A method to increase the quality factor (Q-factor) of flexural resonators is introduced. The method relies on an internal energy pumping mechanism that is based on the interplay between electrical, mechanical, and thermal effects. To the best of the author???s knowledge, the devices that are designed to harness these effects possess the highest electromechanical Qs reported for flexural resonators operating in air; electrically measured Q is enhanced from ~50 to ~50,000 in one exemplary device. A physical explanation for the underlying mechanism is proposed. The design, fabrication, imaging, and tip-based lithographic patterning with the first single-chip Scanning Thermal Microscopes (SThMs) are also presented. In addition to 3 DOF scanning, these devices possess integrated, thermally isolated temperature sensors to detect heat transfer in the tip-sample region. Imaging is reported with thermocouple-based devices and patterning is reported with resistive heater/sensors. An ???isothermal electrothermal scanner??? is designed and fabricated, and a method to operate it is detailed. The mechanism, based on electrothermal actuation, maintains a constant temperature in a central location while positioning a payload over a range of >35??m, thereby suppressing the deleterious thermal crosstalk effects that have thus far plagued thermally actuated devices with integrated sensors. In the thesis, models are developed to guide the design of single-chip SPMs and to provide an interpretation of experimental results. The modelling efforts include lumped element model development for each component of single-chip SPMs in the electrical, thermal and mechanical domains. In addition, noise models are developed for various components of the instruments, including temperature-based position sensors, piezoresistive cantilevers, and digitally controlled positioning devices.

Electrical and structural properties of Bismuth thin films were studied simultaneously. Electrical properties of the Bismuth thin films have been characterized by measuring temperature dependent conductivity and Hall effect. Structural analysis were carried out by X-ray diffraction technique and using a room temperature Atomic Force Microscope (RT-AFM).

O clareamento dental é o meio disponível mais simples, comum e conservador para o cirurgião-dentista proporcionar aos pacientes o padrão de cor de seus dentes mais desejado. Em alguns casos, os dentes que vão ser clareados podem apresentar restaurações realizadas com compósitos dentais, que são mais suscetíveis a alterações químicas, quando comparados a outros materiais restauradores. Alguns estudos mostraram que diferentes concentrações de agentes clareadores levaram a um aumento significativo da rugosidade superficial e das porosidades em compósitos dentais. Este estudo avaliou o efeito de dois agentes clareadores (Whiteness HP Blue 20%, Whiteness HP Max) sobre a rugosidade superficial de dois compósitos dentais, um micro-híbrido (Esthet X, Denstply) e outro nanoparticulado (Z 350, 3M ESPE). Um total de oito corpos de prova (9 x 2 mm) foram confeccionados com auxílio de uma matriz de teflon, sendo divididos em 4 grupos (Esthet X + Whiteness HP Blue 20%; Esthet X + Whiteness HP Max; Z 350 + Whiteness HP Blue 20%; Z 350 + Whiteness HP Max), sendo n=2. Os corpos de prova foram armazenados em saliva artificial neutra e, após 24 horas, foram polidos com discos de óxido de Alumínio (Sof-lex, 3M ESPE). Após sete dias de imersão salivar, cada corpo de prova foi levado a um microscópio de força atômica para obtenção do valor inicial de rugosidade superficial (Ra em nm). Em seguida, sem remover o corpo de prova do microscópio, o agente clareador foi aplicado sobre a superfície do corpo de prova, segundo as instruções do fabricante, de modo que permitisse uma posterior observação da mesma área do corpo de prova observada inicialmente, para obtenção do valor final de rugosidade superficial. Imagens em duas e três dimensões foram obtidas de cada corpo de prova para observação de alterações da topografia. Os resultados foram tratados estatisticamente por ANOVA e pelo teste de contraste Student-Newman-Keuls (p < 0,05). Não houve alteração significativa na rugosidade superficial (Ra) dos corpos da prova de compósitos micro-híbrido e nanoparticulado, submetidos aos agentes clareadores Whiteness HP Blue 20% e Whiteness HP Maxx. No entanto, independente do agente clareador utilizado, foram observadas maiores alterações topográficas nas imagens de microscopia de força atômica da superfície do compósito micro-híbrido do que nas imagens do nanoparticulado. / Dental bleaching is the simplest, the most common and conservative available way for dentists to offer their patients the standard color of teeth more desired. In some cases, the teeth that will be bleached may include restorations made of resin composites, which are more prone to chemical alteration compared with other restoration materials. Some studies have showed that different concentrations of bleaching gels might lead to a significant increase in surface roughness and amount of porosities in composite resins. This study evaluated the effect of two bleaching gels (Whiteness HP Blue 20%, Whiteness HP Max) on surface roughness of two resin composites, micro-hybrid (Esthet X, Denstply) and nanoparticled (Z350, 3M ESPE). A total of eight specimens (9 x 2 mm) were produced with a Teflon mold help, and were divided into four groups (Esthet X + Whiteness HP Blue 20%; Esthet X + Whiteness HP Max; Z 350 + Whiteness HP Blue 20%; Z 350 + Whiteness HP Max), with n=2. They were stored in neutral artificial saliva and, after 24 hours, were polished with aluminium oxide discs (Sof-lex, 3M ESPE). After seven days of salivary immersion, each specimen was taken to an atomic force microscope for recording initial value of surface roughness (Ra in nm). After that procedure, without removing the specimen from microscope, the bleaching gel was applied on the surface of the specimen, following manufacturers instructions, in order to allow posterior observation of the same area of the specimen initially observed, for recording the final value of surface roughness. Two-dimensional and 3D images were taken from each specimen group for observation of surface alterations. The results were statistically analyzed by ANOVA and the SNK test (p< 0.05). There were no statistically significant differences in the surface roughness (Ra) for specimens of micro-hybrid and nanoparticled composites, submitted to the bleaching agents Whiteness HP Blue 20% and Whiteness HP Maxx. However, there were noticed larger surface alterations in atomic force microscope images on the surface of micro-hybrid composites than on the nanoparticled, independently of the bleaching agent used.

Cell motility under physiological and pathological conditions including malignant progression of cancer and subsequent metastasis are founded on environmental confinements. During the last two decades, three-dimensional cell migration has been studied mostly by utilizing biomimetic extracellular matrix models. In the majority of these studies, the in vitro collagen scaffolds are usually assumed to be homogenous, as they consist commonly of one specific type of collagen, such as collagen type I, isolated from one species. These collagen matrices should resemble in vivo extracellular matrix scaffolds physiologically, however, mechanical phenotype and functional reliability have been addressed poorly due to certain limitations based on the assumption of homogeneity. How local variations of extracellular matrix structure impact matrix mechanics and cell migration is largely unknown. Here, we hypothesize that local inhomogeneities alter cell movement due to alterations in matrix mechanics, as they frequently occur in in vivo tissue scaffolds and were even changed in diseased tissues. To analyze the effect of structural inhomogeneities on cell migration, we used a mixture of rat tail and bovine dermal collagen type I as well as pure rat and pure bovine collagens at four different concentrations to assess three-dimensional scaffold inhomogeneities. Collagen type I from rat self-assembled to elongated fibrils, whereas bovine collagen tended to build node-shaped inhomogeneous scaffolds. We have shown that the elastic modulus determined with atomic force microscopy in combination with pore size analysis using confocal laser scanning microscopy revealed distinct inhomogeneities within collagen matrices. We hypothesized that elastic modulus and pore size govern cancer cell invasion in three-dimensional collagen matrices. In fact, invasiveness of three breast cancer cell types is altered due to matrix-type and concentration indicating that these two factors are crucial for cellular invasiveness. Our findings revealed that local matrix scaffold inhomogeneity is another crucial parameter to explain differences in cell migration, which not solely depended on pore size and stiffness of the collagen matrices. With these three distinct biophysical parameters, characterizing structure and mechanics of the studied collagen matrices, we were able to explain differences in the invasion behavior of the studied cancer cell lines in dependence of the used collagen model.

Thesis (PhD (Electrical and Electronic Engineering))--University of Stellenbosch, 2010. / Dissertation presented for the degree of Doctor of Philosophy in Engineering at the University of Stellenbosch / ENGLISH ABSTRACT: Planar weak link structures, such as micro-bridges, variable thickness bridges and nanobridges, have always attracted a lot of attention. Their potential to behave as real Josephson elements make them useful devices, with numerous applications. Powerful techniques, such as focused ion-beam and electron-beam lithography, were successfully used and are well understood in planar weak link structure fabrication. In this dissertation the results of an experimental study on planar weak link structures are presented. For the first time these structures have been successfully fabricated using AFM nanolithography on hard high-temperature superconducting YBCO tracks, where diamond coated silicon tips were used as a ploughing tool. Superconducting YBCO thin films were deposited on different substrates, using inverted cylindrical magnetron sputtering. The films were used to fabricate micro-bridges, variable thickness bridges and nano-bridges, by using conventional photolithography, argon ion-beam milling and AFM nanolithography. The measured I-V characteristics of the fabricated micro-bridges (width down to 1.9 µm), variable thickness bridges (thickness down to 15 nm) and nano-bridge (width down to 490 nm) showed well defined DC and AC Josephson effect characteristics. For better understanding of the behaviour of these types of weak links, critical current versus temperature measurements, and magnetic field modulation of the critical current measurements, were also performed, with the results and discussions given inside the chapters. The major challenges that were experienced in the laboratory during the fabrication processes and the operation of the fabricated devices are also discussed, with the solutions given where appropriate. / AFRIKAANSE OPSOMMING: Swak-skakel vlakstrukture, soos mikrobr.ue, br.ue met veranderlike dikte en nanobr.ue, het nog altyd baie aandag getrek. Hul het die potensiaal om soos werklike Josephson-elemente te kan funksioneer en is, as gevolg hiervan, nuttige toestelle met veelvuldige toepassings. Kragtige tegnieke, soos gefokuste ioonstraal- en elektronstraal litografie, is suksesvol gebruik en word goed verstaan in die vervaardiging van swak-skakel vlakstrukture. In hierdie proefskrif word die resultate van ¡¦n eksperimentele studie van swak-skakel vlakstrukture voorgel.e. Vir die eerste keer is hierdie strukture suksesvol vervaardig, deur gebruik te maak AFMnanolitografie op harde, ho¡Le-temperatuur supergeleier YBCO (Yttrium Barium Koperoksied) spore, waar diamantbedekte silikonpunte gebruik is as ploeginstrument. ¡¦n Dun lagie van supergeleidende YBCO is op verskillende substrate gedeponeer, deur gebruik te maak van omgekeerde silindriese magnetron verstuiwing. Die dun lagies is gebruik in die vervaardiging van mikrobr.ue, br.ue met veranderlike dikte en nanobr.ue, deur die gebruik van gewone fotolitografie, argon-ioonstraal frees en AFM nanolitografie. Die gemete I-V eienskappe van die vervaardigde mikrobr.ue (met breedte so laag as 1.9 µm), veranderlike-dikte br.ue (dikte tot 15 nm) en nanobr.ue (breedte so min as 490 nm) toon goed gedefinieerde GS en WS eienskappe van die Josephson-effek. Ten einde die gedrag van hierdie tipes swak-skakels beter te kan verstaan, is metings gedoen van kritieke stroom teenoor temperatuur, asook magnetiese veld modulasie van die kritieke stroom. Hierdie resultate en besprekings daarvan word binne die toepaslike hoofstukke aangebied. Die grootste uitdagings wat in die laboratorium, sowel as met die toetsing van die vervaardigde toestelle ondervind is, word ook bespreek. Waar moontlik, word toepaslike oplossings voorgestel.

Die eingereichte Dissertation beschäftigt sich mit der messtechnischen Erfassung sowie der Modellierung von Haftkräften zwischen rauen Oberflächen. Dabei wurden durch Variation von Flüssigkeiten sowie dem Nutzen beschichteter Oberflächen verschiedene Benetzungseigenschaften eingestellt und untersucht. Zusätzlich wurden neben dem Kontaktwinkel der untersuchten Systeme die freien Ober- und Grenzflächenenergien bestimmt und mit den Kräften korreliert. Es zeigte sich, dass Haftkräfte auf rauen Oberflächen stets über mehrere Größenordnungen verteilt vorliegen. Die Beschreibung der ermittelten Verteilungen ist dabei entweder durch statistischer Funktionen oder zumindest teils auch durch eine im Rahmen der Arbeit entwickelten Modellierung möglich. Weiterhin zeigte sich, dass eine Unterteilung in verschiedene Haftmechanismen (durch Kapillarbrücken oder van der Waals- sowie polare Wechselwirkungen) vorgenommen werden kann. Kapillarbrücken bilden dabei die größten Kräfte aus. Sie entstehen auf Grund nanoskaliger Blasen (Nanobubbles), welche vor allem auf schlecht benetzenden Oberflächen existieren.

Doctor of Philosophy / Department of Physics / Bruce M. Law / Three diverse first author surfaces science experiments conducted by Sean P. McBride 1-3 will be discussed in detail and supplemented by secondary co-author projects by Sean P. McBride, 4-7 all of which rely heavily on the use of an atomic force microscope (AFM). First, the slip length parameter, b of liquids is investigated using colloidal probe AFM. The slip length describes how easily a fluid flows over an interface. The slip length, with its exact origin unknown and dependencies not overwhelming decided upon by the scientific community, remains a controversial topic. Colloidal probe AFM uses a spherical probe attached to a standard AFM imaging tip driven through a liquid. With the force on this colloidal AFM probe known, and using the simplest homologous series of test liquids, many of the suspected causes and dependencies of the slip length demonstrated in the literature can be suppressed or eliminated. This leaves the measurable trends in the slip length attributed only to the systematically varying physical properties of the different liquids. When conducting these experiments, it was realized that the spring constant, k, of the system depends upon the cantilever geometry of the experiment and therefore should be measured in-situ. This means that the k calibration needs to be performed in the same viscous liquid in which the slip experiments are performed. Current in-situ calibrations in viscous fluids are very limited, thus a new in-situ k calibration method was developed for use in viscous fluids. This new method is based upon the residuals, namely, the difference between experimental force-distance data and Vinogradova slip theory. Next, the AFM’s ability to acquire accurate sub nanometer height profiles of structures on interfaces was used to develop a novel experimental technique to measure the line tension parameter, τ, of isolated nanoparticles at the three phase interface in a solid-liquid-vapor system. The τ parameter is a result of excess energy caused by the imbalance of the complex intermolecular forces experienced at the three phase contact line. Many differences in the sign and magnitude of the τ parameter exist in the current literature, resulting in τ being a controversial topic.

O estudo das não linearidades das séries temporais da microviga de um microscópio de força atômica tem sido essencial para o desenvolvimento e aperfeiçoamento deste equipamento de ampliação de imagens. Não linearidades podem aparecer com frequência nos experimentos, afetando significativamente a resposta prevista de forma que estas instabilidades se concretizam em imagens ruins. Esta tese apresenta resultados obtidos através de uma abordagem experimental e teórica. Buscou-se aperfeiçoar modelos clássicos de osciladores do microscópio de força atômica melhorando seu comportamento caótico através da observação dos resultados dos experimentos. A identificação de sistemas é feita pelo método de espaço de estados. Outra abordagem de séries temporais obtidas através de um microscópio de força atômica torna possível a reconstrução de espaço de estados, utilizando-se de técnicas como informação mútua, falsos vizinhos e defasagem de tempo. Analisa-se também o comportamento caótico das séries temporais usando o teste 0-1 e escala indexada em quatro experimentos que resultam em um mapa que relaciona a altura que a microviga vibra com o coeficiente do teste 0-1 e com a escala indexada. / The study of time series nonlinearities of the cantilever\'s atomic force microscope has been essential to the development and improvement of this image magnification equipment. Nonlinearities may appear frequently in the experiments, significantly affecting expected response in a way that these instabilities generate bad images. This thesis presents results obtained through an experimental and theoretical approach accordingly. We attempted to improve the classical models of oscillators atomic force microscope improving its chaotic behavior by observing the results of the experiments. The system identification is made by method space state. Another approach to time series obtained through an atomic force microscope makes it possible to reconstruct space phase, using techniques such as mutual information and false neighbors delay. It is analyzed chaotic behavior time series by using the 0-1 test and scale index in four experiments resulting in a map that relates the height of cantilever deflections with the 0-1 test coefficient and the indexed scale.

O tratamento clareador pode resultar em alterações na rugosidade superficial do esmalte dental, as quais podem ser vistas a olho nu como alterações de cor, opacidade e perda de brilho. O objetivo deste estudo foi analisar in vitro a alteração de rugosidade, cor e brilho de superfícies de esmalte dental humano após clareamento com um produto a base de peróxido de hidrogênio (PH) 38% e após polimento com fluoreto de sódio 2% neutro (FS2%) ou pasta dentifrícia contendo partículas de nano-hidroxiapatita. Para isso, coroas de incisivos centrais humanos foram preparadas e tiveram suas faces vestibulares analisadas em microscópio de força atômica (MFA), o qual determinou os valores de rugosidade [Ra, RMS, Z range e Power Spectral Density (PSD)] iniciais. A cor e o brilho destas amostras foram determinados por um espectrofotômetro. Todas as amostras foram clareadas com PH 38% por 135 minutos. Os valores de Ra, RMS, Z range e PSD foram estabelecidos pelo MFA e a cor e o brilho determinados pelo espectrofotômetro. As amostras foram divididas em dois grupos: Flúor, que recebeu um polimento com gel de FS2%; e nHA, que recebeu um polimento com pasta dentifrícia contendo partículas de nano-hidroxiapatita. Os valores de Ra, RMS, Z range, PSD, cor e brilho pós-polimento foram determinados pelo MFA e espectrofotômetro. Após o clareamento, os valores de Ra, RMS, Z range e PSD não apresentaram alteração estatisticamente significante, os valores de L* aumentaram e C* diminuiu significativamente em todas as amostras. O brilho superficial não apresentou alteração significativa após o clareamento. O grupo Flúor não apresentou alteração de rugosidade significativa para Ra, RMS, Z range e PSD após o polimento. Os valores de L*, C* e brilho superficial também não apresentaram alterações significativas após o polimento das superfícies clareadas. No grupo nHA, os valores de Ra e RMS não apresentaram alteração significativa após o polimento das superfícies clareadas, porém os valores de Z range e PSD apresentaram alteração estatisticamente significante. Em comparação à superfície clareada, L* e C* não apresentaram alteração significante após o polimento, porém o brilho superficial foi significativamente maior. O tratamento clareador de consultório mostrou ser eficiente quanto à alteração de cor e não gerou aumento na rugosidade superficial do esmalte dental. Um polimento com pasta dentifrícia contendo partículas de nano-hidroxiapatita realizado após o clareamento é capaz de aumentar o brilho e diminuir a rugosidade superficial do esmalte dental. / Bleaching treatment may result in dental enamel surface roughness alterations, which might be seen as color alterations, opacity and gloss loss. The aim of this research was to in vitro investigate roughness, color and gloss alterations of human dental enamel surfaces after bleaching treatment with 38% hydrogen peroxide (HP) and after polishing with neutral 2% sodium fluoride or dental tooth paste containing nano-hydroxiapatite particles. Human central incisors were prepared and buccal surfaces were analyzed by an atomic force microscope (AFM), which determined roughness values [Ra, RMS, Z range and Power Spectral Density (PSD)]. Surface color and gloss were determined by a spectrophotometer. All samples were bleached with 38% HP for 135 minutes. AFM determined Ra, RMS, Z range and PSD after bleaching. Color and gloss were determined by the spectrophotometer. Samples were distributed in two different groups: Fluor, which was polished with neutral 2% sodium fluoride, and nHA, which was polished with dental tooth paste containing nano-hydroxyapatite particles. Ra, RMS, Z range, PSD, color and gloss values were determined by AFM and spectrophotometer after polishing. After bleaching, Ra, RMS, Z range and PSD didnt show any statistical difference. L* increased and C* decreased significantly in all samples after bleaching. Surface gloss didnt show significant alteration after bleaching. Fluor group didnt show surface roughness alteration considering Ra, RMS, Z range and PSD after polishing. L*, C* and gloss didnt change after bleached surfaces are polished with neutral 2% sodium fluoride. Ra and RMS of nHA group didnt change significantly after polishing, but Z range and PSD showed significant alteration. Despite L* and C* didnt change, gloss increased significantly after polishing with dental tooth paste containing nano-hydroxyapatite. In-office bleaching treatment showed to be efficient as for color enhancement and didnt cause roughness alteration in dental enamel surface. An after-bleaching polishing with dental tooth paste containing nano-hydroxyapatite particles may increase gloss and decrease surface roughness of dental enamel.

"An apparatus for the delivery of radiation to the tip-sample interface of an Atomic Force Microscope (AFM) is demonstrated. The Pulsed Light Delivery System (PLDS) was fabricated to probe photoinduced conformational changes of molecules using an AFM. The PLDS is 67 mm long, 59 mm wide, and 21 mm high, leaving clearance to mount the PLDS and a microscope slide coated with a thin film of photoactive molecules beneath the cantilever tip of a stand-alone AFM. The PLDS is coupled into a fiber pigtailed Nd:Yag frequency doubled laser, operating at a wavelength of 532 nm. The radiation delivered to a sample through the PLDS can be configured for continuous or pulsed mode. The maximum continuous wave (CW) power delivered was 0.903 mW and the minimum pulse width was 12.3 ms (maximal 401 ms), corresponding to a minimal energy of 0.150 nJ (maximal 362 nJ), and had a cycle duration of 10.0 ms. The PLDS consists of micro-optical components 3.0 mm and smaller in diameter. The optical design was inspired by the three-beam pick-up method used in CD players, which could provide a method to focus the pulse of light onto the sample layer. In addition, the system can be easily modified for different operational parameters (pulse width, wavelength, and power). As proof that the prototype design works, we observed a photoinduced ‘bimetallic’ bending of the cantilever, as evidenced by observing no photoinduced bending when a reflective-coated cantilever was replaced by an uncoated cantilever. Using the apparatus will allow investigation of many different types of molecules exhibiting photoinduced isomerization."