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Investigations concerning the cellular response of tumor tissue to treatment with dimethyl sulfoxide and hematoxylin have not been reported. To establish the response of neoplastic tissue and cells to this combination of agents, this study was undertaken to determine the effects of dimethyl sulfoxide and hematoxylin on a transplantable lymphosarcoma in mice.

One of the key measurement devices used in characterization of microelectromechanical systems (MEMS) is the interferometric microscope. This device allows remote, noninvasive measurements of the surface shape and deformations of MEMS in full-field-of-view with high spatial resolution and nanometer accuracy in near real-time. As MEMS are becoming more prevalent in the areas of consumer products and national defense, the demand for a versatile and easy to use characterization system is very high. This Thesis describes the design, implementation, and use of an interferometric system that is based on modular components which allow for many loading and measurement capabilities, depending on a specific application. The system has modules for subjecting MEMS to vacuum and dry gas environments, mechanical vibration excitation, thermal loads (both heating and cooling), and electrical loads. Three interferometric measurement modules can be interchanged to spatially measure shape and deformation of micro- and/or meso-scale objects, and temporally measure vibrations of these objects. Representative examples of the measurement and loading capabilities of the system are demonstrated with microcantilevers and a microgyroscope.

We present the development of a far-field magneto-optical Kerr effect microscope. An inverted optical microscope was constructed to accommodate Kerr imaging and atomic force microscopy. In Kerr microscopy, magnetic structure is investigated by measuring the polarization rotation of light reflected from a sample in the presence of a magnetic field. Atomic force microscopy makes use of a probe which is scanned over a sample surface to map the topography. The design was created virtually in SolidWorks, a three-dimensional computer-aided drafting environment, to ensure compatibility and function of the various components, both commercial and custom-machined, required for the operation of this instrument. The various aspects of the microscope are controlled by custom circuitry and a field programmable gate array data acquisition card at the direction of the control code written in National Instrument LabVIEW. The microscope has proven effective for both Kerr and atomic force microscopy. Kerr images are presented which reveal the bit structure of magneto-optical disks, as are atomic force micrographs of an AFM calibration grid. Also discussed is the future direction of this project, which entails improving the resolution of the instrument beyond the diffraction limit through near-field optical techniques. Preliminary work on fiber probe designs is presented along with probe fabrication work and the system modifications necessary to utilize such probes.

This work presents a new form of microscopy, the instrument constructed to demonstrate it, the images produced and the image contrast mechanisms seen for the first time. Some of its future scientific potential is described and finally, recent work towards advancing the method is discussed. Many forms of microscopy exist, each with unique advantages. Of several broad categories that they could be grouped into, those that use particle beams have proven very generally useful for micro and nano-scale imaging, including Scanning Electron, Transmission Electron, and Ion Beam microscopes. These have the disadvantage, however, of implanting electric charges into the sample, and usually at very high energy relative to the binding energy of molecules. For most materials this modifies the sample at a small scale and as we work increasingly towards the nano-scale, this is a serious problem. The Neutral Atom Microscope (NAM) uses a beam of thermal energy (under 70 meV) non-charged atoms or molecules to probe an atomic surface. For several decades scientists have been interested in this possibility, using a focused beam. Scattering of neutral atoms provides a uniquely low-energy, surface-sensitive probe, as is known from molecular beam experiments. We have developed a new approach, operating with the sample at a close working distance from an aperture, the need for optics to focus the beam is obviated. The demonstrated, practical performance of this "Pinhole" NAM exceeds all other attempts by great lengths by many measures. The unique images resulting and contrast mechanism discoveries are described. The future potential for nano-scale resolution is shown.

An instrument, adding the capability to measure 3D volumetric chemical composition, has been constructed by me as a member of the Sánchez Nano Laboratory. The laboratory's in situ atomic force microscope (AFM) and secondary ion mass spectrometry systems (SIMS) are functional and integrated as one instrument. The SIMS utilizes a Ga focused ion beam (FIB) combined with a quadrupole mass analyzer. The AFM is comprised of a 6-axis stage, three coarse axes and three fine. The coarse stage is used for placing the AFM tip anywhere inside a (13x13x5 mm3) (xyz) volume. Thus the tip can be moved in and out of the FIB processing region with ease. The planned range for the Z-axis piezo was 60 µm, but was reduced after it was damaged from arc events. The repaired Z-axis piezo is now operated at a smaller nominal range of 18 µm (16.7 µm after pre-loading), still quite respectable for an AFM. The noise floor of the AFM is approximately 0.4 nm Rq. The voxel size for the combined instrument is targeted at 50 nm or larger. Thus 0.4 nm of xyz uncertainty is acceptable. The instrument has been used for analyzing samples using FIB beam currents of 250 pA and 5.75 nA. Coarse tip approaches can take a long time so an abbreviated technique is employed. Because of the relatively long thro of the Z piezo, the tip can be disengaged by deactivating the servo PID. Once disengaged, it can be moved laterally out of the way of the FIB-SIMS using the coarse stage. This instrument has been used to acquire volumetric data on AlTiC using AFM tip diameters of 18.9 nm and 30.6 nm. Acquisition times are very long, requiring multiple days to acquire a 50-image stack. New features to be added include auto stigmation, auto beam shift, more software automation, etc. Longer term upgrades to include a new lower voltage Z-piezo with strain-gauge feedback and a new design to extend the life for the coarse XY nano-positioners. This AFM-SIMS instrument, as constructed, has proven to be a great proof of concept vehicle. In the future it will be used to analyze micro fossils and it will also be used as a part of an intensive teaching curriculum.

Traditional light microscopy suffers from the diffraction limit, which limits the spatial resolution to λ/2. The current trend in optical microscopy is the development of techniques to bypass the diffraction limit. Resolutions below 40 nm will make it possible to probe biological systems by imaging the interactions between single molecules and cell membranes. These resolutions will allow for the development of improved drug delivery mechanisms by increasing our understanding of how chemical communication within a cell occurs. The materials sciences would also benefit from these high resolutions. Nanomaterials can be analyzed with Raman spectroscopy for molecular and atomic bond information, or with fluorescence response to determine bulk optical properties with tens of nanometer resolution. Near-field optical microscopy is one of the current techniques, which allows for imaging at resolutions beyond the diffraction limit. Using a combination of a shear force microscope (SFM) and an inverted optical microscope, spectroscopic resolutions below 20 nm have been demonstrated. One technique, in particular, has been named tip enhanced near-field optical microscopy (TENOM). The key to this technique is the use of solid metal probes, which are illuminated in the far field by the excitation wavelength of interest. These probes are custom-designed using finite difference time domain (FDTD) modeling techniques, then fabricated with the use of a focused ion beam (FIB) microscope. The measure of the quality of probe design is based directly on the field enhancement obtainable. The greater the field enhancement of the probe, the more the ratio of near-field to far-field background contribution will increase. The elimination of the far-field signal by a decrease of illumination power will provide the best signal-to-noise ratio in the near-field images. Furthermore, a design that facilitates the delocalization of the near-field imaging from the far-field will be beneficial. Developed is a novel microscope design that employs two-photon non-linear excitation to allow the imaging of the fluorescence from almost any visible fluorophore at resolutions below 30 nm without changing filters or excitation wavelength. The ability of the microscope to image samples at atmospheric pressure, room temperature, and in solution makes it a very promising tool for the biological and materials science communities. The microscope demonstrates the ability to image topographical, optical, and electronic state information for single-molecule identification. A single computer, simple custom control circuits, field programmable gate array (FPGA) data acquisition, and a simplified custom optical system controls the microscope are thoroughly outlined and documented. This versatility enables the end user to custom-design experiments from confocal far-field single molecule imaging to high resolution scanning probe microscopy imaging. Presented are the current capabilities of the microscope, most importantly, high-resolution near-field images of J-aggregates with PIC dye. Single molecules of Rhodamine 6G dye and quantum dots imaged in the far-field are presented to demonstrate the sensitivity of the microscope. A comparison is made with the use of a mode-locked 50 fs pulsed laser source verses a continuous wave laser source on single molecules and J-aggregates in the near-field and far-field. Integration of an intensified CCD camera with a high-resolution monochromator allows for spectral information about the sample. The system will be disseminated as an open system design.

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M. Tech. Metallurgical Engineering. / Aims to study tensile deformation mechanisms of aluminium alloy 5083 using in situ SEM techniques. The objectives to achieve this aim are: to investigate the effect of strain rate on mechanical properties ; investigating anisotropy mechanical properties at varying strain rates ; investigating microstructure anisotropy behaviour at varying strain rates and to investigate the influence of intermetallic particles during tensile deformation.

published_or_final_version / abstract / toc / Physics / Doctoral / Doctor of Philosophy