In this thesis work, it was aimed to optimize the conditions to produce silicon carbide (SiC), from rice husks from Turkish Thrace Region, via pyrolysis. Rice husks, coked at 500oC, were high energy ball-milled prior to pyrolysis, in order to investigate the effects of ball-milling on pyrolysis temperature, pyrolysis time and morphology of the SiC produced. Samples of rice husks subjected to different ball milling conditions, were pyrolyzed at temperatures varying from 1500oC to 1600oC and for times varying from &frac12 / hour to 2 hours. Results of experiments showed that, ball-milling reduced the pyrolysis temperature and pyrolysis time to some extent. It was also experimentally shown that ball-milling favored the formation of SiC particles rather than formation of SiC whisker.

Compaction of polymer powders and polymer-based nanocomposites by uniaxial high-velocity cold compaction (HVC), by high-energy ball milling (HEBM) and using a novel technique, relaxation assists, was investigated with a focus on the process parameters, the compactibility characteristics, surface morphology and friction. The basic phenomena associated with HVC are explained and the general energy principle is introduced to explain the pull-out phenomenon, springback gradient, delay time, relative time of the pressure wave, and stick-slip phenomenon during the compaction process. Experimental results for different compaction profiles, different particle size distributions and different milling system for polymer-based nanocomposite are presented, showing the effect of varying the process parameters on the compacted material; the compactibility in the compacted bed, the uniformity of the compacted surface, the pull-out phenomenon, the springback gradient, the stick-slip phenomenon and the homogeneity of the dispersions of nanoparticles in the polymer powders in the solid state. It was found that the high-velocity compaction process is an interruption process and that the opposite velocity and pressure loss during the compaction process have a major influence on the quality of the compacted material. The relaxation assist device is a novel technique that has been successfully developed to improve the compaction process. The relaxation assists are parts of the piston and they are regarded as projectile supports. They are constructed of the same material as the piston, and the diameters are the same but the lengths are different. The relaxation assist device leads to an improvement in the compaction of powders, polymer powders and polymer-based nanocomposites by giving a more homogeneous opposite velocity and a better locking of the powder bed in the compacted form during the compaction process with less change in dimensions in the case of both homogeneous and heterogeneous materials. If the movement of the particles is restricted the powder bed attains a higher density and the total elastic springback is minimized. In addition, there is a more homogeneous dispersion of nanoparticles in the case of a heterogeneous material. A much better transfer of the pressure through the powder bed and a smaller loss of pressure lead to a more homogenous stick-slip of the particles and a higher sliding coefficient due to the overall friction during the compaction process. / QC 20100630

Although a considerable amount of research exists on geometrical aspects of 5-axis flank milling, the dynamics of this efficient milling operation have not yet been given proper attention. In particular, investigating machining chatter in 5-axis flank milling remains as an open problem in the literature. The axial depth of cut in this operation is typically quite large, which makes it prone to machining chatter. In this thesis, chatter in 5-axis flank milling is studied by developing analytical methods of examining vibration stability, generating numerical simulations of the process, and conducting experimental investigations. The typical application of 5-axis milling includes the machining of thermal resistant steel alloys at low cutting speeds, where the process damping dominates the machining vibration. The results of experimental study in this thesis showed that the effect of process damping is even stronger in flank milling due to the long axial engagement. Accordingly, the first part of the thesis is devoted to studying process damping, and in the second part, the modeling of chatter in flank milling is presented. Linear and nonlinear models have been reported in the literature that account for process damping. Although linear models are easier to implement in predicting stability limits, they could lead to misinterpretation of the actual status of the cut. On the other hand, nonlinear damping models are difficult to implement for stability estimation analytically, yet they allow the prediction of “finite amplitude stability” from time domain simulations. This phenomenon of “finite amplitude stability” has been demonstrated in the literature using numerical simulations. In this thesis, that phenomenon is investigated experimentally. The experimental work focuses on uninterrupted cutting, in particular plunge turning, to avoid unduly complications associated with transient vibration. The experiments confirm that, because of the nonlinearity of the process damping, the transition from fully stable to fully unstable cutting occurs gradually over a range of width of cut. The experimental investigation is followed by developing a new formulation for process damping based on the indentation force model. Then, the presented formulation is used to compute the stability lobes in plunge turning, taking into account the effect of nonlinear process damping. The developed lobes could be established for different amplitudes of vibration. This is a departure from the traditional notion that the stability lobes represent a single boundary between fully stable and fully unstable cutting conditions. Moreover, the process damping model is integrated into the Multi-Frequency Solution and the Semi Discretization Method to establish the stability lobes in milling. The basic formulations are presented along with comparisons between the two approaches, using examples from the literature. A non-shallow cut is employed in the comparisons. Assessing the performance of the two methods is conducted using time domain simulations. It is shown that the Semi Discretization Method provides accurate results over the whole tested range of cutting speed, whereas higher harmonics are required to achieve the same accuracy when applying the Multi Frequency Solution at low speeds. Semi Discretization method is modified further to calculate the stability lobes in flank milling with tools with helical teeth. In addition to the tool helix angle and long axial immersion, the effect of instantaneous chip thickness on the cutting force coefficients is considered in the modified formulation of Semi Discretization as well. Considering the effect of chip thickness variation on the cutting force coefficients is even more important in the modeling of 5-axis flank milling, where the feedrate, and consequently the chip thickness, varies at each cutter location. It also varies along the tool axis due to the additional rotary and tilt axis. In addition to the feedrate, the tool and workpiece engagement geometry varies at each cutter location as well. The actual feedrate at each cutter location is calculated by the dynamic processing of the toolpath. The tool and workpiece engagement geometry is calculated analytically using the parametric formulation of grazing surface at the previous and current passes. After calculating the instantaneous chip thickness and tool/workpiece engagement geometry, they are integrated into the Semi Discretization Method in 5-axis flank milling to examine the stability of vibration at each cutter location. While the presented chatter analysis results in establishing stability lobes in 3-axis flank milling, it results in developing a novel approach in presenting the stability of the cut in 5-axis flank milling. The new approach, namely “stability maps”, determines the unstable cutter locations of the toolpath at each spindle speed. The accuracy of established 3-axis flank milling stability lobes and 5-axis stability maps is verified by conducting a set of cutting experiments and numerical simulations.

A titanium dioxide powder co-doped with boron and zirconium was prepared by mechanical ball milling. Photocatalytic performance of the powder was evaluated by degradation of methylene blue (MB) solution under UV illumination. XRD patterns were refined by Rietveld analysis method to obtain accurate lattice parameters and position of the atoms in the crystal structure of TiO2. XRD analysis indicated that the B and/or Zr doped TiO2 powders composed of anatase and did not exhibit any additional phase. Rietveld analysis suggested that dopant B and Zr elements were successfully weaved into crystal structure and distorted the lattice of TiO2. The highest distortion was obtained by co-doping. SEM investigations confirmed that mechanical ball milling technique led to a decrease in particle size of TiO2 powder. XPS analysis revealed that dopant B and Zr atoms did not appear in any form of compound including Ti and O elements. Results of photocatalytic activity test suggested that boron and zirconium co-doped TiO2 particles exhibited a better visible light response and photocatalytic activity than that of mono element doped TiO2 (i.e. B-TiO2 and Zr-TiO2) and undoped TiO2 particles. A 20% improvement in photocatalytic activity of reference TiO2 powder (powder ball milled without dopant addition) was achieved by B and Zr co-doping. The enhanced photocatalytic activity is attributed to synergistic effects of B-Zr co-doping the lattice of TiO2 as well as particle size reduction.

The present work reports a study of the effects of the compositions, and various catalytic additives and nanostructuring by high-energy ball milling, on the hydrogen storage properties of LiBH4, NaBH4, LiNH2 and LiAlH4 complex hydrides and their composites. The composites of (NaBH4+2Mg(OH)2) and (LiBH4+2Mg(OH)2) without and with nanometric nickel (n-Ni) added as a potential catalyst were synthesized by ball milling. The effect of the addition of 5 wt.% nanometric Ni on the dehydrogenation behavior of both the NaBH4-and LiBH4-based composites is rather negligible. In the (LiNH2+nMgH2) system, the phase transformations occurring as a function of the ball milling energy injected into the hydride system (LiNH2+nMgH2), having molar ratios n=0.5 to 2.0, have been thoroughly studied. The milling energy is estimated by a semi-empirical method. The results show that for the molar ratios n<1.0 three new phases such as LiH, amorphous Mg(NH2)2 (a-Mg(NH2)2) and Li2Mg(NH)2 are formed during ball milling depending on the injected energy. For the molar ratios n≥1.0 the new phase of MgNH forms whose formation is accompanied by a profound release of hydrogen. Addition of 5 %wt. KH can improve desorption rate of the LiNH2+0.5 MgH2 system. Furthermore this hydride system can be nearly fully rehydrogenated at 200°C and 50 bar H2 pressure. LiAlH4 containing 5 wt.% of nanometric Fe and Ni shows a profound mechanical dehydrogenation by continuously desorbing hydrogen (H2) during ball milling. X-ray diffraction studies show that Fe and Ni ions dissolve in the lattice, replacing the Al ions and forming a substitutional solid solution. Both Fe and Ni decrease the activation energies of stage I and II , but stage I is more sensitive to the particle size . The addition of 5 wt.% nano-size “interstitial compound” (n-TiC, n-TiN and n-ZrC) shows a continuous desorption of H2 is observed during high energy milling. Mechanical dehydrogenation rate of the doped samples increases noticeably during high-energy ball milling in the order of TiN > TiC > ZrC. The interstitial compound additives are able to strongly reduce the activation energy of Stage II dehydrogenation but do not substantially affect the apparent activation energy of Stage I .

In this dissertation, a numerical method to design a curved surface for accurately flank milling with a general tool of revolution is presented. Instead of using the ruled surface as the design surface, the flank millable surface can better match the machined surface generated by flank milling techniques, and provide an effective tool to the designer to control the properties and the specifications of the design surface. A method using the least squares surface fitting to design the flank millable surface is first discussed. Grazing points on the envelope of the moving tool modeled by the grazing surface are used as the sample points and a NURBS surface is used to approximate the given grazing surface. The deviation between the grazing surface and the NURBS surface can be controlled by increasing the number of the control points. The computation process for this method is costly in time and effort. In engineering design, there is a need for fast and effortless methods to simplify the flank millable surface design procedure. A technique to approximate the grazing curve with NURBS at each tool position is developed. Based on the characteristics of the grazing surface and the geometries of the cutting tool, these NURBS representations at a few different tool positions, namely at the start, interior and end, are lofted to generate a NURBS surface. This NURBS surface represents the grazing surface and is treated as the design surface. Simulation results show that this design surface can accurately match the machined surface. The accuracy of the surface can be controlled by adding control points to the control net of the NURBS surface. A machining test on a 5-axis machine was done to verify the proposed flank millable surface design method. The machined surface was checked on a CMM and the obtained results were compared with the designed flank millable surface. The comparison results show that the machined surface closely matches the design surface. The proposed flank millable surface design method can be accurately used in the surface design.

Tuberculosis causes more deaths worldwide than any other curable infectious disease. This is the case despite tuberculosis appearing to be on the verge of eradication midway through the last century. Efforts at reversing the spread of tuberculosis have intensified since the early 1990s. Since then, microscopy has been the primary frontline diagnostic. In this dissertation, advances in clinical microscopy towards array microscopy for digital detection of Mycobacterium tuberculosis are presented. Digital array microscopy separates the tasks of microscope operation and pathogen detection and will reduce the specialization needed in order to operate the microscope. Distributing the work and reducing specialization will allow this technology to be deployed at the point of care, taking the front-line diagnostic for tuberculosis from the microscopy center to the community health center. By improving access to microscopy centers, hundreds of thousands of lives can be saved. For this dissertation, a lens was designed that can be manufactured as 4×6 array of microscopes. This lens design is diffraction limited, having less than 0.071 waves of aberration (root mean square) over the entire field of view. A total area imaged onto a full-frame digital image sensor is expected to be 3.94 mm2, which according to tuberculosis microscopy guidelines is more than sufficient for a sensitive diagnosis. The design is tolerant to single point diamond turning manufacturing errors, as found by tolerance analysis and by fabricating a prototype. Diamond micro-milling, a fabrication technique for lens array molds, was applied to plastic plano-concave and plano-convex lens arrays, and found to produce high quality optical surfaces. The micro-milling technique did not prove robust enough to produce bi-convex and meniscus lens arrays in a variety of lens shapes, however, and it required lengthy fabrication times. In order to rapidly prototype new lenses, a new diamond machining technique was developed called 4-axis single point diamond machining. This technique is 2-10x faster than micro-milling, depending on how advanced the micro-milling equipment is. With array microscope fabrication still in development, a single prototype of the lens designed for an array microscope was fabricated using single point diamond turning. The prototype microscope objective was validated in a pre-clinical trial. The prototype was compared with a standard clinical microscope objective in diagnostic tests. High concordance, a Fleiss’s kappa of 0.88, was found between diagnoses made using the prototype and standard microscope objectives and a reference test. With the lens designed and validated and an advanced fabrication process developed, array microscopy technology is advanced to the point where it is feasible to rapidly prototype an array microscope for detection of tuberculosis and translate array microscope from an innovative concept to a device that can save lives.

Two species of emergent macrophytes, Typha latifolia (common cattail) and Phalaris arundinacea (reed canary grass) were evaluated as substrates for biogas production. The specific methane yield for each plant was obtained by batch wise anaerobic digestion in 300-mL bottles. Three different pretreatments were evaluated for increased biogas production; mechanical milling, alkaline treatment with lime and fungal degradation with Pleurotus ostreatus (oyseter mushroom).The methane yield for Typha latifolia and Phalaris arundinacea was determined to 300 and 323mL methane per g VS, respectively. There was no statistical difference in methane yield between the two species. Milling pretreatment increased the biogas yield with 16 % by average compared to untreated plant. Alkaline pretreatment with lime increased the biogas yield with 27 % at roomtemp. and 22 % at 55 °C. The fungal pretreatment decreased the biogas production by 20 % and is probably not suitable for this kind of substrate.The results showed that emergent macrophytes have a biogas yield similar to other plants already tested (grasses) and commonly used (pasture crops) in large scale reactors. However, emergent macrophytes and grasses cause mechanical problems in a reactor due to their structure. Probably some kind of milling must be done to decrease the fiber length of the emergent macrophytes. The costs for harvest, transport, handling and possible pretreatment of the emergent macrophytes have to be estimated and included in the overall cost calculations. This can tell if emergent macrophytes should be used as a substrate for biogas production.

In this dissertation, a numerical method to design a curved surface for accurately flank milling with a general tool of revolution is presented. Instead of using the ruled surface as the design surface, the flank millable surface can better match the machined surface generated by flank milling techniques, and provide an effective tool to the designer to control the properties and the specifications of the design surface. A method using the least squares surface fitting to design the flank millable surface is first discussed. Grazing points on the envelope of the moving tool modeled by the grazing surface are used as the sample points and a NURBS surface is used to approximate the given grazing surface. The deviation between the grazing surface and the NURBS surface can be controlled by increasing the number of the control points. The computation process for this method is costly in time and effort. In engineering design, there is a need for fast and effortless methods to simplify the flank millable surface design procedure. A technique to approximate the grazing curve with NURBS at each tool position is developed. Based on the characteristics of the grazing surface and the geometries of the cutting tool, these NURBS representations at a few different tool positions, namely at the start, interior and end, are lofted to generate a NURBS surface. This NURBS surface represents the grazing surface and is treated as the design surface. Simulation results show that this design surface can accurately match the machined surface. The accuracy of the surface can be controlled by adding control points to the control net of the NURBS surface. A machining test on a 5-axis machine was done to verify the proposed flank millable surface design method. The machined surface was checked on a CMM and the obtained results were compared with the designed flank millable surface. The comparison results show that the machined surface closely matches the design surface. The proposed flank millable surface design method can be accurately used in the surface design.

<p>The goal of this work is to develop a practical and comprehensive methodology to study the response and the stability of various delay differential equations (DDEs). The development of these new analysis techniques is motivated by the existence of delays in the governing equations of many physical systems such as turning and milling processes. </p><p>Delay differential equations appear in many models in science in engineering either as an intrinsic component (e.g. machining dynamics) or as a modeling decision (biology related dynamics). However, the infinite dimensionality of DDEs significantly complicates the resulting analysis from both an analytical and numerical perspective. Since the delay results in an infinite dimensional state-space, it is often necessary to use an approximate procedure to study DDEs and ascertain their stability.</p><p>Several approximate techniques appeared in literature to study the stability of DDEs. However, a large number of these techniques---such as D-subdivision, Cluster Treatment of Characteristic Roots and Continuous Time Approximation---are limited to autonomous DDEs. Moreover, the methods that are suitable for non-autonomous DDEs, e.g. the Semi-discretization approach, often result in a very large system of algebraic equations that can cause computational difficulties. Collocation-type methods, such as Chebyshev-collocation approach, have also been used to study DDEs. One major limitation of the conventional Chebyshev collocation approach is that it is strictly applicable to DDEs with continuous coefficients. An alternative approach that can handle DDEs with piecewise continuous coefficients is the Temporal Finite Element Analysis (TFEA). However, TFEA has only linear rates of convergence and is limited to h-convergence schemes. The limited rate of convergence in TFEA has prohibited its application to a wide class of DDEs such as DDEs with complicated coefficients or with distributed and multiple delays. </p><p>In this thesis, I develop a spectral element method for the stability analysis of DDEs. The spectral element method is a Galerkin-type approach that discretizes the infinite dimensional DDE into a finite set of algebraic equations (or a dynamic map). The stability of the system is then studied using the eigenvalues of the map. </p><p>In contrast to TFEA, the spectral element method was shown to have exponential rates of convergence and hp-refinement capabilities. Further, a comparison with the widely-used collocation methods showed that our approach can often yield higher rates of convergence. The higher rates of convergence of the developed approach enabled extending it to DDEs with multiple and distributed delays. I further extended this approach to calculating the periodic orbits of DDEs and their stability. </p><p>As an application of the methods developed in this thesis, I studied the stability of turning and milling models. For example, a distributed force model was proposed to characterize cutting forces in turning. The stability of the resulting delay integro-differential equation was studied using the methods developed in this study and they were shown to agree with practical observations. As another example, the stability of a milling process--- whose model contains piecewise coefficients---was investigated. The effect of multiple-flute engagement, which contributed to the complexity of the coefficients, was also investigated. The resulting stability charts revealed new stability observations in comparison to typical analysis methods. Specifically, I was able to show that unstable regions appear in what was deemed a stable region by prior analysis techniques.</p> / Dissertation