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Description
With the advent of the X-ray free-electron laser (XFEL), an opportunity has arisen to break the nexus between radiation dose and spatial resolution in diffractive imaging, by outrunning radiation damage altogether when using single X-ray pulses so brief that they terminate before atomic motion commences. This dissertation concerns the application of XFELs to biomolecular imaging in an effort to overcome the severe challenges associated with radiation damage and macroscopic protein crystal growth. The method of femtosecond protein nanocrystallography (fsPNX) is investigated, and a new method for extracting crystallographic structure factors is demonstrated on simulated data and on the first experimental fsPNX data obtained at an XFEL. Errors are assessed based on standard metrics familiar to the crystallography community. It is shown that resulting structure factors match the quality of those measured conventionally, at least to 9 angstrom resolution. A new method for ab-initio phasing of coherently-illuminated nanocrystals is then demonstrated on simulated data. The method of correlated fluctuation small-angle X-ray scattering (CFSAXS) is also investigated as an alternative route to biomolecular structure determination, without the use of crystals. It is demonstrated that, for a constrained two-dimensional geometry, a projection image of a single particle can be formed, ab-initio and without modeling parameters, from measured diffracted intensity correlations arising from disordered ensembles of identical particles illuminated simultaneously. The method is demonstrated experimentally, based on soft X-ray diffraction from disordered but identical nanoparticles, providing the first experimental proof-of-principle result. Finally, the fundamental limitations of CFSAXS is investigated through both theory and simulations. It is found that the signal-to-noise ratio (SNR) for CFSAXS data is essentially independent of the number of particles exposed in each diffraction pattern. The dependence of SNR on particle size and resolution is considered, and realistic estimates are made (with the inclusion of solvent scatter) of the SNR for protein solution scattering experiments utilizing an XFEL source.
ContributorsKirian, Richard A (Author) / Spence, John C. H. (Committee member) / Doak, R. Bruce (Committee member) / Weierstall, Uwe (Committee member) / Bennett, Peter (Committee member) / Treacy, Michael M. J. (Committee member) / Arizona State University (Publisher)
Created2011
Description
Protein crystallization is a technique for the formation of three-dimensional protein crystals, which is widely utilized by scientists, engineers, and researchers. Protein crystallography allows for protein structures and functions to be studied. As proteins play a central role in biological systems and life itself, a deeper understanding of their structure-function properties is crucial to elucidating fundamental behaviors, such as protein folding in addition to the role that they play in emerging fields, such as, tissue engineering with application to the emerging field of regenerative medicine. However, a significant limitation toward achieving further advancements in this field is that in order to determine detailed structure of proteins from protein crystals, high-quality and larger size protein crystals are needed. Because it is difficult to produce adequate size, high-quality crystals, it remains difficult to determine the structure of many proteins. However, a new method using a microgravity environment to crystallize proteins has proven effective through various studies conducted on the International Space Station (ISS). In the presence of microgravity, free convection is essentially absent in the bulk solution where crystallization occurs, thus allowing for purely random Brownian motion to exist which favors the nucleation and growth of high-quality protein crystals. Many studies from the ISS to date have demonstrated that growing protein crystals in a microgravity environment produces larger and higher-quality crystals. This method provides new opportunities for better structure identification and analysis of proteins. Although there remains many more limitations and challenges in the field, microgravity protein crystallization holds many opportunities for the future of biotechnology and scientific development. The objective of this thesis was to study the crystallization of hen egg white lysozyme (HEWL) and determine the effects of both unit and microgravity on growth/size and quality of HEWL. Through preliminary trials using a universal ground-based reduced-gravity system, the crystallization of HEWL in a simulated microgravity environment was successfully conducted and the results reported are promising. The utility of continuous, scalable ground-based, microgravity platforms for studies on a wide range of material systems and behavior, such as, protein crystallization, has significant implications regarding its impact on many industries, including drug development as well as regenerative medicine.
ContributorsTran, Amanda Marie (Author) / Pizziconi, Vincent (Thesis director) / Alford, Terry (Committee member) / Chemical Engineering Program (Contributor) / Barrett, The Honors College (Contributor)
Created2020-12
Description
Gallium-based liquid metals are of interest for a variety of applications including flexible electronics, soft robotics, and biomedical devices. Still, nano- to microscale device fabrication with these materials is challenging because of their strong adhesion to a majority of substrates. This unusual high adhesion is attributed to the formation of a thin oxide shell; however, its role in the adhesion process has not yet been established. In the first part of the thesis, we described a multiscale study aiming at understanding the fundamental mechanisms governing wetting and adhesion of gallium-based liquid metals. In particular, macroscale dynamic contact angle measurements were coupled with Scanning Electron Microscope (SEM) imaging to relate macroscopic drop adhesion to morphology of the liquid metal-surface interface. In addition, room temperature liquid-metal microfluidic devices are also attractive systems for hyperelastic strain sensing. Currently two types of liquid metal-based strain sensors exist for inplane measurements: single-microchannel resistive and two-microchannel capacitive devices. However, with a winding serpentine channel geometry, these sensors typically have a footprint of about a square centimeter, limiting the number of sensors that can be embedded into. In the second part of the thesis, firstly, simulations and an experimental setup consisting of two GaInSn filled tubes submerged within a dielectric liquid bath are used to quantify the effects of the cylindrical electrode geometry including diameter, spacing, and meniscus shape as well as dielectric constant of the insulating liquid and the presence of tubing on the overall system's capacitance. Furthermore, a procedure for fabricating the two-liquid capacitor within a single straight polydiemethylsiloxane channel is developed. Lastly, capacitance and response of this compact device to strain and operational issues arising from complex hydrodynamics near liquid-liquid and liquid-elastomer interfaces are described.
ContributorsLiu, Shanliangzi (Author) / Rykaczewski, Konrad (Thesis advisor) / Alford, Terry (Committee member) / Herrmann, Marcus (Committee member) / Hildreth, Owen (Committee member) / Arizona State University (Publisher)
Created2015
Description
Stress-related failure such as cracking are an important photovoltaic (PV) reliability issue since it accounts for a high percentage of power losses in the midlife-failure and wear-out failure regimes. Cell cracking can only be correlated with module degradation when cracks are of detectable size and detrimental to the performance. Several techniques have been explored to access the deflection and stress status on solar cell, but they have disadvantages such as high surface sensitivity.
This dissertation presents a new and non-destructive method for mapping the deflection on encapsulated solar cells using X-ray topography (XRT). This method is based on Bragg diffraction imaging, where only the areas that meet diffraction conditions will present contrast. By taking XRT images of the solar cell at various sample positions and applying an in-house developed algorithm framework, the cell‘s deflection map is obtained. Error analysis has demonstrated that the errors from the experiment and the data processing are below 4.4 and 3.3%.
Von Karman plate theory has been applied to access the stress state of the solar cells. Under the assumptions that the samples experience pure bending and plain stress conditions, the principal stresses are obtained from the cell deflection data. Results from a statistical analysis using a Weibull distribution suggest that 0.1% of the data points can contribute to critical failure. Both the soldering and lamination processes put large amounts of stress on solar cells. Even though glass/glass packaging symmetry is preferred over glass/backsheet, the solar cells inside the glass/glass packaging experience significantly more stress. Through a series of in-situ four-point bending test, the assumptions behind Von Karman theory are validated for cases where the neutral plane is displaced by the tensile and compressive stresses.
The deflection and stress mapping method is applied to two next generation PV concepts named Flex-circuit and PVMirror. The Flex-circuit module concept replaces traditional metal ribbons with Al foils for electrical contact and PVMirror concept utilizes a curved PV module design with a dichroic film for thermal storage and electrical output. The XRT framework proposed in this dissertation successfully characterized the impact of various novel interconnection and packaging solutions.
This dissertation presents a new and non-destructive method for mapping the deflection on encapsulated solar cells using X-ray topography (XRT). This method is based on Bragg diffraction imaging, where only the areas that meet diffraction conditions will present contrast. By taking XRT images of the solar cell at various sample positions and applying an in-house developed algorithm framework, the cell‘s deflection map is obtained. Error analysis has demonstrated that the errors from the experiment and the data processing are below 4.4 and 3.3%.
Von Karman plate theory has been applied to access the stress state of the solar cells. Under the assumptions that the samples experience pure bending and plain stress conditions, the principal stresses are obtained from the cell deflection data. Results from a statistical analysis using a Weibull distribution suggest that 0.1% of the data points can contribute to critical failure. Both the soldering and lamination processes put large amounts of stress on solar cells. Even though glass/glass packaging symmetry is preferred over glass/backsheet, the solar cells inside the glass/glass packaging experience significantly more stress. Through a series of in-situ four-point bending test, the assumptions behind Von Karman theory are validated for cases where the neutral plane is displaced by the tensile and compressive stresses.
The deflection and stress mapping method is applied to two next generation PV concepts named Flex-circuit and PVMirror. The Flex-circuit module concept replaces traditional metal ribbons with Al foils for electrical contact and PVMirror concept utilizes a curved PV module design with a dichroic film for thermal storage and electrical output. The XRT framework proposed in this dissertation successfully characterized the impact of various novel interconnection and packaging solutions.
ContributorsMeng, Xiaodong (Author) / Bertoni, Marian I (Thesis advisor) / Meier, Rico (Committee member) / Holman, Zachary C (Committee member) / Alford, Terry (Committee member) / Arizona State University (Publisher)
Created2019
Description
Nanoholes on the basal plane of graphene can provide abundant mass transport channels and chemically active sites for enhancing the electrochemical performance, making this material highly promising in applications such as supercapacitors, batteries, desalination, molecule or ion detection, and biosensing. However, the current solution-based chemical etching processes to manufacture these nanoholes commonly suffer from low process efficiency, scalability, and controllability, because conventional bulk heating cannot promote the etching reactions. Herein, a novel manufacturing method is developed to address this issue using microwave irradiation to facilitate and control the chemical etching of graphene. In this process, microwave irradiation induces selective heating of graphene in the aqueous solution due to an energy dissipation mechanism coupled with the dielectric and conduction losses. This strategy brings a remarkable reduction of processing time from hour-scale to minute-scale compared to the conventional approaches. By further incorporating microwave pretreatment, it is possible to control the population and area percentage of the in-plane nanoholes on graphene. Theoretical calculations reveal that the nanoholes emerge and grow by a repeating reduction–oxidation process occurring at the edge-sites atoms around vacancy defects on the graphene basal plane. The reduced holey graphene oxide sheets obtained via the microwave-assisted chemical etching method exhibit great potentials in supercapacitors and electrocatalysis. Excellent capacitive performance and electrocatalytic activity are observed in electrochemical measurements. The improvements against the non-holey counterpart are attributed to the enhanced kinetics involving ion diffusion and heterogeneous charge transfer.
ContributorsWang, Dini (Author) / Nian, Qiong (Thesis advisor) / Alford, Terry (Committee member) / Wang, Qing Hua (Committee member) / Zhuang, Houlong (Committee member) / Arizona State University (Publisher)
Created2021