Current Search: neutron diffraction (x)
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- Title
- LOW TEMPERATURE NITIFE SHAPE MEMORY ALLOYS: ACTUATOR ENGINEERING AND INVESTIGATION OF DEFORMATION MECHANISMS USING IN SITU NEUTRON DIFFRACTION AT LOS ALAMOS NATIONAL LABORATORY.
- Creator
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Krishnan, Vinu, Vaidyanathan, Raj, University of Central Florida
- Abstract / Description
-
Shape memory alloys are incorporated as actuator elements due to their inherent ability to sense a change in temperature and actuate against external loads by undergoing a shape change as a result of a temperature-induced phase transformation. The cubic so-called austenite to the trigonal so-called R-phase transformation in NiTiFe shape memory alloys offers a practical temperature range for actuator operation at low temperatures, as it exhibits a narrow temperature-hysteresis with a desirable...
Show moreShape memory alloys are incorporated as actuator elements due to their inherent ability to sense a change in temperature and actuate against external loads by undergoing a shape change as a result of a temperature-induced phase transformation. The cubic so-called austenite to the trigonal so-called R-phase transformation in NiTiFe shape memory alloys offers a practical temperature range for actuator operation at low temperatures, as it exhibits a narrow temperature-hysteresis with a desirable fatigue response. Overall, this work is an investigation of selected science and engineering aspects of low temperature NiTiFe shape memory alloys. The scientific study was performed using in situ neutron diffraction measurements at the newly developed low temperature loading capability on the Spectrometer for Materials Research at Temperature and Stress (SMARTS) at Los Alamos National Laboratory and encompasses three aspects of the behavior of Ni46.8Ti50Fe3.2 at 92 K (the lowest steady state temperature attainable with the capability). First, in order to study deformation mechanisms in the R-phase in NiTiFe, measurements were performed at a constant temperature of 92 K under external loading. Second, with the objective of examining NiTiFe in one-time, high-stroke, actuator applications (such as in safety valves), a NiTiFe sample was strained to approximately 5% (the R-phase was transformed to B19' phase in the process) at 92 K and subsequently heated to full strain recovery under a load. Third, with the objective of examining NiTiFe in cyclic, low-stroke, actuator applications (such as in cryogenic thermal switches), a NiTiFe sample was strained to 1% at 92 K and subsequently heated to full strain recovery under load. Neutron diffraction spectra were recorded at selected time and stress intervals during these experiments. The spectra were subsequently used to obtain quantitative information related to the phase-specific strain, texture and phase fraction evolution using the Rietveld technique. The mechanical characterization of NiTiFe alloys using the cryogenic capability at SMARTS provided considerable insight into the mechanisms of phase transformation and twinning at cryogenic temperatures. Both mechanisms contribute to shape memory and pseudoelasticity phenomena. Three phases (R, B19' and B33 phases) were found to coexist at 92 K in the unloaded condition (nominal holding stress of 8 MPa). For the first time the elastic modulus of R-phase was reported from neutron diffraction experiments. Furthermore, for the first time a base-centered orthorhombic (B33) martensitic phase was identified experimentally in a NiTi-based shape memory alloy. The orthorhombic B33 phase has been theoretically predicted in NiTi from density function theory (DFT) calculations but hitherto has never been observed experimentally. The orthorhombic B33 phase was observed while observing shifting of a peak (identified to be B33) between the R and B19' peaks in the diffraction spectra collected during loading. Given the existing ambiguity in the published literature as to whether the trigonal R-phase belongs to the P3 or P space groups, Rietveld analyses were separately carried out incorporating the symmetries associated with both space groups and the impact of this choice evaluated. The constrained recovery of the B19' phase to the R-phase recorded approximately 4% strain recovery between 150 K and 170 K, with half of that recovery occurring between 160 K and 162 K. Additionally, the aforementioned research methodology developed for Ni46.8Ti50Fe3.2 shape memory alloys was applied to experiments performed on a new high temperature Ni29.5Ti50.5Pd20 shape memory alloys. The engineering aspect focused on the development of (i) a NiTiFe based thermal conduction switch that minimized the heat gradient across the shape memory actuator element, (ii) a NiTiFe based thermal conduction switch that incorporated the actuator element in the form of helical springs, and (iii) a NiTi based release mechanism. Patents are being filed for all the three shape memory actuators developed as a part of this work. This work was supported by grants from SRI, NASA (NAG3-2751) and NSF (CAREER DMR-0239512) to UCF. Additionally, this work benefited from the use of the Lujan Center at the Los Alamos Neutron Science Center, funded by the United States Department of Energy, Office of Basic Energy Sciences, under Contract No. W-7405-ENG-36.
Show less - Date Issued
- 2007
- Identifier
- CFE0001934, ucf:47437
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0001934
- Title
- Multi-axial Thermomechanical Characterization of Shape Memory Alloys for Improved Stability.
- Creator
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Nicholson, Douglas, Vaidyanathan, Raj, Kumar, Ranganathan, Chen, Ruey-Hung, University of Central Florida
- Abstract / Description
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Shape recovery in shape memory alloys (SMAs) occurs against external stress by means of a reversible thermoelastic solid state phase transformation typically between so-called austenite, martensite and R-phases. The ability to do work enables their use as high-force actuators in automotive and aerospace applications while superelastic NiTi is of interest in biomedical devices such as stents. Both R-phase and martensite can detwin, reorient and undergo a thermal or stress induced...
Show moreShape recovery in shape memory alloys (SMAs) occurs against external stress by means of a reversible thermoelastic solid state phase transformation typically between so-called austenite, martensite and R-phases. The ability to do work enables their use as high-force actuators in automotive and aerospace applications while superelastic NiTi is of interest in biomedical devices such as stents. Both R-phase and martensite can detwin, reorient and undergo a thermal or stress induced transformation. For these reasons, it is difficult from ordinary macroscopic measurements to decouple elastic and inelastic contributions (from their respective phases) from the overall deformation. In situ neutron diffraction is ideally suited to probing these microstructural and micromechanical changes while they occur under external stress fields. Despite SMAs typically operating under multi-axial stress states in applications, most previous in situ neutron diffraction based investigations on SMAs have been limited to homogenous stress states as a result of uniaxial loading. The current investigation spatially maps thermoelastic deformation mechanisms during heating and uniaxial/torsional loading of shape memory and superelastic NiTi by recourse to in situ neutron diffraction, performed at Oak Ridge and Los Alamos National Laboratories. SMA spring actuators were also used to experimentally validate the ability of a recently developed model to predict the evolutionary deformation response under multi-axial loading conditions.By recourse to in situ neutron diffraction, martensite variants were tracked during isothermal, isobaric, and isostrain loading in shape memory NiTi. Results show variants were equivalent for the corresponding strain and more importantly, the reversibility and equivalency was immediately evident in variants that were first selected isobarically but then reoriented to a near random self-accommodated structure by isothermal deformation. Variants selected isothermally were not significantly affected by a subsequent thermal cycle under constant strain. During uniaxial/torsional loading and heating, thermoelastic deformation mechanisms in non-uniform states of stress in superelastic NiTi were spatially mapped. The preferred selection of R-phase variants by reorientation and detwinning processes were equivalent for the corresponding strain (in tension and compression) and was reversed by isothermal loading. The variants selected were consistent between uniaxial and torsional loading when the principal stress directions of the stress state were considered (for the crystallographic directions considered here). The similarity in general behavior between uniaxial and torsional loading, in spite of the implicit heterogeneous stress state associated with torsional loading, pointed to the ability of the reversible thermoelastic transformation to accommodate both stress and strain mismatch associated with deformation.Overall, various thermomechanical combinations of heating and loading sequences yielded the same final texture (preferred selection of variants), which highlighted the ability to take different paths yet still obtain the desired response while minimizing irrecoverable deformation mechanisms. These paths have implications for minimizing the number of cycles required to train an SMA, which limits the amount of work required for stabilizing their evolutionary response thereby increasing the fatigue life and overall durability of the SMA. This finding is valuable to the aerospace and medical device industries where SMAs find current application.
Show less - Date Issued
- 2017
- Identifier
- CFE0006952, ucf:51676
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0006952
- Title
- INVESTIGATION OF THERMAL, ELASTIC AND LOAD-BIASED TRANSFORMATION STRAINS IN NITI SHAPE MEMORY ALLOYS.
- Creator
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Qiu, Shipeng, Vaidyanathan, Raj, University of Central Florida
- Abstract / Description
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Polycrystalline NiTi shape memory alloys have the ability to recover their original, pre-deformed shape in the presence of external loads when heated through a solid-solid phase transformation from a lower-symmetry B19' martensite phase to a higher-symmetry B2 austenite phase. The strain associated with a shape memory alloy in an actuator application typically has thermal, elastic and inelastic contributions. The objective of this work was to investigate the aforementioned strains by...
Show morePolycrystalline NiTi shape memory alloys have the ability to recover their original, pre-deformed shape in the presence of external loads when heated through a solid-solid phase transformation from a lower-symmetry B19' martensite phase to a higher-symmetry B2 austenite phase. The strain associated with a shape memory alloy in an actuator application typically has thermal, elastic and inelastic contributions. The objective of this work was to investigate the aforementioned strains by recourse to in situ neutron diffraction experiments during selected combinations of heating, cooling and/or mechanical loading. The primary studies were conducted on polycrystalline Ni49.9Ti50.1 specimens on the Spectrometer for MAterials Research at Temperature and Stress (SMARTS) at Los Alamos National Laboratory. Quantitative information on the phase-specific strain, texture and phase fraction evolution was obtained from the neutron data using Rietveld refinement and single-peak analyses, and compared with macroscopic data from extensometry. First, the lattice strain evolution during heating and cooling in an unloaded sample (i.e., free-recovery experiment) was studied. The lattice strain evolution remained linear with temperature and was not influenced by intergranular stresses, enabling the determination of a thermal expansion tensor that quantified the associated anisotropy due to the symmetry of B19' NiTi. The tensor thus determined was subsequently used to obtain an average coefficient of thermal expansion that was consistent with macroscopic dilatometric measurements and a 30,000 grain polycrystalline self-consistent model. The accommodative nature of B19' NiTi was found to account for macroscopic shape changes lagging (with temperature) the start and finish of the transformation. Second, the elastic response of B19' martensitic NiTi variants during monotonic loading was studied. Emphasis was placed on capturing and quantifying the strain anisotropy which arises from the symmetry of monoclinic martensite and internal stresses resulting from intergranular constraints between individual variants and load re-distribution among variants as the texture evolved during variant reorientation and detwinning. The methodology adopted took into account both tensile and compressive loading given the asymmetric response in the texture evolution. Plane specific elastic moduli were determined from neutron measurements and compared with those determined using a self-consistent polycrystalline deformation model and from recently reported elastic stiffness constants determined via ab initio calculations. The comparison among the three approaches further helped understand the influence of elastic anisotropy, intergranular constraint, and texture evolution on the deformation behavior of polycrystalline B19' NiTi. Connections were additionally made between the assessed elastic properties of martensitic NiTi single crystals (i.e., the single crystal stiffness tensor) and the overall macroscopic response in bulk polycrystalline form. Lastly, the role of upper-cycle temperature, i.e., the maximum temperature reached during thermal cycling, was investigated during load-biased thermal cycling of NiTi shape memory alloys at selected combinations of stress and temperature. Results showed that the upper-cycle temperature, under isobaric conditions, significantly affected the amount of transformation strain and thus the work output available for actuation. With the objective of investigating the underlying microstructural and micromechanical changes due to the influence of the upper-cycle temperature, the texture evolution was systematically analyzed. While the changes in transformation strain were closely related to the evolution in texture of the room temperature martensite, retained martensite in the austenite state could additionally affect the transformation strain. Additionally, multiple thermal cycles were performed under load-biased conditions in both NiTi and NiTiPd alloys, to further assess and understand the role of retained martensite. Dimensional and thermal stabilities of these alloys were correlated with the volume fraction and texture of retained martensite, and the internal strain evolution in these alloys. The role of symmetry, i.e., B19' monoclinic martensite vs. B19 orthorhombic martensite in these alloys was also assessed. This work not only established a methodology to study the thermal and elastic properties of the low symmetry B19' monoclinic martensite, but also provided valuable insight into quantitative micromechanical and microstructural changes responsible for the thermomechanical response of NiTi shape memory alloys. It has immediate implications for optimizing shape memory behavior in the alloys investigated, with extension to high temperature shape memory alloys with ternary and quaternary elemental additions, such as Pd, Pt and Hf. This work was supported by funding from NASAÃÂ's Fundamental Aeronautics Program, Supersonics Project (NNX08AB51A) and NSF (CAREER DMR-0239512). It benefited additionally from the use of the Lujan Neutron Scattering Center at Los Alamos National Laboratory, which is funded by the Office of Basic Energy Sciences (Department of Energy) and is operated by Los Alamos National Security LLC under DOE Contract DE-AC52-06NA25396.
Show less - Date Issued
- 2010
- Identifier
- CFE0003362, ucf:48440
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0003362
- Title
- Scandia and ceria stabilized zirconia based electrolytes and anodes for intermediate temperature solid oxide fuel cells: Manufacturing and properties.
- Creator
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Chen, Yan, Orlovskaya, Nina, An, Linan, Chen, Quanfang, Sohn, Yongho, Raghavan, Seetha, Huang, Xinyu, University of Central Florida
- Abstract / Description
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Scandia and ceria stabilized zirconia (10 mol% Sc2O3 (-) 1 mol% CeO2 (-) ZrO2, SCSZ) has superior ionic conductivity in the intermediate temperature range for the operation of solid oxide fuel cells, but it does not exhibit good phase stability in comparison with yttria stabilized zirconia (8 mol% Y2O3 (-) ZrO2, YSZ). To maintain high ionic conductivity and improve the stability of the electrolyte, layered structures with YSZ outer layers and SCSZ inner layers were designed, along with the...
Show moreScandia and ceria stabilized zirconia (10 mol% Sc2O3 (-) 1 mol% CeO2 (-) ZrO2, SCSZ) has superior ionic conductivity in the intermediate temperature range for the operation of solid oxide fuel cells, but it does not exhibit good phase stability in comparison with yttria stabilized zirconia (8 mol% Y2O3 (-) ZrO2, YSZ). To maintain high ionic conductivity and improve the stability of the electrolyte, layered structures with YSZ outer layers and SCSZ inner layers were designed, along with the referential electrolytes containing pure SCSZ or YSZ. The electrolytes were manufactured by tape casting, laminating, and pressureless sintering techniques. After sintering, while the thickness of YSZ outer layers remained constant at ~30 ?m, the thickness of inner layers of SCSZ for the 3-, 4- and 6-layer designs varied at ~30, ~60 and ~120 ?m, respectively. Selected characterizations were employed to study the structure, morphology, impurity content and the density of the electrolytes. Furthermore, in situ X-ray diffraction, neutron diffraction and Raman scattering were carried out to study the phase transition and lattice distortion during long-term annealing at 350 (&)deg;C and 275 (&)deg;C for SCSZ and YSZ, respectively, where the dynamic damping occurred when Young's modulus was measured.In YSZ/SCSZ electrolytes, thermal residual stresses and strains were generated due to the mismatch of coefficients of thermal expansion from each layer of different compositions. They could be adjusted by varying the thickness ratios of each layer in different designs of laminates. The theoretical residual stresses have been calculated for different thickness ratios. The effect of thermal residual stress on the biaxial flexural strength was studied in layered electrolytes. The biaxial flexure tests of electrolytes with various layered designs were performed using a ring-on-ring method at both room temperature and 800 (&)deg;C. The maximum principal stress during fracture indicated an increase of flexural strength in the electrolytes with layered structure at both temperatures in comparison with the electrolytes without compositional gradient. Such an increase of strength is the result of the existence of residual compressive stresses in the outer YSZ layer. In addition, Weibull statistics of the strength values were built for the layered electrolytes tested at room temperature, and the effect of thermal residual stresses on Weibull distribution was established. The calculation of residual stress present at the outer layers was verified. The high ionic conductivity was maintained with layered electrolyte designs in the intermediate temperature range. It was also established that the ionic conductivity of layered electrolytes exhibited 7% (-) 11% improvement at 800 (&)deg;C due to the stress/strain effects, and the largest improvements in a certain electrolyte was found to nearly coincide with the largest residual compressive strain in the outer YSZ layer.In addition to the study of layered electrolytes, mechanical properties of porous Ni/SCSZ cermet were studied. The anode materials were reduced by 65 wt% NiO (-) 35 wt% SCSZ (N65) and 50 wt% NiO (-) 50 wt% SCSZ (N50) porous ceramics in the forming gas. Young's modulus as well as strength and fracture toughness of non-reduced and reduced anodes has been measured, both at room and high temperatures. High temperature experiments were performed in the reducing environment of forming gas. It was shown that while at 700 (&)deg;C and 800 (&)deg;C the anode specimens exhibited purely brittle deformation, a brittle-to-ductile transition occurred at 800 (-) 900 (&)deg;C, and the anode deformed plastically at 900 (&)deg;C. Fractography of the anode specimens were studied to identify the fracture modes of the anodes tested at different temperatures.
Show less - Date Issued
- 2013
- Identifier
- CFE0005090, ucf:50750
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0005090
- Title
- A multi-scale approach to study Solid Oxide Fuel Cells: from Mechanical Properties and Crystal Structure of the Cell's Materials to the Development of an Interactive and Interconnected Educational Tool.
- Creator
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Aman, Amjad, Orlovskaya, Nina, Xu, Yunjun, Das, Tuhin, University of Central Florida
- Abstract / Description
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Solid Oxide Fuel Cells are energy conversion devices that convert chemical energy of a fuel directly into electrical energy. They are known for being fuel-flexible, have minimal harmful emissions, ideal for combined heat and power applications, highly energy-efficient when combined with gas or steam turbines. The current challenges facing the widespread adoption these fuel cells include cost reduction, long-term testing of fully integrated systems, improving the fuel cell stack and system...
Show moreSolid Oxide Fuel Cells are energy conversion devices that convert chemical energy of a fuel directly into electrical energy. They are known for being fuel-flexible, have minimal harmful emissions, ideal for combined heat and power applications, highly energy-efficient when combined with gas or steam turbines. The current challenges facing the widespread adoption these fuel cells include cost reduction, long-term testing of fully integrated systems, improving the fuel cell stack and system performance, and studies related to reliability, robustness and durability. The goal of this dissertation is to further the understanding of the mechanical properties and crystal structure of materials used in the cathode and electrolyte of solid oxide fuel cells, as well as to report on the development of a supplementary educational tool that could be used in course related to fuel cells. The first part of the dissertation relates to the study of LaCoO3 based perovskites that are used as cathode material in solid oxide fuel cells and in other energy-related applications. In-situ neutron diffraction of LaCoO3 perovskite during uniaxial compression was carried out to study crystal structure evolution and texture development. In this study, LaCoO3 was subjected to two cycles of uniaxial loading and unloading with the maximum stress value being 700-900 MPa. The in-situ neutron diffraction revealed the dynamic crystallographic changes occurring which is responsible for the non-linear ferroelastic deformation and the appearance of hysteresis in LaCoO3. At the end of the first cycle, irreversible strain was observed even after the load was removed, which is caused by non-recoverable domain reorientation and texture development. At the end of the second cycle, however, no irreversible strain was observed as domain reorientation seemed fully recovered. Elastic constants were calculated and Young's modulus was estimated for LaCoO3 single crystals oriented along different crystallographic directions. The high temperature mechanical behavior study of LaCoO3 based perovskites is also of prime importance as solid oxide fuel cells operate at high temperatures. Incidentally, it was observed that as opposed to the behavior of most materials, LaCoO3 exhibits stiffening between 700 oC to 900 oC, with the Young's modulus going from a value of ~76 GPa at room temperature to ~120 GPa at 900 oC. In-situ neutron diffraction, XRD and Raman spectroscopy were used to study structural changes occurring in the material as it was heated. The results from these experiments will be discussed.The next portion of the dissertation will focus on electrolytes. Numerical simulation was carried out in order to predict the non-linear load-stress relationship and estimation of biaxial flexure strength in layered electrolytes, during ring-on-ring mechanical testing.Finally, the development of an interactive and inter-connected educational software is presented that could serve as a supplementary tool to teach fuel cell related topics.
Show less - Date Issued
- 2016
- Identifier
- CFE0006436, ucf:51467
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0006436
- Title
- DIFFRACTION STUDIES OF DEFORMATION IN SHAPE MEMORY ALLOYS AND SELECTED ENGINEERING COMPONENTS.
- Creator
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RATHOD, CHANDRASEN, Vaidyanathan, Raj, University of Central Florida
- Abstract / Description
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Deformation phenomena in shape memory alloys involve stress-, temperature-induced phase transformations and crystallographic variant conversion or reorientation, equivalent to a twinning operation. In near equiatomic NiTi, Ti rich compositions can exist near room temperature as a monoclinic B19' martensitic phase, which when deformed undergoes twinning resulting in strains as large as 8%. Upon heating, the martensite transforms to a cubic B2 austenitic phase, thereby recovering the strain and...
Show moreDeformation phenomena in shape memory alloys involve stress-, temperature-induced phase transformations and crystallographic variant conversion or reorientation, equivalent to a twinning operation. In near equiatomic NiTi, Ti rich compositions can exist near room temperature as a monoclinic B19' martensitic phase, which when deformed undergoes twinning resulting in strains as large as 8%. Upon heating, the martensite transforms to a cubic B2 austenitic phase, thereby recovering the strain and exhibiting the shape memory effect. Ni rich compositions on the other hand can exist near room temperature in the austenitic phase and undergo a reversible martensitic transformation on application of stress. Associated with this reversible martensitic transformation are macroscopic strains, again as large as 8%, which are also recovered and resulting in superelasticity. This work primarily focuses on neutron diffraction measurements during loading at the Los Alamos Neutron Science Center at Los Alamos National Laboratory. Three phenomena were investigated: First, the phenomena of hysteresis reduction and increase in linearity with increasing plastic deformation in superelastic NiTi. There is usually a hysteresis associated with the forward and reverse transformations in superelastic NiTi which translates to a hysteresis in the stress-strain curve during loading and unloading. This hysteresis is reduced in cold-worked NiTi and the macroscopic stress-strain response is more linear. This work reports on measurements during loading and unloading in plastically deformed (up to 11%) and cycled NiTi. Second, the tension-compression stress-strain asymmetry in martensitic NiTi. This work reports on measurements during tensile and compressive loading of polycrystalline shape-memory martensitic NiTi with no starting texture. Third, a heterogeneous stress-induced phase transformation in superelastic NiTi. Measurements were performed on a NiTi disc specimen loaded laterally in compression and associated with a macroscopically heterogeneous stress state. For the case of superelastic NiTi, the experiments related the macroscopic stress-strain behavior (from an extensometer or an analytical approach) with the texture, phase volume fraction and strain evolution (from neutron diffraction spectra). For the case of shape memory NiTi, the macroscopic connection was made with the texture and strain evolution due to twinning and elastic deformation in martensitic NiTi. In all cases, this work provided for the first time insight into atomic-scale phenomena such as mismatch accommodation and martensite variant selection. The aforementioned technique of neutron diffraction for mechanical characterization was also extended to engineering components and focused mainly on the determination of residual strains. Two samples were investigated and presented in this work; first, a welded INCONEL 718 NASA space shuttle flow liner was studied at 135 K and second, Ti-6Al-4V turbine blade components were investigated for Siemens Westinghouse Power Corporation. Lastly, also reported in this dissertation is a refinement of the methodology established in the author's masters thesis at UCF that used synchrotron x-ray diffraction during loading to study superelastic NiTi. The Los Alamos Neutron Science Center is a national user facility funded by the United States Department of Energy, Office of Basic Energy Sciences, under Contract No. W-7405-ENG-36. The work reported here was made possible by grants to UCF from NASA (NAG3-2751), NSF CAREER (DMR-0239512), Siemens Westinghouse Power Corporation and the Space Research Initiative.
Show less - Date Issued
- 2005
- Identifier
- CFE0000723, ucf:46608
- Format
- Document (PDF)
- PURL
- http://purl.flvc.org/ucf/fd/CFE0000723