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Actuator applications of shape memory alloys have typically been limited by their phase transformation temperatures to around 100 degrees C. However, recently with a focus on aerospace and turbomachinery applications there have been successful efforts to increase the phase transformation temperatures. Several of these alloy development efforts have involved ternary and quaternary elemental additions (e.g., Pt, Pd, etc.) to binary NiTi alloys. Experimentally assessing the effects of varying composition and thermo-mechanical processing parameters can be cost intensive, especially when expensive, high-purity elemental additions are involved. Thus, in order to save on development costs there is value in establishing a methodology that facilitates the fabrication, processing and testing of smaller specimens, rather than larger specimens from commercial billets. With the objective of establishing such a methodology, this work compares thermo-mechanical test results from bulk dog-bone tensile Ni29.5Ti50.5Pd20 samples (7.62 mm diameter) with that of thin wires (100 μm-150 µm diameter) extracted from comparable, untested bulk samples by wire electrical-discharge machining (EDM). The wires were subsequently electropolished to different cross-sections, characterized with Scanning Electron Microscopy, Transmission Electron Microscopy and Energy Dispersive X-Ray Spectroscopy to verify the removal of the heat affected zone following EDM and subjected to Laser Scanning Confocal Microscopy to accurately determine their cross-sections before thermo-mechanical testing. Stress-strain and load-bias experiments were then performed on these wires using a dynamic mechanical analyzer and compared with results established in iv previous studies for comparable bulk tensile specimens. On comparing the results from a bulk tensile sample with that of the micron-scale wires, the overall thermomechanical trends were accurately captured by the micron-scale wires for both the constrained recovery and monotonic tensile tests. Specifically, there was good agreement between the stress-strain response in both the martensitic and austenitic phases, the transformation strains at lower stresses in constrained recovery, and the transformation temperatures at higher stresses in constrained recovery. This work thus validated that carefully prepared micron-diameter samples can be used to obtain representative bulk thermo-mechanical properties, and is useful for fabricating and optimizing composition and thermomechanical processing parameters in prototype button melts prior to commercial production. This work additionally assesses potential applications of high temperature shape memory alloy actuator seals in turbomachinery. A concept for a shape memory alloy turbine labyrinth seal is also presented. Funding support from NASA’s Fundamental Aeronautics Program, Supersonics Project (NNX08AB51A) and Siemens Energy is acknowledged.

To date the commercial use of shape memory alloys (SMAs) has been mostly limited to binary NiTi alloys with transformation temperatures approximately in the -100 to 100 ºC range. In an ongoing effort to develop high-temperature shape memory alloys (HTSMAs), ternary and quaternary additions are being made to binary NiTi to form NiTi-X (e.g., X: Pd, Pt, Au and Hf) alloys. Stability and repeatability can be further increased at these higher temperatures by limiting the stress, but the tradeoff is reduced work output and stroke. However, HTSMAs operating at decreased stresses can still be used effectively in actuator applications that require large strokes when used in the form of springs. The overall objective of this work is to facilitate the development of HTSMAs for use as high-force actuators in active/adaptive aerospace structures. A modular test setup was assembled with the objective of acquiring stroke, stress, temperature and moment data in real time during joule heating and forced convective cooling of Ni19.5Ti50.5Pd25Pt5 HTSMA springs. The spring actuators were evaluated under both monotonic axial loading and thermomechanical cycling. The role of rotational constraints (i.e., by restricting rotation or allowing for free rotation at the ends of the springs) on stroke performance was also assessed. Recognizing that evolution in the material microstructure results in changes in geometry and vice versa in HTSMA springs, the objective of the present study also included assessing the contributions from the material microstructural evolution, by eliminating contributions from changes in geometry, to overall HTSMA spring performance. The finite element method (FEM) was used to support the analytical analyses and provided further insight into the behavior and heterogeneous stress states that exist in these spring actuators. iv Furthermore, with the goal of improving dimensional stability there is a need to better understand the microstructural evolution in HTSMAs that contributes to irrecoverable strains. Towards this goal, available Ni29.5Ti50.5Pd20 neutron diffraction data (from a comparable HTMSA alloy without the solid solution strengthening offered by the Pt addition) were analyzed. The data was obtained from in situ neutron diffraction experiments performed on Ni29.5Ti50.5Pd20 during compressive loading while heating/cooling, using the Spectrometer for Materials Research at Temperature and Stress (SMARTS) at Los Alamos National Laboratory. Specifically, in this work emphasis was placed on neutron diffraction data analysis via Rietveld refinement and capturing the texture evolution through inverse pole figures. Such analyses provided quantitative information on the evolution of lattice strain, phase volume fraction (including retained martensite that exists above the austenite finish temperature) and texture (martensite variant reorientation and detwinning) under temperature and stress. Financial support for this work from NASA’s Fundamental Aeronautics Program Supersonics Project (NNX08AB51A), Subsonic Fixed Wing Program (NNX11AI57A) and the Florida Center for Advanced Aero-Propulsion (FCAAP) is gratefully acknowledged. 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.

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As crucial infrastructure systems remain in service up to and beyond their originally intended service lives, there has been a significant increase in efforts to quantify their current strength and remaining life span. Suspension bridges are of particular concern due to their impact on commerce, low repairability, and high replacement cost. As such, quantification of the performance of suspension bridge main cables at elevated temperatures is necessary for a holistic safety assessment. These cables are the primary load-carrying members, and are susceptible to vehicular fires near the midspan and anchorage where the cable sweeps low to the deck. Due to the dearth of empirical data regarding the thermomechanical properties of main cables, previous studies were forced to rely on thermomechanical properties derived for different materials, geometries, and scales. It is the chief goal of this dissertation to fill this void in high-temperature empirical data. First, the high temperature stress-strain behavior of the constituent ASTM A586 wires is examined. The coldworked wires are highly susceptible to recovery at elevated temperatures, which has the power to undo the primary strengthening mechanism. Large decreases in elastic modulus, yield stress, and ultimate stress are observed at elevated temperature. The high temperature stress-strain curves are fully parameterized, and a procedure for generating stress-strain curves at temperatures between 22°C and 724°C is provided. Next, the post-fire performance of the wire is quantified. Wires are heated to various temperatures up to 842°C and then allowed to cool before being tensile tested. The results of this testing show that a significant portion of the high-temperature strength-loss observed in the in-situ tests persists after cool-down. Exposure to elevated temperatures reduces strength and fundamentally alters the shape of the stress-strain curves of the heated and cooled wires. These post-fire stress-strain curves are fully parameterized, and a procedure for recreating them between 22°C and 842°C is provided. Next, the metallurgical underpinnings for the observed changes in mechanical behavior at and after high-temperature exposure are explored using neutron diffraction techniques. Two engineering beamline experiments generate peak-narrowing data that sheds light on the evolving dislocation density and crystallite size in this wire during and after heating. Results confirm that the decreases in wire strength that persist after cool-down are the product of recovery; temperatures in excess of 700°C decrease wire dislocation density to values similar to those of undeformed structural materials. Finally, the thermal conductivity of the main cable is addressed. The air voids and point contacts between the wires create a complex (and anisotropic) heat transfer situation within main cables. A one-to-one, 8200 kg mock-up of a panel of a suspension bridge main cable is constructed, instrumented, and heated. The data provided by the internal temperature sensors is used to tune the thermal conductivity of a representative finite element via a gradient descent algorithm. The resulting temperature-dependent thermal conductivity function allows the complex internal heat transfer of the main cable to be accurately approximated by a monolithic section with conductivity tuned to the measured behavior of a physical main cable. Cumulatively, the results of these studies shows that the thermomechanical properties of main cables are not well represented by previous approximations that are based on other materials and applications. The properties derived herein will facilitate more accurate performance estimates of suspension bridges subjected to fires than previously possible.

Surface free energy of a polymer is of great importance in adhesive studies. Acid/base specific interactions play pertinent roles in adhesive bond performance and polymer-polymer miscibility. In this study, the correlation between the surface characteristics of two polymers and their adhesive bond behavior as well as the compatibility of their blend systems are investigated through both the surface characterizations and bulk examinations. Inverse Gas Chromatography (IGC) is employed to determine the surface free energies, the dispersive component and acid/base specific interactions, of polyethylene terephthalate (PET), cellulose acetate (CA) and their blend. Dynamic Contact Angle (DCA) measurements are performed to obtain the surface free energies of PET and CA so that they can be compared to that from IGC. Moreover, the DCA data are used to calculate their spreading coefficients and the adhesive bond behavior between PET and CA is predicted as well. The bulk examinations on specific interactions and the miscibility of the PET/CA , PBT/CA blends are completed through Fourior Transform Infrared-Diffuse Reflectance Spectroscopy (FTIR-DRIFT), Differential Scanning Calorimeter (DSC) and Dynamic Mechanical Analyzer (DMA). Scanning Electron Microscopy (SEM) micrographs of these blends are taken to examine their morphologies. From IGC, it is deterrnined that the surfaces of PET and CA are predominantly basic. The spreading coefficients calculated from DCA data indicate the poor adhesive bond between PET and CA. The bulk examinations reveal that both PET/CA and PBT/CA blends are immiscible systems. / Master of Science

Shape memory alloy (SMA) materials such as nitinol have unique properties associated with the shape recovery effect and the material’s phase changes that have been used in a variety of actuator and sensing applications. By embedding SMA elements into host composite materials, control or modification of the SMA hybrid composite’s structural properties can be accomplished in-service, thereby increasing the hybrid composite’s structural functionality. Previous studies addressed increasing composite materials’ functionality by enabling in-service control of their dynamic response. Utilizing the SMA’s substantial recovery stress and capacity to dissipate strain energy to increase the hybrid composite’s static functionality is addressed herein. Specific applications for SMA hybrid composites include improving composite material’s impact damage resistance and composite cylinder stress and deflection control. In stress and deflection control of cylindrical structures, SMA actuators are placed within the composite cylinder to form an active compound cylinder. The active SMA elements can significantly reduce the internal pressure-induced radial dilation and creep so that under severe loading, piston to cylinder tolerances may be maintained. Similar to a conventional metallic compound cylinder, the active compound cylinder also reduces peak cylinder hoop stresses. Hybridizing composites with nitinol improves their impact resistance because of nitinol’s tremendous capacity to absorb impact strain energy through the stress-induced martensitic phase transformation. The amount of impact damage is reduced and the material’s resistance to impact perforation at various velocities is improved. The experimental response of nitinol hybrid composites and the associated mechanics are presented. The unique toughness and resistance to permanent deformation that is a result of the stress-induced martensitic phase transformation enables the nitinol to absorb on the order of 4 times the strain energy of high alloy steel and 16 times that of many graphite/epoxy composites. In most static applications where SMA elements are used for reinforcement, maintaining the integrity of the interface between the SMA elements and the host polymeric matrix composite material is critical to operation. The relationship between preparation of SMA elements for hybrid composite fabrication and interfacial bond strength is presented to address this issue. The mechanics of interfacial shear failure between SMA element and composite is also presented. / Ph. D.

Hot sections of gas engine turbines require specialized materials to withstand extreme conditions present during engine operation. Nickel-base superalloys are typically used as blades and disks in the high pressure turbine section because they possess excellent fatigue strength, creep strength and corrosion resistance at elevated temperatures. Components undergo thermomechanical fatigue conditions as a result of transient engine operation. Sharp geometric features, such as cooling holes in blades or fir-tree connections in disks, act as local stress raisers. The material surrounding these features are potential sites of localized inelastic deformation and crack formation. To reduce customer costs associated with unnecessary overhauls or engine down-time, gas turbine manufacturers require accurate prediction methods to determine component endurances. The influence of stress concentration severity on thermomechanical fatigue crack formation is of particular importance as cracks often initiate in these hot spots. Circumferentially notched specimens were utilized to perform thermomechanical fatigue experiments on blade material CM247LC DS and disk material PM IN100. A parametric study on CM247LC DS was performed utilizing four notched specimens. Experimental results were coupled with finite element simulations utilizing continuum based constitutive models. The effects of applied boundary conditions on crack initiation life was studied in both alloys by performing experiments under remotely applied force and displacement boundary conditions. Finite element results were utilized to develop a life prediction method for notched components under thermomechanical fatigue conditions.

The exciting thermomechanical properties of nickel-titanium shape memory alloys have sparked significant research efforts seeking to exploit their exotic capabilities. Until recently, the performance capabilities of nickel-titanium devices have been inhibited by the retention of only one thermomechanical characteristic. However, laser processing technology promises to deliver enhanced material offerings which are capable of multiple functional responses. Presented in this thesis, is an investigation of the effects of laser processing on the thermomechanical behaviour of nickel-titanium shape memory alloys. In the context of this work, laser processing refers to removal of alloy constituents, as in the case of laser ablation, or alternatively, addition of elements through laser alloying. The effects of laser ablation on the composition, crystallography and phase transformation temperatures of a nickel-titanium strip have been studied. Application of laser energy was shown to ablate nickel constituents, induce an austenite-martensite phase change and cause an increase in phase transformation onset temperatures, which correlated well with reported findings. Laser processing of a nickel-titanium wire was shown to locally embed an additional thermomechanical response which manifested as unique shape memory and pseudoelastic properties. Localized alloying of ternary species via laser processing of nickel-titanium strip was investigated. Synthesis of a ternary shape memory intermetallic within the laser processing region was achieved through melting of copper foils. Results from thermoanalytical testing indicated that the ternary compound possessed a higher phase transformation temperature and reduced transformation hysteresis in comparison to the reference alloy. Indentation testing was used to demonstrate the augmented thermomechanical characteristics of the laser processed shape memory alloy. In order to demonstrate the enhanced functionality of laser processed nickel-titanium shape memory alloys, a self-positioning nickel-titanium microgripper was fabricated. The microgripper was designed to actuate through four different positions, corresponding to activation of three embedded shape memory characteristics. Thermoanalytical and tensile testing instrumentations were used to characterize the thermomechanical performance of the laser processed nickel-titanium microgripper. Results indicated that each of the laser processed microgripper components possessed unique mechanical and shape memory recovery properties.

The exciting thermomechanical properties of nickel-titanium shape memory alloys have sparked significant research efforts seeking to exploit their exotic capabilities. Until recently, the performance capabilities of nickel-titanium devices have been inhibited by the retention of only one thermomechanical characteristic. However, laser processing technology promises to deliver enhanced material offerings which are capable of multiple functional responses. Presented in this thesis, is an investigation of the effects of laser processing on the thermomechanical behaviour of nickel-titanium shape memory alloys. In the context of this work, laser processing refers to removal of alloy constituents, as in the case of laser ablation, or alternatively, addition of elements through laser alloying. The effects of laser ablation on the composition, crystallography and phase transformation temperatures of a nickel-titanium strip have been studied. Application of laser energy was shown to ablate nickel constituents, induce an austenite-martensite phase change and cause an increase in phase transformation onset temperatures, which correlated well with reported findings. Laser processing of a nickel-titanium wire was shown to locally embed an additional thermomechanical response which manifested as unique shape memory and pseudoelastic properties. Localized alloying of ternary species via laser processing of nickel-titanium strip was investigated. Synthesis of a ternary shape memory intermetallic within the laser processing region was achieved through melting of copper foils. Results from thermoanalytical testing indicated that the ternary compound possessed a higher phase transformation temperature and reduced transformation hysteresis in comparison to the reference alloy. Indentation testing was used to demonstrate the augmented thermomechanical characteristics of the laser processed shape memory alloy. In order to demonstrate the enhanced functionality of laser processed nickel-titanium shape memory alloys, a self-positioning nickel-titanium microgripper was fabricated. The microgripper was designed to actuate through four different positions, corresponding to activation of three embedded shape memory characteristics. Thermoanalytical and tensile testing instrumentations were used to characterize the thermomechanical performance of the laser processed nickel-titanium microgripper. Results indicated that each of the laser processed microgripper components possessed unique mechanical and shape memory recovery properties.