Titanium-nickel is a unique class of material known as Shape Memory Alloy (SMA). A thermoelastic martensitic phase transformation is responsible for its extraordinary properties such as shape memory effect and superelasticity. The near equiatomic Ti-Ni alloys are the commercially most exploited SMAs because of the unique combination of these properties and superior ductility, strength, fatigue resistance and corrosion resistance. The properties of Ti-Ni SMAs are very sensitive to composition and the processing parameters. The properties of Ti-Ni SMAs can be modified to a great extent by choice of composition, mechanical working and heat treatment. Thermo-mechanical treatments are required to strengthen the matrix and improve the shape memory characteristics. Plastic deformation and subsequent annealing is the common way to improve shape memory properties. In the present study, Ti- 50 at% Ni wire specimens are produced and used for the investigation of the effect of different heat treatment and cold working processes on shape memory characteristics. To investigate the thermomechanical behavior of differently processed wire specimens, a fully computerized servo hydraulic thermomechanical testing machine was designed and constructed. Testing machine was capable to perform different types of tests that are selected by the user. It can both heat and cool the specimen automatically according to the testing sequence by applying DC current directly through the SMA wire or by sending liquid nitrogen into the cooling chamber. Temperature is measured by a K-type thermocouple directly mounted on the wire specimen with a glass tape. Force that is applied to the specimen is produced by hydraulic power unit with a double action cyclinder and it is controlled by a controller which takes the feedback from the loadcell and LVDT (Linear Variable Distance Transducer). During performig thermomechanical-tests all the data of loadcell, LVDT and thermocouple are collected by a data acqusition system integrated with a host computer that operates the program XPC Target. Ti-Ni alloy with equiatomic composition is prepared in vacum induction furnace. Specimen cast in the form of rod was then hot swaged. Subsequent to swaging, cold wire drawing, intermediate annealing at 500 &amp / #61616 / C and water quenching was applied to obtain SMA wire with a diameter of 1.52 mm. Ti-Ni wires produced were subjected to four different processes. All the samples were initially solution heat treated at 925 &amp / #61616 / C for 30 minutes prior to water quenching. Some of the samples were further treated by an intermediate anneal at 500 &amp / #61616 / C. To see the effect of cold working / prior to intermediate annealing, 20 % or 40 % cold work was applied to another group of specimens. To study the shape memory characteristics of specimens subjected to the above mentioned processes, four types of test, namely constant stress free recovery test, constant strain free recovery test, constant stress constrained recovery test and constant strain constrained recovery test, were designed and applied cyclically. The tests have shown that the stress plateau observed in the first cycle of the tests disappear upon cycling and the shape memory characteristics improve and stabilize with cycling. Once trained by cycling, fractional free recovery was observed to reach to 100 % and recovery stress to reach 120% of the applied stress if shape recovery is prevented.

Porous TiNi alloys (Ti-50.4 at. %Ni and Ti-50.6 at. %Ni) with porosities in the range 21%-81% were prepared successfully applying a new powder metallurgy fabrication route in which magnesium was used as space holder resulting in either single austenite phase or a mixture of austenite and martensite phases dictated by the composition of the starting prealloyed powders but entirely free from secondary brittle intermetallics, oxides, nitrides and carbonitrides. Magnesium vapor do not only prevents secondary phase formation and contamination but also provides higher temperature sintering opportunity preventing liquid phase formation at the eutectic temperature, 1118 &deg / C resulting from Ni enrichment due to oxidation. By two step sintering processing (holding the sample at 1100 &deg / C for 30 minutes and subsequently sintering at temperatures higher than the eutectic temperature, 1118 &deg / C) magnesium may allow sintering probably up to the melting point of TiNi. The processed alloys exhibited interconnected (partially or completely depending on porosity content) open macro-pores spherical in shape and irregular micro-pores in the cell walls resulting from incomplete sintering. It has been found that porosity content of the foams have no influence on the phase transformation temperatures while deformation and oxidation are severely influential. Porous TiNi alloys displayed excellent superelasticity and shape memory behavior. Space holder technique seems to be a promising method for production of porous TiNi alloys. Desired porosity level, pore shape and accordingly mechanical properties were found to be easily adjustable.

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Shape memory alloys (SMAs) exhibit unique combination of structural and functional properties and hence have a variety of current and potential applications. The mechanical behaviour of SMAs, in particular the influence of processing on the microstructure, which in turn influences the performance of the alloy, mechanical properties at the nano-scale, and under cyclic loading conditions, are of great current interest. In this thesis, specific issues within each of these broad areas are examined with a view to suggest further optimize/characterize SMAs. They are the following: (a) For thermo-mechanical secondary processing of SMAs, can we identify the optimum combination of temperature- strain rate window that yields a desirable microstructure? (b) How can indentation be used to obtain information about functional properties of shape memory alloys so as to complement traditional methods? (c) How can the information obtained from indentation be utilized for the identification of the alloy composition that yields a high temperature SMA through the combinatorial diffusion couple approach? Towards achieving the first objective, we study the hot deformation behavior of a cast NiTi alloy with a view of controlling the final microstructure. The “processing maps” approach is used to identify the optimum combination of temperature and strain rate for the thermomechanical processing of a SMA system commonly used in actuators applications (NiTiCu). Uniaxial compressions experiments are conducted in the temperature range of 800- 1050 °C and at strain rate range of 10-3 and 102 s-1. 2-D power dissipation efficiency and instability maps are generated and various deformation mechanisms, which operate in different temperature–strain rate regimes, are identified with the aid of these maps. Complementary microstructural analysis of specimens (post deformation) is performed with the help of electron backscattered diffraction (EBSD) analysis to arrive at a processing route which produces stress free grains. A safe window suitable for industrial processing of this alloy which leads to grain refinement and strain-free grains (as calculated by various methods of misorientation analysis representation) is suggested. Regions of the instability (characterized by the same analysis) result in strained microstructure, which in turn can affect the performance of the SMA in a detrimental manner. Next, to extract useful information from indentation responses, microindentation experiments at a range of temperatures (as the shape memory transformation is in progress) are conducted underneath the Vickers indenter. SME was observed to cause a change in the calculated recovery ratios at temperatures above As. Spherical indentation of austenite and martensite show different characteristics in elastic and elasto- plastic regimes but are similar in the plastic regime. NanoECR experiments are also conducted under a spheroconical indenter at room temperature, where the resistance measured is observed to increase during the unloading of room temperature austenite SMA. This is a signature of the reverse transformation back to austenite during the withdrawal of the indenter. Lastly, recovery ratios are monitored in the case of a NiTiPd diffusion couple before and after heat treatment at different temperature intervals using non- contact optical profilometry. The recovery ratio approach is successfully used to determine the useful temperature and %Pd range for a potential NiTiPd high temperature SMA. The method makes high throughput identification of high temperature shape memory alloys possible due to promising alloy compositions being identified at an early stage.

This thesis presents methods for fabricating MicroElectroMechanical System (MEMS) actuators and high-flow gas microvalves using wafer-level integration of Shape Memory Alloys (SMAs) in the form of wires and sheets. The work output per volume of SMA actuators exceeds that of other microactuation mechanisms, such as electrostatic, magnetic and piezoelectric actuation, by more than an order of magnitude, making SMA actuators highly promising for applications requiring high forces and large displacements. The use of SMAs in MEMS has so far been limited, partially due to a lack of cost efficient and reliable wafer-level integration approaches. This thesis presents new methods for wafer-level integration of nickel-titanium SMA sheets and wires. For SMA sheets, a technique for the integration of patterned SMA sheets to silicon wafers using gold-silicon eutectic bonding is demonstrated. A method for selective release of gold-silicon eutectically bonded microstructures by localized electrochemical etching, is also presented. For SMA wires, alignment and placement of NiTi wires is demonstrated forboth a manual approach, using specially built wire frame tools, and a semiautomatic approach, using a commercially available wire bonder. Methods for fixing wires to wafers using either polymers, nickel electroplating or mechanical silicon clamps are also shown. Nickel electroplating offers the most promising permanent fixing technique, since both a strong mechanical and good electrical connection to the wire is achieved during the same process step. Resistively heated microactuators are also fabricated by integrating prestrained SMA wires onto silicon cantilevers. These microactuators exhibit displacements that are among the highest yet reported. The actuators also feature a relatively low power consumption and high reliability during longterm cycling. New designs for gas microvalves are presented and valves using both SMA sheets and SMA wires for actuation are fabricated. The SMA-sheet microvalve exhibits a pneumatic performance per footprint area, three times higher than that of previous microvalves. The SMA-wire-actuated microvalve also allows control of high gas flows and in addition, offers benefits of lowvoltage actuation and low overall power consumption. / QC 20120514

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This thesis presents methods for the wafer-level integration of shape memory alloy (SMA) and electrostatic actuators to functionalize MEMS devices. The integration methods are based on heterogeneous integration, which is the integration of different materials and technologies. Background information about the actuators and the integration method is provided. SMA microactuators offer the highest work density of all MEMS actuators, however, they are not yet a standard MEMS material, partially due to the lack of proper wafer-level integration methods. This thesis presents methods for the wafer-level heterogeneous integration of bulk SMA sheets and wires with silicon microstructures. First concepts and experiments are presented for integrating SMA actuators with knife gate microvalves, which are introduced in this thesis. These microvalves feature a gate moving out-of-plane to regulate a gas flow and first measurements indicate outstanding pneumatic performance in relation to the consumed silicon footprint area. This part of the work also includes a novel technique for the footprint and thickness independent selective release of Au-Si eutectically bonded microstructures based on localized electrochemical etching. Electrostatic actuators are presented to functionalize MEMS crossbar switches, which are intended for the automated reconfiguration of copper-wire telecommunication networks and must allow to interconnect a number of input lines to a number of output lines in any combination desired. Following the concepts of heterogeneous integration, the device is divided into two parts which are fabricated separately and then assembled. One part contains an array of double-pole single-throw S-shaped actuator MEMS switches. The other part contains a signal line routing network which is interconnected by the switches after assembly of the two parts. The assembly is based on patterned adhesive wafer bonding and results in wafer-level encapsulation of the switch array. During operation, the switches in these arrays must be individually addressable. Instead of controlling each element with individual control lines, this thesis investigates a row/column addressing scheme to individually pull in or pull out single electrostatic actuators in the array with maximum operational reliability, determined by the statistical parameters of the pull-in and pull-out characteristics of the actuators. / QC20100729