Pure platinum was probed with a nanoindenter fitted with a Berkovich tip to various depths. The indent pattern was made on the as-polished specimen prior to heat treating, after heat treating at 500 °C for 30 min, and again after further heat treating at 1000 °C for 30 min. The variability in the measured hardness decreased as the indentation depth increased from 50 to 300 nm. When the sampled was annealed, the hardness variation was also greater. Increasing hardness variation with decreasing dislocation density and sampling volume indicates that dislocation density plays a critical role in the observed variation, beyond solely instrumentation uncertainty, and supports a defect-based explanation for the stochastic behavior. It appears that the stochastic behavior occurs when multiple dislocations are present in the sampled volume rather than sampling only a single dislocation.

Atomistic simulations of nanoindentation tests were used to study the indenter radius size effect in the presence of vacancies in a (111) single crystal of nickel. For radii from 2 nm to 8 nm, the maximum shear stresses under the indenter at the onset of plastic deformation in crystals with vacancies were compared to those which cause yield in perfect crystals by placing a single vacancy in a position near the maximum shear stress underneath the indenter tip. The effect of the presence of vacancies is lowered by decreasing the indenter radius. Results obtained for several random distributions of vacancies, in the range 3.3e-4 to 0.0033, show that placing a single vacancy near a specific location produces similar results as using larger numbers of vacancies while simplifying the complexity of the simulation. Finally, visualizations of atomic configurations of a single crystal with vacancy concentration of 3.3e-4 for radii of 4 nm and 6nm show that the heterogeneous nucleation is a size dependent phenomenon.

An experimental study of the elastic and plastic properties of sucrose single crystals, which can be considered to be a model material for both pharmaceutical excipients and explosives, has been carried out using nanoindentation. Instrumented indentation was used to characterize the properties of both habit and cleavage planes on the (100) and (001) orientations; the elastic modulus on the (100) is 38 GPa, while the modulus on the (001) is 33 GPa. The hardness of sucrose is approximately 1.5 GPa. Nanoindentation enables assessment of the onset of plastic deformation on cleaved surfaces, and a maximum shear stress of 1 GPa can be supported prior to plastic deformation. The deformation in this material is crystallographically dependent, with pileup around residual indentation impressions showing evidence of preferential slip system activity.

Dislocation nucleation in solid solutions of face-centered-cubic metallic materials was studied using nanoindentation. The effects of solute impurities in the copper–nickel system on the formation of dislocations in a previously dislocation-free region were demonstrated to be minimal. The shear stress required to nucleate dislocations in copper is approximately 1.6 GPa, while in nickel a 3.9 GPa shear stress is required. Changes in shear stress for nucleation track closely with changes in elastic modulus showing the nucleation stress is approximately 1/30 to 1/20 of the shear modulus. The expected solid-solution strengthening is identified within the same experimental method, demonstrating unambiguously the fact that solid-solution impurities in this system will impact the propagation of dislocations during plastic deformation but not alter the homogeneous nucleation of dislocations in these materials.

The mechanical properties of thermally grown oxide films on various aluminum substrates were tested using nanoindentation. A sudden discontinuity, indicative of film fracture, was observed upon loading portion of the load–depth curve. The 63-nm-thick films were determined to have ultimate strengths between 4.8 and 8.9 GPa. The ultimate stress is a superposition of the bending and membrane stress. The stress intensity at fracture for each of the films was developed by approximating the resulting bending moment and various cracks sizes. At a constant ratio of crack size to oxide thickness of 0.3, the applied stress intensity at fracture of these aluminum oxide films were between 0.46 and 1.20 MPa m1/2. The residual stress in the film was assumed to be negligible in the stress intensity calculation.

Piezoelectric materials convert mechanical to electrical energy under stretching and bending conditions. Optimizing the coupling conversion is imperative to the electromechanical behavior of a micromachined membrane's performance. This paper discusses analytical calculations that were devised to determine the microscale structure that minimizes residual stress and outlines the implementation of fabrication technique variations including three different electrode configurations, trenching around the membrane, and reducing the total composite residual stress of the support structure using compressive silicon oxide. Lead zirconacte titanate (PZT) films between 1 and 3 μm thick with a ratio of Zr to Ti of 40:60 were deposited onto 3 mm square silicon membranes. The total tensile stress in the composite structure reaches 100 MPa during standard fabrication processing. Utilizing analytical calculations, a structure was determined that lowered the residual stress of the composite to 11 MPa and increased the electromechanical coupling 35 times. Changing the geometry of the electrode coverage decreased the residual stress of the composite by 40%. Trenching around the membrane provided a membrane with boundary conditions that approached simply supported and decreased the composite residual stress by another 16%. A comparison of the electromechanical behavior for these structures will be discussed, showing a route towards increasing electromechanical coupling in PZT MEMS.

Understanding the hardening response of small volumes is necessary to completely explain the mechanical properties of thin films and nanostructures. This experimental study deals with the deformation and hardening response in gold and copper films ranging in thickness from 10 to 400 nm and silicon nanoparticles with particle diameters less than 100 nm. For very thin films of both gold and copper, it was found that hardness initially decreases from about 2.5 to 1.5 GPa with increasing penetration depth. Thereafter, an increase occurs with depths beyond about 5–10% of the film thickness. It is proposed that the observed minima are produced by two competing mechanisms. It is shown that for relatively deep penetrations, a dislocation back stress argument reasonably explains the material hardening behavior unrelated to any substrate composite effect. Then, for shallow contacts, a volume-to-surface length scale argument relating to an indentation size effect is hypothesized. A simple model based on the superposition of these two mechanisms provides a reasonable fit to the experimental nanoindentation data.

This study used nanoindentation coupled with stressed overlayers to evaluate the effect of titanium interlayers on the interfacial fracture energy of platinum films on SiO2 substrates. Interfacial fracture energy was calculated three ways: from platinum buckles that formed spontaneously upon deposition of the film, from buckles that formed upon deposition of a stressed tungsten overlayer, and from blisters triggered by indentation of a platinum film with a tungsten stressed overlayer. The calculated values for the interfacial fracture energy of the Pt-SiO2 interface were 0.2 and 0.5 J/m2 for indentation blisters and spontaneous buckles, respectively. The effect of a titanium interlayer on adhesion was examined using a tungsten stressed overlayer coupled with nanoindentation. The addition of a titanium layer improved the adhesion of the platinum film on SiO2 from 0.2 to 1.0 J/m2.

The mechanical properties of monolayer and multilayer structures of several symmetrically substituted alkoxy copper phthalocyanine, CuPc(OR)8, Langmuir–Blodgett (LB) films were evaluated. One-dimensional compliance of the monolayers was determined from the slopes of the surface pressure–area isotherms. Multilayers were examined using a SPM and a commercial nanoindentation system. The nanomechanical studies show a distinct relationship between the position and length of alkoxy substituents on the Pc macrocycle and the LB film elasticity and hardness. The phthalocyanine complexes with peripheral octabutoxy and octaoctyloxy substituents form stiff LB monolayers and multilayers. The nonperipheral alkoxy derivetized CuPc films were less stiff. For monolayer films, it appears that the extent of π-π interaction determines the strength of the film. In multilayers, significant additional stability can be imparted through interdigitation of long paraffinic chains which play a significant role in determining the interlayer structure of the LB layers.

A summer Research Experience for Undergraduate (REU) site program has been operating at Washington State University for the past five summers. Over this time we have experimented with several modes of organized summer research methods, including students working in individual projects as well as students working in teams. We have balanced the academic standing of the students (freshmen to seniors), as well providing a diverse demographic background. The results of these past five summers will be presented, as well as recommendations for which methods have been the most successful in terms of generating publications and presentations from the students as well as the likelihood of students entering graduate school.

The effect of chemical etching on the surface roughness and fracture strength of Nd:yttrium-aluminum-garnet single crystals was investigated. Etching the laser host material in a 1:1 mixture of concentrated sulfuric and phosphoric acid at elevated temperatures enabled material removal from the surface of laser rods cored from single-crystal boules. The roughness on the rod surface increased from the as-drilled condition after etching, but after 17 μm of material was removed, the roughness remained approximately constant. The modulus of rupture increased from 133-530 MPa when 87 μm of material was removed by the chemical etching procedure.

Grain size can be controlled by varying the process conditions used to deposit the film and post growth processing. This study examines how the grain size will impact the mechanical properties, hardness and adhesion, of thin ductile films on brittle substrates. The grain structures of copper and tin films were examined using OIM and AFM. The interfacial fracture toughness of each film was calculated using a tungsten overlayer and mechanics based models. The hardnesses of the films were correlated to the measured interfacial fracture toughness, and demonstrate that increased hardness correlates to an increased sensitivity to the Mode II component of loading.

Flexing piezoelectric membranes can be used to convert mechanical energy to electrical energy. The overall deflection of individual membranes is impacted by the residual stress in the system. Membranes comprised of silicon dioxide, Ti/Pt, lead- zirconate- titanate (PZT), and TiW/Au layers deposited on a micromachined boron doped silicon wafer were examined for both morphology and residual stress. By characterizing the membrane residual stress induced during processing with x-ray diffraction, wafer curvature, and bulge testing and identifying methods to reduce stress, the membrane performance and reliability can be optimized. For Zr:Ti ratios of 52:48, the residual stress in the PZT was 350 MPa tensile, with an overall effective stress in the composite membrane of 150 MPa. A reduction of stress was accomplished by changing the PZT chemistry to 40:60 Zr:Ti in the PZT to obtain a stress in the PZT of 160 MPa tensile and an overall effective membrane stress of 100 MPa. The crystallization of the 52:48 PZT film at 700 °C causes a 28% reduction in the thickness of the film.

PZT films between 1 and 3 μm thick were grown using solution deposition techniques to study the effects of crystal structure, orientation, chemistry and PZT/PZT crystallization interfaces on the piezoelectric output of these films. By varying the chemistry of the film from Zr-rich to Ti-rich the film orientation increased towards {h00}. PZT with 60 wt% Ti exhibited tetragonality and produced greater electrical output at a given strain than the rhombohedral films with concentrations less than 50 wt% Ti. Multiple steps of solution deposition left identifiable PZT/PZT interfaces within the film. TEM, FESEM, and Auger spectroscopy were used to characterize these interfaces, which form upon crystallization of the amorphous PZT film. Internal PZT interfaces are associated with both structural defects (voids) as well as chemical variations such as Pb deficiencies.

Thin films of lead zirconate titanate (PZT) are currently being used in a novel MEMS device to generate power. A piezoelectric stack consisting of platinum/PZT/gold is deposited by sputtering, spin coating, and subsequent heat treatments onto a thin silicon membrane, which is cyclically polarized by a flexing motion. The membrane must withstand strains between 0.1% and 0.5% for several billion cycles to provide a useful device. This study has examined the processing-structure-property relationships in developing the PZT film for use in this device. In the sol-gel deposition of PZT, pyrolysis and crystallization temperatures have been shown to alter both microstructure and properties of the piezoelectric film. The chemistry of the PZT film has also been tailored to increase piezoelectric output for this device. Ferroelectric properties are compared to the piezoelectric outputs, and fatigue behavior is measured on bulk silicon and on membranes.

The P3 Micro Heat Engine relies on a thin film PZT based transducer to convert mechanical energy into usable electrical power. In an effort to increase process yield for these were used on sputtered Ti/Pt bottom electrodes to compare roughness, grain size, and diffusion for annealing temperatures between 550 and 700 °C. For an optimized bottom electrode, process yield for various sized top electrodes were then studied for PZT thickness between 0.54 and 1.62 for reducing stress concentrations. Two PZT etching geometries on 2.3 μm thick Si/SiO2 membranes, with 1.5-3.5 mm side-lengths, were examined and one was used to increase the strain at failure by at least 40%. Integrating improvements in process yield and strain at failure, single PZT based MEMS devices capable of generating power of up to 1 mW and in excess of 2 volts have been demonstrated operating at frequencies between 300 and 1,100 Hz.

Piezoelectric oxide films, such as lead zirconate titanate (PZT), are now being integrated into MEMS applications. Many PZT derived systems are deposited using a sol-gel process, which can be used in a microelectronics processing route using spin coating as the deposition method. An application of interest for PZT films is in power generation, where a flexing membrane is used to transform mechanical to electrical energy. The current study was undertaken to identify the relationships between the processing, microstructure, and mechanical reliability of these films. Films were deposited onto both monolithic and bulk micromachined platinized silicon wafers using standard sol-gel chemistries, with roughness and grain size tracked using electron and scanning probe microscopy. Mechanical properties were evaluated in a dynamic bulge testing apparatus. Grain size variations in the Pt film between 35 and 125 nm are shown to have little effect on grain size of the subsequent PZT film and the adhesion of the PZT to the Pt film. Only the Pt film with 125 nm grains was shown to undergo any significant interfacial fracture. Fatigue tests suggest film lifetime is primarily limited by the number of pre- existing flaws in the film from processing. Reducing the microcrack density has been shown to produce films and devices that fail at strains of 1.4% and have mechanical fatigue lifetimes in excess of 100 million cycles at strains simulating the operating conditions.

A piezoelectric thin film MEMS device for generating power from a novel heat engine which approaches a Carnot cycle has been developed. The structure of the underlying electrode and PZT thin film generator has been optimized for increased adhesion. Atomic force microscopy was used to track electrode grain size and roughness; generating grain sizes of approximately 100 and 200 nm in diameter and a roughness of about 14-20 nm provide substantial improvements in film adhesion over systems with smaller grains and smoother surfaces. This has led to the ability to operate the engine at frequencies between 10 and 1500 Hz. The system of interest (a fluid filled cavity sealed by a micromachined silicon membrane and the PZT film) shows increased deflections for a given pressure applied to the membrane at frequencies where the system resonates. By operating the system dynamically, it is possible to generate more than 2 V from a single generator structure.

Nanoindentation testing of hard film – soft substrate systems can exhibit permanent deformation prior to a yield excursion, indicating that the occurrence of this sudden discontinuity is predominantly controlled by the hard film cracking rather than dislocation nucleation and multiplication. In a previous paper, a model was developed to predict the mechanical response prior to hard film fracture. In the current study a this model, which superimposes large deflection of the hard film and plastic deformation of the substrate the model, is further refined by testing a variety of materials with different film formation conditions. The tested materials include anodic titanium oxide on titanium, thermal aluminum oxide on aluminum and sputtered tungsten films on aluminum. The film fracture strength of titanium oxides on titanium is estimated as 15 GPa and that of aluminum oxides on aluminum is around 10 GPa. In the case of vacuum sputtered tungsten film on aluminum, the tungsten layer is likely plastically deformed. The strain at film fracture is roughly estimated to be 3.4%.