Tungsten (W) films have many applications in the semiconducting industry for sensor technology. Deposition conditions can significantly impact the resulting W films in terms of the phases present (α-BCC or β-A12), microstructural grain orientation (texture), and residual strain. Tilt-A-Whirl methodology has been employed for the evaluation of a W film showing both texture and residual strain. Sin2(ψ) analysis of the film was performed to quantify the strongly tensile in-plane strain (+0.476%) with an estimated in-plane tensile stress of ~1.9 GPa. The 3D dataset was also evaluated qualitatively via 3D visualization. Visualization of 3D texture/strain data poses challenges due to peak broadening resulting from defocusing of the beam at high ψ tilt angles. To address this issue, principal component analysis (PCA) was employed to diagnose, model, and remove the broadening component from the diffraction data. Evaluation of the raw data and subsequent corrected data (after removal of defocusing effects) has been performed through projection of the data into a virtual 3D environment (via CAD2VR software) to qualitatively detect the impact of residual strain on the observed pole figure.
Staruch, M.; Bennett, S.P.; Matis, B.R.; Baldwin, J.W.; Bussmann, K.; Gopman, D.B.; Kabanov, Y.; Lau, J.W.; Shull, R.D.; Langlois, Eric L.; Arrington, C.; Pillars, Jamin R.; Finkel, P.
Magnetostrictive Co77Fe23 films are fully suspended to produce free-standing, clamped-clamped, microbeam resonators. A negative or positive shift in the resonant frequency is observed for magnetic fields applied parallel or perpendicular to the length of the beam, respectively, confirming the magnetoelastic nature of the shift. Notably, the resonance shifts linearly with higher-bias fields oriented perpendicular to the beam's length. Domain imaging elucidates the distinction in the reversal processes along the easy and hard axes. Together, these results suggest that through modification of the magnetic anisotropy, the frequency shift and angular dependence can be tuned, producing highly magnetic-field-sensitive resonators.
The ability to track nuclear material is a challenge for resiliency of complex systems, e.g., harsh environments. RF tags, frequently used in national security applications, cannot be used for technological, operational, or safety reasons. Magnetic Smart Tags (MaST) is a novel tag technology based on magnetoelastic sensing that circumvents these issues. This technology is enabled by a new, cost-effective, batch manufacturing electrochemical deposition (ECD) process. This new advancement in fabrication enables multi-frequency tags capable of providing millions of possible codes for tag identification unlike existing theft deterrent tags that can convey only a single bit of information. Magnetostrictive 70% Co: 30% Fe was developed as the base alloy comprising the magnetoelastic resonator transduction element. Saturation magnetostriction, S , has been externally measured by the Naval Research Laboratory to be as high as 78 ppm. Description of a novel MEMS variable capacitive test structure is described for future measurements of this parameter.
Recent studies have shown the potential for nanocrystalline metals to possess excellent fatigue resistance compared to their coarse-grained counterparts. Although the mechanical properties of nanocrystalline metals are believed to be particularly susceptible to material defects, a systematic study of the effects of geometric discontinuities on their fatigue performance has not yet been performed. In the present work, nanocrystalline Ni-40 wt%Fe containing both intrinsic and extrinsic defects were tested in tension-tension fatigue. The defects were found to dramatically reduce the fatigue resistance, which was attributed to the relatively high notch sensitivity in the nanocrystalline material. Microstructural analysis within the crack-initiation zones underneath the defects revealed cyclically-induced abnormal grain growth (AGG) as a predominant deformation and crack initiation mechanism during high-cycle fatigue. The onset of AGG and the ensuing fracture is likely accelerated by the stress concentrations, resulting in the reduced fatigue resistance compared to the relatively defect-free counterparts.
Magnetostrictive CoFe films were investigated for use as magnetoelastic tags or sensors. The ability to electrodeposit these films enables batch fabrication processes to pattern a variety of geometries while controlling the film stoichiometry and crystallography. In current research looking at CoFe, improved magnetostriction was achieved using a co-sputtering, annealing, and quenching method1. Other current research has reported electrodeposited CoFe films using a sulfate based chemistry resulting in film compositions that are Fe rich in the range of Co0.3-0.4Fe0.7-0.6 and have problems of codeposition of undesirables that can have a negative impact on magnetic properties. The research presented here focused on maximizing magnetostriction at the optimal stoichiometry range of Co0.7-0.75Fe0.3-0.25, targeting the (fcc+bcc)/bcc phase boundary, and using a novel chemistry and plating parameters to deposit films without being limited to “line of sight” deposition.
The development of an electrodeposition process for cobalt/iron (CoFe) alloys with minimal oxygen concentration and controlled stoichiometry is necessary for the advancement of magnetostrictive device functionalities. CoFe alloy films were electrodeposited out of a novel chemistry onto copper test structures enabling magnetic displacement testing for magnetostriction calculations. Using a combination of additives that served as oxygen scavengers, grain refiners, and complexing agents in conjunction with a pulsed plating technique, CoFe films were synthesized at thicknesses as high as 10μm with less than 8 at% oxygen at a stoichiometry of 70-75% Co and 25-30% Fe. X-Ray diffraction (XRD) analysis confirmed that these films had a crystal structure consistent with 70% Co 30% Fe Wairuaite with a slight lattice contraction due to Co doping in the film. A novel characterization technique was used to measure the displacement of the CoFe films electrodeposited, as a function of applied magnetic bias, in order to determine the saturation magnetostriction (λS) of the material. With this chemistry and a tailored pulse plating regime, λS values as high as 172 ± 25ppm have been achieved. This is believed by the authors to be the highest reported value of magnetostriction for an electrodeposited CoFe film.
Using galvanostatic pulse deposition, we studied the factors influencing the quality of electroformed Bi1-xSbxnanowires with respect to composition, crystallinity, and preferred orientation for high thermoelectric performance. Two nonaqueous baths with different Sb salts were investigated. The Sb salts used played a major role in both crystalline quality and preferred orientations. Nanowire arrays electroformed using an SbI3-based chemistry were polycrystalline with no preferred orientation, whereas arrays electroformed from an SbCl3-based chemistry were strongly crystallographically textured with the desired trigonal orientation for optimal thermoelectric performance. From the SbCl3 bath, the electroformed nanowire arrays were optimized to have nanocompositional uniformity, with a nearly constant composition along the nanowire length. Nanowires harvested from the center of the array had an average composition of Bi0.75Sb0.25. However, the nanowire compositions were slightly enriched in Sb in a small region near the edges of the array, with the composition approaching Bi0.700.30.
Tin (Sn) whiskers are conductive Sn filaments that grow from Sn-plated surfaces, such as surface finishes on electronic packages. The phenomenon of Sn whiskering has become a concern in recent years due to requirements for lead (Pb)-free soldering and surface finishes in commercial electronics. Pure Sn finishes are more prone to whisker growth than their Sn-Pb counterparts and high profile failures due to whisker formation (causing short circuits) in space applications have been documented. At Sandia, Sn whiskers are of interest due to increased use of Pb-free commercial off-the-shelf (COTS) parts and possible future requirements for Pb-free solders and surface finishes in high-reliability microelectronics. Lead-free solders and surface finishes are currently being used or considered for several Sandia applications. Despite the long history of Sn whisker research and the recently renewed interest in this topic, a comprehensive understanding of whisker growth remains elusive. This report describes recent research on characterization of Sn whiskers with the aim of understanding the underlying whisker growth mechanism(s). The report is divided into four sections and an Appendix. In Section 1, the Sn plating process is summarized. Specifically, the Sn plating parameters that were successful in producing samples with whiskers will be reviewed. In Section 2, the scanning electron microscopy (SEM) of Sn whiskers and time-lapse SEM studies of whisker growth will be discussed. This discussion includes the characterization of straight as well as kinked whiskers. In Section 3, a detailed discussion is given of SEM/EBSD (electron backscatter diffraction) techniques developed to determine the crystallography of Sn whiskers. In Section 4, these SEM/EBSD methods are employed to determine the crystallography of Sn whiskers, with a statistically significant number of whiskers analyzed. This is the largest study of Sn whisker crystallography ever reported. This section includes a review of previous literature on Sn whisker crystallography. The overall texture of the Sn films was also analyzed by EBSD. Finally, a short Appendix is included at the end of this report, in which the X-Ray diffraction (XRD) results are discussed and compared to the EBSD analyses of the overall textures of the Sn films. Sections 2, 3, and 4 have been or will be submitted as stand-alone papers in peer-reviewed technical journals. A bibliography of recent Sandia Sn whisker publications and presentations is included at the end of the report.