Corrosion resistance of a Nitinol ocular microstent: Implications on biocompatibility.

Nitinol is commonly used in medical implants due to its unique thermomechanical properties of shape memory and superelasticity. Free nickel has the potential to induce biological responses that may be a concern for permanent implants manufactured from nickel-containing alloys. Although there are extensive reports on the effects of surface treatments on corrosion behavior in cardiovascular Nitinol implants, there is a lack of data on corrosion resistance and impact on biocompatibility for ocular implants. Therefore, the objective of this study was to determine localized corrosion and nickel elution resistance of an electropolished Nitinol-based ocular device (Hydrus Microstent, Ivantis, Inc.) intended for patients with primary open angle glaucoma. Pitting corrosion susceptibility was characterized by potentiodynamic polarization testing per ASTM F2129. In addition, nickel ion release was quantified with immersion testing to 63 days. The results indicated high localized corrosion resistance as all samples reached polarization potentials of 800 mV without pitting initiation. Maximum nickel elution rates per device were less than approximately 1.1 ng/device/day after the first day of immersion and reduced to less than 0.1 ng/device/day after 7 days. For a patient with bilateral microstents, these nickel concentrations are ×10,000 lower than previously published tolerable intake levels for systemic toxicity. Overall, these corrosion results are in good agreement with literature values of well processed and biocompatible Nitinol devices indicating adverse systemic biological responses are not expected in vivo.

A statistical approach to understand the role of inclusions on the fatigue resistance of superelastic Nitinol wire and tubing.

Superelastic wires and diamond-shaped stent surrogates were manufactured from Nitinol rods and tubing, respectively, from five different mill product suppliers - Standard VAR, Standard VIM, Standard VIM+VAR, Process-Optimized VIM+VAR, and High-Purity VAR. High-cycle fatigue tests up to 10(7) cycles were conducted under tension-tension conditions for wires and bending conditions for diamonds. These materials were compared under both testing methods at 37°C with 6% prestrain and 3% mean strain (unloading plateau) with a range of alternating strains. The High-Purity VAR material outperformed all alloys tested with a measured 10(7)-fatigue alternating strain limit of 0.32% for wire and 1.75% for diamonds. Process-Optimized VIM+VAR material was only slightly inferior to the High Purity VAR with a diamond alternating bending strain limit of 1.5%. These two "second generation" Nitinol alloys demonstrated approximately a 2× increase in 10(7)-cycle fatigue strain limit compared to all of the Standard-grade Nitinol alloys (VAR, VIM, and VIM+VAR) that demonstrated virtually indistinguishable fatigue performance. This statistically-significant increase in fatigue resistance in the contemporary alloys is ascribed to smaller inclusions in the Process-Optimized VIM+VAR material, and both smaller and fewer inclusions in the High-Purity VAR Nitinol.

High compressive pre-strains reduce the bending fatigue life of nitinol wire.

Prior to implantation, Nitinol-based transcatheter endovascular devices are subject to a complex thermo-mechanical pre-strain associated with constraint onto a delivery catheter, device sterilization, and final deployment. Though such large thermo-mechanical excursions are known to impact the microstructural and mechanical properties of Nitinol, their effect on fatigue properties is still not well understood. The present study investigated the effects of large thermo-mechanical pre-strains on the fatigue of pseudoelastic Nitinol wire using fully reversed rotary bend fatigue (RBF) experiments. Electropolished Nitinol wires were subjected to a 0%, 8% or 10% bending pre-strain and RBF testing at 0.3-1.5% strain amplitudes for up to 10(8) cycles. The imposition of 8% or 10% bending pre-strain resulted in residual set in the wire. Large pre-strains also significantly reduced the fatigue life of Nitinol wires below 0.8% strain amplitude. While 0% and 8% pre-strain wires exhibited distinct low-cycle and high-cycle fatigue regions, reaching run out at 10(8) cycles at 0.6% and 0.4% strain amplitude, respectively, 10% pre-strain wires continued to fracture at less than 10(5) cycles, even at 0.3% strain amplitude. Furthermore, over 70% fatigue cracks were found to initiate on the compressive pre-strain surface in pre-strained wires. In light of the texture-dependent tension-compression asymmetry in Nitinol, this reduction in fatigue life and preferential crack initiation in pre-strained wires is thought to be attributed to compressive pre-strain-induced plasticity and tensile residual stresses as well as the formation of martensite variants. Despite differences in fatigue life, SEM revealed that the size, shape and morphology of the fatigue fracture surfaces were comparable across the pre-strain levels. Further, the mechanisms underlying fatigue were found to be similar; despite large differences in cycles to failure across strain amplitudes and pre-strain levels, cracks initiated from surface inclusions in nearly all wires. Compressive pre-strain-induced damage may accelerate such crack initiation, thereby reducing fatigue life. The results of the present study indicate that large compressive pre-strains are detrimental to the fatigue properties of Nitinol, and, taken together, the findings underscore the importance of accounting for thermo-mechanical history in the design and testing of wire-based percutaneous implants.

Influence of microstructural purity on the bending fatigue behavior of VAR-melted superelastic Nitinol.

The bending fatigue resistance of commercially-available Standard versus High Purity Nitinol was evaluated at 3% mean strain and a range of strain amplitudes with the simple wire Z-specimen geometry. The Standard grade Nitinol demonstrated a 10(7)-cycle fatigue strain limit of 0.50% alternating strain, comparable to results reported elsewhere in the literature. Conversely, the High Purity grade VAR Nitinol demonstrated a 5-fold improvement in fatigue resistance with an impressive 10(7)-cycle fatigue strain limit of 2.5% alternating strain. The High Purity Nitinol has an oxygen+nitrogen content of 60wppm, maximum wrought-material inclusion length of 17µm, and inclusion volume fraction of 0.28%, all substantially less than industry standards. With all processing variables held constant except for inclusion content, it is clear that this marked fatigue superiority is due exclusively to the reduction in both size and area fraction of inclusions.

An equivalent strain/Coffin-Manson approach to multiaxial fatigue and life prediction in superelastic Nitinol medical devices.

Medical devices, particularly endovascular stents, manufactured from superelastic Nitinol, a near-equiatomic alloy of Ni and Ti, are subjected to complex mixed-mode loading conditions in vivo, including axial tension and compression, radial compression, pulsatile, bending and torsion. Fatigue lifetime prediction methodologies for Nitinol, however, are invariably based on uniaxial loading and thus fall short of accurately predicting the safe lifetime of stents under the complex multiaxial loading conditions experienced physiologically. While there is a considerable body of research documented on the cyclic fatigue of Nitinol in uniaxial tension or bending, there remains an almost total lack of comprehensive fatigue lifetime data for other loading conditions, such as torsion and tension/torsion. In this work, thin-walled Nitinol tubes were cycled in torsion at various mean and alternating strains to investigate the fatigue life behavior of Nitinol and results compared to equivalent fatigue data collected under uniaxial tensile/bending loads. Using these strain-life results for various loading modes and an equivalent referential (Lagrangian) strain approach, a strategy for normalizing these data is presented. Based on this strategy, a fatigue lifetime prediction model for the multiaxial loading of Nitinol is presented utilizing a modified Coffin-Manson approach where the number of cycles to failure is related to the equivalent alternating transformation strain.