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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Kinetic Investigation by Batch Processing of Film Growth during the Electrodeposition of Titanium from Ethaline

Titanium electrodeposition as a technological advance has been out of reach due to the poor film quality obtained when using previously developed methods. This study shows that the electrodeposition of Ti is possible and feasible from the deep eutectic solvent ethaline. Moreover, this study shows through batch analysis that this deposition has temperature-dependent aspects that alter the film deposition kinetics upon modest heating. This ultraviolet–visible spectroscopic study is highlighting the more facile reduction of Ti 4+ to Ti 3+ and then to Ti 2+ at elevated temperatures. Understanding the underlying kinetics of electrodeposition opens up new venues for the application of this important metal.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Microstructure-Based Estimation of Strength and Ductility Distributions for \(\alpha +\beta \) Titanium Alloys

Titanium alloys are processed to develop a wide range of microstructure configurations and therefore material properties. While these properties are typically measured experimentally, a framework for property prediction could greatly enhance alloy design and manufacturing. In this work, a microstructure-sensitive framework is presented for the prediction of strength and ductility as well as estimates of the bounds in variability for these properties. The framework explicitly considers distributions of microstructure via new approaches for instantiation of structure in synthetic samples. The parametric evaluation strategy, including the finite element simulation package FEpX, is used to create and test virtual polycrystalline samples to evaluate the variability bounds of mechanical properties in Ti-6Al-4V. Critical parameters for the property evaluation framework are provided by measurements of single crystal properties and advanced characterization of microstructure and slip system strengths in 2D and 3D. Property distributions for yield strength and ductility are presented, along with the validation and verification steps undertaken. Comparisons between strain localization and slip activity in virtual samples and in experimental grain-scale strain measurements are also discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Grain boundary slip – twin transmission in titanium

Here, using a combination of mechanical testing, scanning electron microscopy, and a unified crystal plasticity framework for discrete intragranular shear localization, we investigate intense, localized slip bands on prismatic planes and {10$\bar{1}$2} $\langle$$\bar{1}$011$\rangle$ tensile twins, and their transmission across the grain boundaries (GBs) in commercially pure titanium. The analyses show that the orientation and curvature of the GB influence the local stress fields at the GBs, and consequently, the slip/twin transmission across the boundary. In addition to host grain properties, neighboring grain properties, such as active slip systems and instances of heterogeneity like slip bands and twins, heavily affect the deformation mechanisms in each grain. Finally, the applicability of geometric factors to predict the transmission in the experimentally observed co-located pairs is discussed. The local stress field calculated by the discrete slip and twin band model is shown to be capable of determining whether a transmission has occurred in an observed co-located pair, and also the direction of the transmission.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Role of niobium in the high-temperature oxidation of titanium

Here, we compared the oxidation of Ti and Ti-2 at.% Nb at 800°C in Ar-20% O 2 and in sequential 16 O 2 - 18 O 2 atmospheres to clarify the role of niobium in the high-temperature oxidation of titanium. Niobium had no effect on the amount of oxygen dissolved in the metal or on oxygen diffusion in the metal. Instead, niobium enhanced oxidation resistance by segregating to TiO 2 grain boundaries, where it likely slowed outward Ti diffusion. These findings spotlight doping of TiO 2 grain boundaries as a strategy for improving the oxidation resistance of Ti alloys and, more generally, TiO 2 -forming alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Role of nitrogen in the high-temperature oxidation of titanium alloys

Here, we characterized the oxidation of pure Ti, Ti-0.8Si, and Ti-2Nb at 800 °C in N 2 -20% O 2 and in sequential isotopically labeled N 2 -20% O 2 atmospheres to clarify how nitrogen influences the high-temperature oxidation mechanisms of titanium alloys. The alloys always exhibited a nitride layer beneath a compact oxide scale with localized nitrogen concentrations in the underlying metal. Nitrogen is found to limit the oxygen concentrations in the metal. The synergy between alloying and nitrogen helps maintain compact oxide scales, preventing the formation of the lamellar scales observed during oxidation in nitrogen-free atmosphere and the oxidation of pure Ti regardless of the atmosphere.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Cross-slip and easy-glide CRSS in titanium: Theoretical predictions and in-situ TEM measurements

This study investigates the mechanics of prismatic and first-order pyramidal $\langle$a$\rangle$ slip in titanium (Ti), elucidating the physics of easy-glide and cross-slip through a combination of theory and experiments. Screw-character prismatic (Pr) dislocations in Ti are of particular interest because their complex cores can be stable or unstable, leading to activation by either cross-slip or planar glide. To investigate these mechanisms, site-specific micro tensile samples were prepared using focused ion beam (FIB) milling and mounted on a push-to-pull (PTP) device for in-situ transmission electron microscopy (TEM) tensile testing. The in-situ experiments provide direct observations of the onset of dislocation motion and the precise determination of the critical resolved shear stress (CRSS) for the activated mechanisms, and its evolution with load cycling. A comprehensive theory has been developed to predict the CRSS values for easy glide, cross-slip, and multiplication of dislocations. Predicted critical stresses for pyramidal (π)-to-Pr and reverse cross-slip agree closely with the experimental measurements. The latter cross-slip stress is a factor of two higher than that of unobstructed planar slip. The model accounts for overlapping dislocation cores and employs a Wigner-Seitz based cell to evaluate misfit energies. By combining ab initio density functional theory (DFT) with anisotropic elasticity, the framework identifies minimum energy pathways for dislocation glide, which can be intermittent and zig-zag. A simplified expression utilizing (π) and Pr Schmid factor ratios is proposed for critical stress corresponding to (π)-to-Pr cross-slip transition. The results are strongly dependent on crystal orientation, underscoring non-Schmid behavior. Overall, this study explores key critical stress parameters essential for informing higher-scale simulations of plasticity in Ti.

Critical stress↗
DOE OSTI2021

On the existence of orthorhombic martensite in a near-α titanium base alloy used for additive manufacturing

Additive manufacturing is a state-of-the-art production technology to produce tailor-made and highly complex parts. Among various other alloys, Ti base alloys are frequently used in this manufacturing technique due to their well-balanced properties and their wide range of applications. Allotropic phases and the occurrence of athermal phase transformations are the main reasons why these alloys hold a great development potential and are the basis of extensive use. High cooling rates during manufacturing lead to martensitic phases and the formation of nanometer-sized microstructures resulting in extraordinary strength. Simultaneously, such high cooling rates cause a high amount of lattice defects and the occurrence of residual stresses, which finally may result in delamination effects and cracks. Usually, a common approach to reduce residual stresses during additive manufacturing is to decrease thermal gradients by increasing the heat input or preheating the building platform. Instead of applying the typical approaches to lower thermal gradients, this study deals with the origin of the ‘softer’ orthorhombic martensite by accelerating the solidification process. The implementation of the orthorhombic phase in bulk components was inspired by a new phase transformation herein reported for the first time in the powder material, which also validates the possible occurrence of two martensitic phases in the same alloy. Various sophisticated characterization techniques like high energy and high-temperature X-ray diffraction, high-resolution transmission electron microscopy as well as atom probe tomography were applied to characterize this softer orthorhombic martensitic phase in detail aiming to highlight the opportunities accompanied by this new approach for additive manufacturing of titanium alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Damage evolution and ductile fracture of commercially-pure titanium sheets subjected to simple tension and cyclic bending under tension

This paper describes a study into the evolution of damage in commercial-purity titanium (CP–Ti) sheets subjected to cyclic bending under tension (CBT) and uniaxial tension (simple tension, ST). Sections were taken from sheets that were strained to various levels under both methods and were imaged using X-ray computed tomography (XCT) to reveal insights into the size, density, and distribution of microvoids in the sheets. Digital image correlation (DIC) was also used to observe the surface strain of CBT and ST sheets during testing. These results showed that elongation to failure (ETF) for CBT deformation is about 2.5× higher than for ST, local longitudinal strains in the bulk of the CBT sample are around 1.3× higher than the peak strain in the ST necked region, and 1.7× higher in the localized region of CBT failure. It was found that the volume-density of voids in both sheets followed a similar exponential increase with strain, reaching nearly 45× higher in the CBT than the ST sheets before the onset of failure, mainly due to the higher strain levels achieved. A higher volume density of voids developed in the center of sheets at high levels of strain, for both processes, with the density in the sheet center becoming approximately double that found near the edges. Scanning electron microscopy (SEM) was used to examine the fracture surface of CBT and ST sheets after failure. The observations are presented and discussed highlighting the CBT process as effective to delay ductile fracture of the CP-Ti sheets.

Commercially pure titanium↗
DOE OSTI2020

Homogeneous titanium hydroxide yields hydroxyl decorated nanofiber separator with improved electrolyte uptake and device capacitance

Good wettability of separators in batteries and capacitors is crucial for performance. Titanium hydroxide (Ti(OH) x ) has been shown to greatly improve the wettability of polyvinylidene fluoride (PVDF) nanofibers (NFs). Here, PVDF/Ti(OH) x NFs were evaluated for their potential use as separators. Results show that PVDF NFs incorporated with Ti(OH) x have improved electrolyte uptake (EU) between 550 and 1200 EU% compared to untreated PVDF with less than 100 EU%. Significant improvements in capacitance are seen from capacitors utilizing PVDF/Ti(OH) x NF separators with the best performing PVDF/Ti(OH) x NF at 15 wt% Ti(OH)x with 446.8 mF/cm 2 compared to untreated PVDF NF separator with 262.7 mF/cm 2 .

36 MATERIALS SCIENCE↗
DOE OSTI2021

Strain rate effects on the mechanical behavior of porous titanium with different pore sizes

High strain-rate (up to 6600 s –1 ) and quasi-static compression tests are conducted on a powder-sintered porous titanium with different pore sizes (mean: 30 μm and 120 μm). In situ X-ray imaging is implemented to characterize the pores-scale deformation dynamics. The yield strength as a function of strain rate exhibits two stages of rate sensitivity, and the transition occurs at 1600 s –1 . X-ray images show that pore compaction and strain localizations occur preferentially at pores oriented perpendicular to the loading direction under quasi-static loading, but become more random under high strain-rate loading as a result of higher driving force and plastic deformation nucleation rate. Here, the more homogeneous nucleation of plastic deformation contributes to the increased rate sensitivity beyond 1600 s –1 . At the same strain rate, the yield strength of porous Ti as well as strain field homogeneity decreases significantly with increasing pore size. The small pore spacing in fine-pored Ti reduces the degree of stress concentrations around pores. Therefore, the higher stress concentrations in coarse-pored Ti lead to an earlier yield of matrix around pores and thus a lower bulk yield strength.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Nanoporous Titanium (Oxy)nitride Films as Broadband Solar Absorbers

Broadband absorption of solar light is a key aspect in many applications that involve an efficient conversion of solar energy to heat. Titanium nitride (TiN)-based materials, in the form of periodic arrays of nanostructures or multilayers, can promote significant heat generation upon illumination thanks to their efficient light absorption and refractory character. In this work, pulsed laser deposition was chosen as a synthesis technique to shift metallic bulk-like TiN to nanoparticle-assembled hierarchical oxynitride (TiO x N y ) films by increasing the background gas deposition pressure. The nanoporous hierarchical films exhibit a tree-like morphology, a strong broadband solar absorption (~90% from the UV to the near-infrared range), and could generate temperatures of ~475 °C under moderate light concentration (17 Suns). The high heat generation achieved by treelike films is ascribed to their porous morphology, nanocrystalline structure, and oxynitride composition, which overall contribute to a superior light trapping and dissipation to heat. These properties pave the way for the implementation of such films as solar absorber structures.

14 SOLAR ENERGY↗
DOE OSTI2024

A Titanium-Based Metal–Organic Framework For Tandem Metallaphotocatalysis

Metal–organic frameworks (MOFs) have garnered substantial attention for their unique properties, such as high porosity and tunable structures, making them versatile for various applications. This paper constructs photoactive titanium–organic frameworks by combining Ti(IV) clusters and a bipyridine linker. The MOF is synthesized in situ through imine condensation, resulting in NU-2300. Subsequent ex situ nickel salt complexation results in NU-2300-Ni, which is then used for light-mediated carbon–heteroatom cross-couplings. The photophysical properties of the metallaphotocatalyst were investigated by UV-vis and EPR analysis, and both the Ti cluster and the bipyridine linker were found to contribute to successful catalysis, making it a tandem catalyst. The heterogeneous material retained its performance through five cycles of thioetherification. As a result, this work contributes not only to MOF synthetic strategies, but also to expanding MOF applications as recyclable, tandem metallaphotocatalysts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Pseudocapacitive Titanium Oxynitride Nanowires for Ultrahigh Capacitance Supercapacitors

High-quality, multifunctional two-dimensional (2D) titanium oxynitide (TiNO) thin films and one-dimensional (1D) TiNO nanowires have been synthesized using a pulsed laser deposition, a simple, fast, and congruent evaporation method. First-principles calculations as a function of surface orientation and termination indicate that surface oxidation of TiNO nanowires can stabilize the (110) orientation observed experimentally. The specific capacitance value for the TiNO nanowire samples (2725 mF/cm 2 ) has been found to be nearly six times more than that of the TiNO thin film samples (400 mF/cm 2 ), which is attributed to the high packing density of TiNO nanowires over a given area. The nanowire samples have also been found to exhibit a significantly higher energy density (1.35 μWh/cm 2 ) than the TiNO thin-film samples (0.33 μWh/cm 2 ). Thus, the TiNO material system in thin-film and nanowire forms has been demonstrated to be a promising candidate for use as an electrode material in supercapacitors and other charge-storage applications.

capacitors↗
DOE OSTI2020

Local spring effect in titanium-based layered oxides

Titanium-based layered oxides (TLOs) are one of the most promising electrode material families for sodium-ion batteries (NIBs) due to their smooth charge/discharge profiles and excellent cycle performance. However, the reaction mechanism of these materials, especially the reason for the disappearance of multiple voltage plateaus, is still not clear. Herein, two representative TLOs (Na 2/3 Ni 1/3 Ti 2/3 O 2 and Na 2/3 Co 1/3 Ti 2/3 O 2 ) with the same P2 crystal structure have been studied to scrutinize those unexplained issues. In situ synchrotron high-energy X-ray diffraction revealed a solid solution reaction mechanism for both, suggesting the absence of rigid phase transitions upon electrochemical cycling. An interesting “spring effect” of the TiO 6 octahedron, i.e., the reversible vibration of the central Ti atom inside the local octahedron upon electrochemical redox, was demonstrated by advanced X-ray absorption spectroscopy and theoretical calculations. Such an effect could suppress the rigid phase transitions, and result in smooth charge/discharge profiles and enhanced cycle stability. Finally, this work not only accounts for the disappearance of multiple voltage plateaus of TLOs for NIBs, but also provides an effective local-structure viewpoint to increase the cycle stability of electrode materials for other advanced battery systems.

25 ENERGY STORAGE↗
DOE OSTI2023

Titanium dioxide and table sugar enhance the leaching of silver out of nanosilver packaging

We manufactured laboratory-scale food packages containing 2.57 ± 0.18 × 10 –3 wt% silver nanoparticles (AgNPs) and used them to show that table sugar (sucrose) and microcrystalline titanium dioxide (μTiO 2 ) enhance Ag migration from these packages and into aqueous food simulants. Ag migration into purified water was detected but was below the limit of ICP-MS quantitation, giving a range of potential Ag migration between 0.059 and 0.082 ng cm –2 packaging surface area. Ag migration into 9 wt% aqueous sucrose solution was 0.547 ± 0.084 ng cm –2 and migration into 9 wt% sucrose solution containing 0.01 wt% μTiO 2 was 0.724 ± 0.032 ng cm –2 . Total Ag migration into a 0.01 wt% μTiO 2 aqueous dispersion without sucrose was between 0.122 and 0.162 ng cm –2 , with upper and lower limits defined by the detectability of Ag in the supernatant phase of the simulant. If the midpoint of this range is taken as a baseline, these results imply that, compared to purified water, Ag migration was increased by approximately 10.3 times when the water simulant contained μTiO 2 and sucrose at commercially-relevant concentrations. Notably, the Ag migrated into water containing both ingredients exceeded the total Ag migrated into either of the single-ingredient simulants, pointing to a potential cooperative relationship between sucrose and μTiO 2 that possibly derives from binding and redox interactions between these two ingredients. Sucrose and μTiO 2 also both reduced a portion of migrated Ag + back into AgNPs, and μTiO 2 particles efficiently captured (>25% by mass) migrated Ag on their surfaces. Similar effects on migration were observed with nanocrystalline TiO 2 . Furthermore, these experiments are the first to show that TiO 2 particles exert a strong influence on the quantity and form of Ag that could migrate from AgNP-enabled packaging, suggesting that food formulations and interactions between individual food components may be important to consider when evaluating the fate of nanoparticles in these consumer applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Electroplating Titanium from Ionic Mixtures

Titanium & Zirconium metal films have been electroplated by a near-ambient scalable process for high value-add/lower volume applications. The films have been commercially tested as bonding layers

36 MATERIALS SCIENCE↗
DOE OSTI2025

Defining the Shape Density of Cerium Oxide and Titanium Dioxide Aerosol

The “shape density” of CeO 2 (cerium oxide) powder (American Elements, Los Angeles CA) is estimated to be 0.82 ± 0.02 g cm -3 and the shape density for TiO 2 (titanium dioxide) powder (American Elements, Los Angeles CA) is estimated as 0.54 ± 0.01 g cm -3 . The “shape density” is defined as the measured loose density (ASTM 2018 and ASTM 2021) of a powder divided by the ICRP (International Commission on Radiological Protection) default aerosol shape factor (Valetin 2002). This information is used for experimental measurements of the RRF (respirable release factor) and other respirable source term parameter (US DOE 1994) experiments at the Los Alamos National Laboratory (LANL). The shape density is the input parameter to the TSI Inc (Shoreview MN) AIM (Aerosol Instrument Manager) software for the TSI model 3321 APS (Aerodynamic Particle Sizer) (Figure 1).

61 RADIATION PROTECTION AND DOSIMETRY↗
DOE OSTI2024

Titanium-45 (45Ti) Radiochemistry and Applications in Molecular Imaging

Molecular imaging is an important part of modern medicine which enables the non-invasive identification and characterization of diseases. With the advancement of radiochemistry and scanner technology, nuclear medicine is providing insight into efficient treatment options for individual patients. Titanium-45 (45Ti) is a lesser-explored radionuclide that is garnering increasing interest for the development of positron emission tomography (PET) radiopharmaceuticals. This review discusses aspects of this radionuclide including production, purification, radiochemistry development, and molecular imaging studies.

62 RADIOLOGY AND NUCLEAR MEDICINE↗