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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
NASA NTRS2018

Characterization of Titanium Alloys Produced by Electron Beam Directed Energy Deposition

Functionally graded materials offer the potential to improve structural efficiency by allowing the material composition and/or microstructural features to spatially vary within a component. Additive manufacturing techniques enable the fabrication of such graded materials and structures. While examining several titanium alloys, this paper focuses on Ti-8Al-1Er as it has a unique microstructure that is only feasible when produced by rapid solidification methods like electron beam directed energy deposition, an additive manufacturing process. The results show that, when mixed, Ti-8Al-1Er and commercially-pure titanium uniformly mix at various ratios and the resultant static tensile properties of the mixed alloys behave according to rule-of-mixtures. At discontinuous interfaces between Ti-8Al-1Er and commercially-pure titanium, the crack growth behavior progresses smoothly across the discontinuity as the crack transitions from one crack growth regime into another. Studies on monolithic samples shows the mechanisms of damage in the Ti-8Al-1Er; specifically, that strain localization occurs near grain boundaries of high mis-orientation on the microscale and that twinning and dislocation density is concentrated near erbia-strengthening particles (Er2O3) on the nanoscale.

Newman, John A.↗
DOE OSTI2025

Ex-situ Heat Treatment of TEM Foils in a Custom Titanium Fixture: A Case Study on Ni-based Superalloy

The advancement of microstructural characterization at the nanoscale is critical to understanding the microstructural evolution and performance of engineering materials. Transmission electron microscopy (TEM) plays a vital role in such investigations, particularly when coupled with controlled ex- and in-situ experiments. In this study, we introduce a novel method for ex-situ heat treatment (HT) of TEM foils using a custom-designed fixture, made from pure titanium, and vacuum furnace to inhibit oxidation. This approach ensures precise temperature control and minimal sample contamination during HT, critical for substructural characterization and analysis of metallic materials. The fixture consists of a titanium base with three slits, for three sample foils, and a titanium cap for closure. The entire assembly is placed in a vacuum heat treatment furnace with high vacuum capability to prevent oxidation. To validate the effectiveness of the setup, precipitation behavior and microstructural changes were studied in an IN725 variant heat-treated at 500°C for 1 hour and 282 variant heat-treated at 700°C for 1 hour, as case studies.

electron microscopy↗
DOE OSTI2025

Improving Surface Quality of Titanium Electrodeposition from a Deep Eutectic Solvent with Organic and Inorganic Additives

Titanium electroreduction is desired for a variety of medical, electronic, and bonding applications but has not been possible until recently. Titanium electrodeposition with leveler and brightener additives in the deep eutectic solvent ethaline has been studied for effects on spectroscopic reflectance. Polymeric leveling agents and several small‐molecule brighteners produce level/bright films (respectively) with high values for both specular and diffuse reflectance. The application of these leveling and brightening agents can produce films with appearances and surface roughnesses that may be suitable for application in medical implants such as stents, corrosion protection of electronics for wearable technology, and as interlayers between dissimilar metals.

deep eutectic solvents↗
DOE OSTI2026

Low-Pressure Diffusion Bonding of Vanadium to Commercially Pure Titanium and Ti-6Al-4V

Modern technology increasingly requires components to be made from specific high-performance materials. To support complex multi-metal structures, a variety of techniques are required to join dissimilar metal parts with precise shapes. This study evaluates vacuum diffusion bonding as a method for joining titanium and vanadium, focusing on both pure titanium and the common alloy Ti-6Al-4V. We employ modest pressure provided by a weight and simple surface preparation to simulate the most commercially applicable process. Here, we show that Ti-6Al-4V alloy bonds readily to V, forming a continuous, clearly defined interdiffusion layer with predictable kinetics. Conversely, commercially pure Ti forms a crack-prone bond with V that fails to improve at higher bonding temperatures or longer times. We attribute this failure to the concentration of stress caused by the ß-to-α phase transformation in Ti. The contrasting bonding efficacy between pure Ti and the alloy provides insight into the crystallographic interactions that occur at the interface during bonding and cooling. These results provide surprising insight into a new method for bonding Ti alloys to V and possibly other metals that share the body-centered cubic crystal structure.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Deformation behavior of CP-titanium under strain path changes: Experiment and crystal plasticity modeling

The deformation behavior of commercially pure rolled titanium subjected to strain path changes is studied using experiments and a crystal plasticity model. Four different loading combinations are performed at room temperature to study the activation of slip, twinning, de-twinning and double-twinning in hexagonal closed packed titanium. The strain paths considered are: rolling direction compression (RDC) followed by normal direction compression (NDC), RDC followed by transverse direction compression (TDC), NDC followed by RDC, and NDC followed by TDC. An EBSD-based analysis of the distribution of boundary misorientation angles before and after reload was developed to analyze the evolution of {$10\bar{1}2$} tensile and {$11\bar{2}2$} compression twins. This analysis supports the model results concerning the treatment of twin reorientation. A de-twinning and double-twinning model accounting for back stress effects, an important feature of strain path changes, is implemented within the framework of the visco-plastic self-consistent (VPSC) model along with a dislocation density (DD) based hardening scheme. In the model, plasticity is accommodated by prismatic $\langle$a$\rangle$, basal $\langle$a$\rangle$ and pyramidal $\langle$c+a$\rangle$ slip modes, and {$10\bar{1}2$} tensile and {$11\bar{2}2$} compression twinning modes. The VPSC model predicts the evolution of twinning, de-twinning and double-twinning processes for both tensile and compression twinning modes under strain path change. The model predicts macroscopic stress-strain response, texture evolution, and twin volume fraction that are in agreement with experimental observations. The evolution of texture is investigated in detail by separately analyzing the twinned domains, rather than the evolution of the global texture.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Crystallographic stability of the BCC phase during quenching of metastable beta titanium alloy Ti-5553 and comparison of structural criteria for the predictive capability of α” martensite

This work evaluates the compositional standard currently developed for Ti-5553 powder and explores the metastable β region for sensitivity to martensitic formation during rapid quenching from the melt. Ti-5553 is a beta-stabilized titanium alloy that is increasingly being used in additive manufacturing applications. A series of alloys within the Ti-5553 compositional space was processed using two-piston spat quenching to perform rapid solidification and quenching for each of these alloy compositions. Typical empirical models such as molybdenum equivalency are not able to fully separate the retained BCC and martensitic compositions. Further, the use of thermodynamic data to estimate the transformation energy needed to form martensite can differentiate the alloys and provide a metric to further develop compositional limits for metastable beta titanium alloy development.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Experimental investigation of the dependence of void nucleation and growth on initial microstructure in high-purity titanium under tension

An experimental investigation of failure mechanisms in relation to the initial microstructure in high-purity titanium samples is presented. The initial microstructure of the specimens was measured in 3D using diffraction-contrast tomography (DCT). Ex-situ X-ray computed tomography (XCT) was used to visualize voids in specimens at various levels of deformation attained by interrupted tensile testing. Electron backscatter diffraction (EBSD) mapping was used to characterize the deformed microstructures per specimen. The investigation showed that the location of failures was unrelated to the formation of the first voids, but rather the nucleation and growth of cracks were from heavily deformed surface regions. The areas surrounding the failure-causing cracks had the highest propensity for void development of any area in the specimen. This facilitated crack propagation through the specimen via “linking up”. The failure of the specimens by microvoid coalescence was bolstered by “dimpled” fracture surfaces. Paint composed of gallium embedded in rubber was used to track the displacement of points along the loading direction of the specimens, to relate the location of failure to the material's initial microstructure. However, the correlation proved difficult, due to complex microstructural evolution involving voids, grain fragmentations, and profuse twinning. Nevertheless, it was shown that necking occurred near the largest grain in the gauge section of the specimens. This is likely caused by the decrease in strength of larger grains, causing strain to concentrate in their vicinity. Here, a comprehensive picture of the failure processes in high-purity titanium under axial loading is presented and discussed in the paper.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Cooling dynamics of two titanium alloys during laser powder bed fusion probed with in situ X-ray imaging and diffraction

Metal parts produced by laser powder bed fusion (LPBF) additive manufacturing exhibit characteristic microstructures comparable to those observed in laser welding. The primary cause of this characteristic microstructure is rapid, localized heating and cooling cycles, which result in extreme thermal gradients where material solidification is followed by fast cooling in the solid state. The final microstructure and mechanical performance are also influenced by pore formation caused by melt pool fluid dynamics. Here, we use high speed, in situ X-ray diffraction to probe the kinetics of cooling and solid-solid phase transitions after laser melting in two aerospace titanium alloys: Ti-6Al-4V, an α + β alloy; and Ti-5Al-5V-5Mo-3Cr, a near-β alloy. We complement these diffraction studies with in situ X-ray imaging to probe melt pool dynamics and pore formation. From these two complementary probes, we quantify pore formation during melting and the subsequent microstructural evolution as the material rapidly cools after solidification. These results are critical for understanding defect formation and residual stress development in different titanium alloys under LPBF conditions and can help inform process models to predict final part performance.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Stabilization of Low Valent Zirconium Nitrides in Titanium Nitride via Plasma-Enhanced Atomic Layer Deposition and Assessment of Electrochemical Properties

The increasing awareness of metal nitrides as feasible electrocatalysts in numerous energy-relevant transformations motivates greater synthetic control of mixed metal nitride compositions and their valence states. We report plasma-enhanced atomic layer deposition of titanium zirconium nitride, with an emphasis on the experimental parameters that influence the valence states of the two metal ions. We further examined the consequence of various ratios of Ti and Zr on the electrochemically active surface areas (ECSAs). Films with a Zr-to-Ti ratio of 1:2 or 1:1 yielded the highest ECSA; deviation from these values led to a large fraction of electrically insulating or semiconducting titanium or zirconium oxynitrides/oxides. The systematic examination establishes a fundamental structure-property relationship critical to assessing the electrochemical/electrocatalytic properties of metal nitrides.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Electrolyte Engineering for Efficient Electrochemical Nitrate Reduction to Ammonia on a Titanium Electrode

Nitrates from agricultural runoff and industrial waste streams are a notorious waste product and hazardous pollutant. Traditional electrochemical water remediation approaches aim to solve this problem by converting nitrates to environmentally benign N 2 while minimizing the production of environmentally hazardous side products such as ammonia and nitrous oxide in a process known as “denitrification”. We modify this concept and outline an opportunity to optimize the conversion of nitrates into ammonia, which is also a key commodity product used as a fertilizer, potential fuel, and chemical precursor. The electrochemical conversion of nitrates to ammonia recycles the fixed nitrogen and offers an appealing and supplementary alternative to the energy- and resource-intensive Haber-Bosch process. In this study, we investigated the effect of varying electrochemical conditions (pH, nitrate concentration, and applied potential) on the selective reduction of nitrate to ammonia at a titanium cathode. We observed that high concentrations of both protons and nitrate ions are needed to achieve high selectivity, reaching a peak of 82% Faradaic efficiency to ammonia at an applied potential of -1 V versus RHE and a partial current density to NH 3 of -22 mA/cm 2 , using 0.4 M [NO 3 – ] at pH ~0.77. The Ti electrode, as a poor hydrogen evolution catalyst with notable corrosion resistance, provides a large window of operating conditions to achieve high selectivity in the reduction of nitrate anions. Stability of the system was evaluated, and we found a high Faradaic efficiency throughout the course of an 8 h experiment. After electrochemical testing, titanium hydride was observed at the cathode surface. We also show a preliminary technoeconomic study, indicating that it may be feasible to employ an electrochemical strategy for the production of ammonium nitrate.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

The influence of alloying on slip intermittency and the implications for dwell fatigue in titanium

Dwell fatigue, the reduction in fatigue life experienced by titanium alloys due to holds at stresses as low as 60% of yield, has been implicated in several uncontained jet engine failures. Dislocation slip has long been observed to be an intermittent, scale-bridging phenomenon, similar to that seen in earthquakes but at the nanoscale, leading to the speculation that large stress bursts might promote the initial opening of a crack. Here we observe such stress bursts at the scale of individual grains in situ, using high energy X-ray diffraction microscopy in Ti–7Al–O alloys. This shows that the detrimental effect of precipitation of ordered Ti 3 Al is to increase the magnitude of rare pri $\langle$a$\rangle$ and bas $\langle$a$\rangle$ slip bursts associated with slip localisation. By contrast, the addition of trace O interstitials is beneficial, reducing the magnitude of slip bursts and promoting a higher frequency of smaller events. This is further evidence that the formation of long paths for easy basal plane slip localisation should be avoided when engineering titanium alloys against dwell fatigue.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Sulfidation kinetics of titanium and Ti-6Al-4V with elemental sulfur

The sulfidation kinetics of titanium and Ti-6Al-4V (Ti64) using elemental sulfur were studied by measuring the amount of metal consumed instead of the change in mass or scale thickness. Here this metal consumption approach combines the parabolic oxidation law, Arrhenius equation, and Pilling-Bedworth ratio to determine the apparent activation energy and the pre-exponential factor of consumption of Ti64 during sulfidation. The estimations of apparent activation energy and pre-exponential factor were 110.4 kJ·mol -1 and 1.3×10 -9 m 2 s -1 for the titanium-sulfur, and 116.2 kJ·mol -1 and 1.2×10 -9 m2s -1 for the Ti64-sulfur system. Finally, a material removal predictor was developed to predict the amount of Ti64 consumed for a given sulfidation temperature and time.

36 MATERIALS SCIENCE↗
DOE OSTI2024

A method for crystallographic mapping of an alpha-beta titanium alloy with nanometre resolution using scanning precession electron diffraction and open-source software libraries

An approach for the crystallographic mapping of two-phase alloys on the nanoscale using a combination of scanned precession electron diffraction and open-source python libraries is introduced in this paper. This method is demonstrated using the example of a two-phase α/β titanium alloy. The data were recorded using a direct electron detector to collect the patterns, and recently developed algorithms to perform automated indexing and analyse the crystallography from the results. Very high-quality mapping is achieved at a 3 nm step size. The results show the expected Burgers orientation relationships between the α laths and β matrix, as well as the expected misorientations between α laths. A minor issue was found that one area was affected by 180° ambiguities in indexing occur due to this area being aligned too close to a zone axis of the α with twofold projection symmetry (not present in 3D) in the zero-order Laue Zone, and this should be avoided in data acquisition in the future. Nevertheless, this study demonstrates a good workflow for the analysis of nanocrystalline two- or multi-phase materials, which will be of widespread use in analysing two-phase titanium and other systems and how they evolve as a function of thermomechanical treatments.

36 MATERIALS SCIENCE↗
DOE OSTI2021

In Situ High Energy X-ray Diffraction Characterization of Phase Transformations and Mechanical Behaviors in Rapidly Solidified Titanium and Stainless Steel Alloys [Thesis]

Advanced manufacturing techniques like additive manufacturing (AM) have poised themselves to revolutionize metal manufacturing. A wide range of AM techniques are capable of manufacturing metal components with unique, complex geometries and hastening the scientific-engineering-development cycle. Metal AM relies on a layer-by-layer rapid manufacturing process to build components from the substrate up. Rapid solidification is a large departure from traditional metal manufacturing due to its complex physics. Characterization of rapid solidification is difficult, stemming from the small volumes used in AM and the fast dynamics of the process. High energy X-ray diffraction (HEXRD) is a solution to the characterization problems of rapidly solidified alloys and AM. HEXRD can probe small volumes at fast rates and provides a wide range of thermomechanical and kinetic information. This thesis presents the application of HEXRD to rapidly solidified titanium and stainless steel alloys through a series of case studies. In the first two studies, HEXRD is applied to rapidly solidified titanium and stainless steel welds. The materials are characterized for their temperature history, phase changes, kinetics, and microstructural evolution. In the next case study, HEXRD is applied to characterize phase changes in elastocaloric NiTi shape memory alloys (SMAs) under thermomechanical load. HEXRD, in conjunction with other tools, is used to explain the superior performance of the additively manufactured SMAs. In the final two case studies, HEXRD is used to measure the mechanical response of AM parts with complex geometries; namely, the octet truss lattice. Diffraction reveals a wide range of materials information about the AM microstructure including unexpected phases, texture, and mechanical response to loading. The mechanical results from HEXRD and then compared with theoretical predictions about the performance of octet truss lattices. Summarily, HEXRD is a diverse tool that is poised to address the complex characterization problems of many aspects of the additive manufacturing process.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Recycling of Titanium Scrap by Shear Assisted Processing and Extrusion (ShAPE)

Titanium and its alloys are used in the aviation and automobile industries due to their remarkable strength to weight ratio, but, commonly, machining loss is high with ~90 wt.% of the material being converted to scrap. Recycling post-consumer Ti scrap directly into solid bulk products is a potential solution for repurposing valuable material. Further, reducing or even eliminating fresh Ti sponge during recycling might lead to lower energy and greenhouse gas emissions. In this study, a solid-phase process known as friction extrusion was utilized to recycle Ti-6Al-4V machining chips into solid wires which could be used as feedstock in additive manufacturing. The friction consolidation technique was first used to convert chips with varying degrees of oxygen content into solid billets for its use as feedstock material in subsequent friction extrusion. The extrudates were fabricated above the beta transition temperature, which was achieved by selecting rotation rate and feed rate, to process the billets near 1000°C using a tungsten-lanthana extrusion die. This work presents the first occurrence of friction extruded titanium alloy wires. The effect of friction extrusion on microstructural features, tensile properties, and texture are reported. Overall, the friction extrusion method is capable of recycling Ti-6Al-4V scrap directly into extruded wire.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Applying Dynamic Strain on Thin Oxide Films Immobilized on a Pseudoelastic Nickel-Titanium Alloy

Direct alteration of materials structure/function through strain is a burgeoning area of research that has allowed for novel properties of materials to emerge. Tuning materials structure can be achieved by controlling an external force imposed on materials and inducing stress-strain responses (i.e., applying dynamic strain). Electroactive thin films are typically deposited on shape or volume tunable elastic substrates, where mechanical loading (i.e. compression or tension) can affect films structure and function through imposed strain. Here we summarize methods for straining n-type doped titanium dioxide (TiO2) films prepared by a thermal treatment of a pseudo-elastic nickel-titanium alloy. The main purpose of the described methods is to study how strain affects electrocatalytic activities of metal oxide, specifically hydrogen evolution and oxygen evolution reactions. The same system can be adapted to study the effect of strain more broadly. Strain engineering can be applied for optimization of a material function, as well as for design of adjustable, multifunctional (photo)electrocatalytic materials under external stress control.

92 SC - Basic Energy Sciences (BES) (SC-22)↗