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At least 343 records · Page 19

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DOE OSTI2021

Acid-resistant catalyst supports and catalysts

A process for preparing a catalyst comprises coating substantial internal surfaces of porous inorganic powders with titanium oxide to form titanium oxide-coated inorganic powders. After the coating, an extrudate comprising the titanium oxide-coated inorganic powders is formed and calcined to form a catalyst support. Then, the catalyst support is impregnated with a solution containing one or more salts of metal selected from the group consisting of molybdenum, cobalt, and nickel.

Schmidt, Stephen R.↗

DOE OSTI2023

Advanced Material Studies for High Intensity Proton Production Targets and Windows

The titanium alloy Ti6Al4V is widely used in accelerator facilities as beam windows, which are exposed to high cycle compressive stress waves from intense pulsed proton beams. Such materials interacting with the beam are subject to various forms of radiation damage, which can adversely affect their endurance limit. However, no fatigue data is currently available for high energy proton irradiated titanium alloy. Due to limitations in proton irradiation facilities, only miniature flat samples can be used for irradiation. To address this issue, we have developed a custom-made bend fatigue tester at Fermilab specifically for testing proton irradiated titanium alloy. In this presentation, we report on the fatigue test results obtained from this custom-fatigue tester using a non-ASTM standard specimen design. We plan to validate these sparse fatigue data with ASTM standard samples using standard fatigue samples. Furthermore, we have modified another commercial bend fatigue tester to accommodate miniature samples, and discuss some inherent deficiencies of the commercial fatigue tester to test miniature samples. To overcome this issue, a new fixture design is presented, which enables satisfactory fatigue testing on miniature samples over long periods. Finally, we present an upgrade to the custom-fatigue tester, featuring this new fixture design.

43 PARTICLE ACCELERATORS↗

DOE OSTI2023

Acid-resistant catalyst supports and catalysts

Schmidt, Stephen R.↗

DOE OSTI2020

TiO2 Nanocrystal-Framed Li 2 TiSiO 5 Platelets for Low-Voltage Lithium Battery Anode

Titanium-based anode materials are attracting considerable attention for use in high-performance lithium-ion batteries, but the compromised energy density caused by high voltage plateaus and unsatisfactory capacities severely retards their practical applications. Herein, a molten-salt synthesis of Li 2 TiSiO 5 crystalline platelets and a subsequent selective facet modification by in situ growth of TiO 2 nanocrystal frames are facilely achieved. The discharge voltage plateau at around 0.5 V renders the Li 2 TiSiO 5 anode safe compared with graphite and confers a high energy density compared with zero-strain Li 4 Ti 5 O 12 anode. With the optimized size, structure, and content of modified TiO2 nanocrystals associated with the exposed (001) plane of Li 2 TiSiO 5 , the Li 2 TiSiO 5 -based anodes can deliver a capacity of above 300 mAh g -1 , enhanced rate performance, and a capacity retention of 66% after 10 000 cycles. In situ X-ray diffraction and ex situ transmission electron microscopy have demonstrated the structural stability of the anodes upon charge/discharge. Further theoretical calculation reveals 3D migration paths of Li + ions in Li 2 TiSiO 5 . The selective modification of in situ grown TiO2 nanocrystals on certain facets of crystallites opens a new door for the development of electrode materials possessing superior electrochemical properties.

anodes↗

DOE OSTI2022

Oxides and Nitrides with Asymmetric Pore Structure from Block Copolymer Co–Assembly and Non–Solvent Induced Phase Separation

Materials combining an asymmetric pore structure with mesopores everywhere enable high surface area accessibility and fast transport, making them attractive for e.g., energy conversion and storage applications. Block copolymer (BCP)/inorganic precursor co-assembly combined with non-solvent induced phase separation (NIPS) provides a route to materials in which a mesoporous top surface layer merges into an asymmetric support with graded porosity along the film normal and mesopores throughout. Here, the co-assembly and non-solvent-induced phase separation (CNIPS) of poly(isoprene)-b-poly(styrene)-b-poly(4-vinylpyridine) (ISV) triblock terpolymer and titanium dioxide (TiO 2 ) sol-gel nanoparticlesare reported. Heat-treatment in air results in free-standing asymmetric porous TiO 2 . Further thermal processing in ammonia results in free-standing asymmetric porous titanium nitride (TiN). processing changes alter structural membrane characteristics is demonstrated. Changing the CNIPS evaporation time results in various membrane cross-sections ( finger-like to sponge-like). Further, oxide and nitride material composition, crystallinity, and porosity are tuned by varying thermal processing conditions. Finally, thermal processing condition effects are probed on phase-pure asymmetric nitride membrane behavior using cyclic voltammetry to elucidate their influence, e.g., on specific capacitance. Results provide further insights into improving asymmetric and porous materials for applications including energy conversion and storage, separation, and catalysis and motivate a further expansion of CNIPS to other (in)organic materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Unveiling Synergetic Photocatalytic Activity from Heterometallic Ti/Ce Clusters

Titanium-oxo clusters, with their robust structure and suitable optical and electronic properties, have been widely investigated as photocatalysts. Heterometallic Ti/M-oxo clusters provide additional tunability and functionality, which enable systematic structure-activity investigations to elucidate reaction mechanisms and improve catalyst de-sign. Incorporating cerium into Ti-oxo clusters can provide additional redox (Ce IV /Ce III ) and oxygen harvesting ability, but to date only limited number of structurally defined titanium-cerium (Ti/Ce) clusters have been reported due to their synthetic challenges. Herein, we report the synthesis and photocatalytic properties of two structurally defined Ti/Ce-oxo clusters, Ti 8 Ce 2 (BA) 16 and Ti 9 Ce 4 (BA) 20 , as well as a TiCe-BA cluster with a calculated formula of Ti 20 Ce 9 O 36 (BA) 42 . Photocatalytic study of these clusters demonstrates that the amount of Ce 3+ species greatly impacts its photocatalytic oxidation performance, and their superior photocatalytic reactivity towards aerobic alcohol oxidation can be contributed to the synergistic effects of the multiple radical species generated upon light absorption. Furthermore, this work represents a significant milestone in the construction of stable Ti/Ce-oxo clusters, enriching the current library of known heterometallic Ti/M-oxo clusters, and providing a series of crystalline materials with great promise of photo-luminescence and photovoltaic chemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

A New Method for Creating Structured High-Performance Current Collectors for Electrochemical Applications

A significant challenge in many electrochemical systems is finding a stable, high-performing current collector material that is mechanically robust, adaptable in form factor, and free of precious metals. Titanium electrodes are robust in many of these regards but exhibit poor charge transfer performance due to self-passivation. Herein, a new materials processing paradigm based on the titanium/titanium nitride (Ti/TiN) system which allows for robust, stable, and low-resistance current collectors of arbitrary form factor is presented. Specifically, a gas-nitriding process for 3D-printed titanium electrodes that results in a 20-fold improvement of charge transfer characteristics relative to the untreated material is outlined. The ability to utilize 3D-structured current collectors with a net 40-fold improvement in performance over nonstructured electrodes is further demonstrated. This novel approach to creating electrochemical current collectors requires minimal laboratory resources and can be widely adapted for a variety of applications, including desalination, electrolysis, energy storage, and basic research. In conclusion, the work described herein provides both a means for accelerating research and opens the door to hierarchical tuneability for enhanced performance.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Friction-based recycling: an evaluation of friction extrusion for fabricating Ti-6Al-4 V wire fabricated from machining chip feedstock

Abstract Titanium and its alloys are used in aviation and automobile industries due to their remarkable strength to weight ratio, but machining loss commonly is high with ~ 80 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, 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-4 V 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 the 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 directly recycling Ti-6Al-4 V scrap into extruded wire.

Friction Extrusion↗

DOE OSTI2024

The derivation of CRSS in pure Ti and Ti-Al alloys

The work focuses on the determination of the critical resolved shear stress (CRSS) in titanium (Ti) and titanium-aluminum (Ti-Al) alloys, influenced by an array of factors such as non-symmetric fault energies and minimum energy paths, dislocation core-widths, short-range order (SRO) effects which alter the local atomic environment, and tension-compression (T-C) asymmetry affected by intermittent slip motion. To address these multifaceted complexities, an advanced theory has been developed, offering an in-depth understanding of the mechanisms underlying slip behavior. The active slip systems in these materials are basal, prismatic, and pyramidal planes, with the latter involving both $\langle$a$\rangle$ and $\langle$c + a$\rangle$ dislocations. Each slip system is characterized by distinct Wigner-Seitz cell configurations for misfit energy calculations, varying partial dislocation separation distances, and unique dislocation trajectories—all critical to precise CRSS calculations. The theoretical CRSS results were validated against a comprehensive range of experimental data, demonstrating a strong agreement and underscoring the model's efficacy.

Critical stress↗

DOE OSTI2023

Coating developments towards enabling aluminum as a bipolar plate material for PEM fuel cells

Bipolar plates represent a significant portion of the cost and weight of a proton exchange membrane fuel cell stack. As a result, there has been significant interest in using low weight and cost materials, such as aluminum. Aluminum has good mechanical and physical properties; however, it performs poorly in the corrosive environment within the fuel cell stack. To overcome the corrosion performance issue, there have been efforts towards developing coating processes to enable aluminum to attain corrosion targets. In an effort to enable aluminum as a viable bipolar plate material, a solid phase processing (diffusion bonding) approach for bonding a titanium foil to aluminum is investigated in this study. The microstructure, corrosion performance, mechanical properties and electrical resistance are investigated. To avoid the known reduction in contact resistance performance of titanium after exposure to bipolar plate media, the effect of addition of highly conductive gold particles after diffusion bonding, on contact resistance and corrosion behavior, is also studied and compared with diffusion bonded Ti to Al. In conclusion, the results indicate that diffusion bonded Ti to Al provides a viable alternative material combination for bipolar plate that avoids the micro pores and crevasses that are associated with vapor deposition or electroplating.

25 ENERGY STORAGE↗

DOE OSTI2023

Solid-state reaction mediated microstructural evolution in a spark plasma sintered in situ Ti–B 4 C composite

For this study, a novel porosity-free in situ Ti–B 4 C composite was fabricated via spark plasma sintering (SPS). Detailed analysis of the phase evolution, coupling results from XRM, XRD and SEM-EBSD-EDS, indicate that primarily TiB 2 precipitates formed due to the in-situ reactions between the boron-carbide and titanium powders. The precipitation of TiB 2 resulted in the formation of a graphitic C-rich thin layer circumscribing the partially reacted B 4 C particles. Further progression of the in-situ reaction leads to the out-diffusion of the excess carbon from the B 4 C particles, across the graphite and TiB 2 phases, forming TiC upon reacting with the titanium matrix. Therefore, the final microstructure primarily consisted of TiB 2 , TiC, and partially reacted B 4 C phases, with small amounts of TiB, α-Ti, and graphite. Furthermore, the microstructure in these SPS processed in situ composites appeared to be the product of a solid-state Ti–B 4 C diffusion couple, substantially different from their fusion-based additively manufactured counterparts. Nano-indentation tests revealed a remarkably high average hardness of ~25 GPa for this SPS-processed Ti–B 4 C composite and comparable (with literature) phase-specific hardness and modulus values for the constituent TiB 2 , TiC, and B 4 C phases.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Crystallographic ordering of Al and Sn in α-Ti

Increasing attention is being paid to α (2) Ti 3 (Al,Sn) precipitation from the α phase of titanium alloys owing to its effect on slip band formation, localisation and the implications for fatigue performance in jet engine titanium. However, the early stages of α 2 precipitation have historically been difficult to observe by electron microscopy, neutron diffraction or atom probe analysis. Here, small angle X-ray scattering is used to reexamine the phase boundary in binary Ti-Al and Ti-Sn alloys with around 500 ppmw O. It is found that the phase boundaries in the literature are approximately correct, at 6.2 wt.% Al and 16.9 wt.% Sn, and that this favours the use of Al as a solid solution strengthener over Sn for ambient temperature applications. However, once O content and phase partitioning in α + β alloys are taken into account, this implies that Al eq limits for future alloy design of critical rotating parts should be lowered substantially.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Design of a high-temperature cell for cobalt-60 irradiations of aqueous solutions with in situ UV–visible spectroscopy

To understand the speciation of solutes in aqueous solutions in high temperature radiation environments, we report the design and fabrication of a custom-built, high temperature (≤300 °C) titanium irradiation cell with in situ optical spectroscopy capabilities, as afforded by coupled fiber optic cables. The wetted surfaces of the 8-inch tall cylindrical cell with 3.5 in. diameter are entirely made of titanium, sapphire, and gold, which are chemically and radiolytically inert. The initial benchmarking results are reported, including the baseline spectrum of deionized water as a function of temperature, the stability of a spectrum over 4 h at 100 °C, and an irradiated Fricke dosimetry solution under ambient irradiator temperature conditions (27.0 ± 0.5 °C). Further, the average gamma radiation dose rate in the cell in its current configuration is 26.1 ± 1.3 Gy min -1 . This cell has application in studying several processes throughout the nuclear fuel cycle, including the reactor coolant behavior.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2020

Synthesis of TiO{sub 2} nanoparticles decorated with gold nanoclusters using pulsed laser ablation in liquid

Amorphous spherical titanium dioxide (TiO{sub 2}) nanoparticles, decorated gold nanoparticles, are shown to be formed under irradiation of commercial TiO{sub 2} nanopowders dispersed in aqueous solution of hydrogen tetrachloroaurate (HAuCl{sub 4}) by second-harmonic nanosecond pulses of an Nd : YAG laser. It is found that these hybrid nanostructures are formed during laser-induced remelting of the initial nanoparticles, stimulated by gold nanoclusters (providing more efficient absorption of visible laser radiation by titanium dioxide) recovered on their surface. The morphology and chemical composition of the newly formed hybrid nanomaterials are investigated in detail by electron microscopy, Raman spectroscopy, and energy-dispersive analysis. It is shown that the average size and number of gold nanoparticles recovered on the TiO{sub 2} surface can be controlled by varying the concentration ratio of the initial nanomaterial and HAuCl{sub 4}. A spectroscopic analysis of light scattering by single hybrid nanoparticles and the results of numerical calculation of the structure of electromagnetic fields near their surface indicate good prospects of these hybrid nanomaterials for various applications in modern optics, optoelectronics, and nanophotonics; for example, for designing chemo- and biosensor platforms and new-generation solar cells. (nanoparticles)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2022

Improving the damage tolerance of Si 3 N 4 by forming laminate composites with refractory metals

The objective of this research was to demonstrate that the damage tolerance of Si 3 N 4 could be significantly improved by forming laminate composites with refractory metals, providing materials that undergo graceful failure, rather than the fast-fracture mechanism exhibited by monolithic Si 3 N 4 . A damage tolerant Si 3 N 4 could be used as a ring material in an all-ceramic bearing, decreasing the chance for catastrophic failure if the ring is stressed in tension during operation. The technical approach formed a laminate composite material using alternating Si 3 N 4 -metallic layers, with both outer layers being Si 3 N 4 to take advantage of its greater wear resistance, chemical stability, and thermal stability. The metallic layers are designed to arrest any cracks in the outer layers, thus producing a toughened Si 3 N 4 and avoiding the catastrophic failure behavior exhibited by monolithic ceramics. The laminate composites were fabricated using a combination of tape-casting Si 3 N 4 and metals from slurries, as well as metal foils, followed by hot pressing at 1500°C. The metallic materials employed were chromium, titanium, and tantalum. Analysis confirmed that the interfaces were well formed, and the laminates with chromium and titanium formed intermetallic compounds more readily than the composites with tantalum. The Si 3 N 4 -Ta laminates demonstrated crack deflection and bridging behavior during failure and flexural strength of 800–900 MPa. The hardness and elastic modulus of Si 3 N 4 -Ta laminates measured by nanoindentation were similar to those reported in literature. The hardness across the interface of the Si 3 N 4 -Ta composite varied according to the composition of the interface, which displayed a profile indicative of a diffusion bond.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Industrial Scalable Additives for Enhanced Decomposition of Plastic Waste Through Photocatalysis

Polymer pollution is a dangerous environmental problem that can lead to the spread of toxic chemicals and microplastics throughout aquatic biomes. Commonly littered plastic from consumer goods and products with a limited or single use can be embedded with photocatalysts to avoid an increase in the amount of plastic present in Earth’s bodies of water. In this work, the photocatalyst nanoparticles, less than 100 nm particle size, were integrated into polyethylene terephthalate, high-density polyethylene, low-density polyethylene, and polystyrene and exposed under ultraviolet light over two independent experimental trials examining both the environmental factors impacting decay and the physical parameters required to implement this solution on a large scale. The plastics were chosen due to their prolific use in items such as grocery bags, bottles, and packaging. The first half of the project examined the effects of water and light frequency on polymer decay, and the second half of the project examined photodecomposition of polymer films. We report that low-density and high-density polyethylene films with titanium dioxide decayed approximately 11.7 and 9.6 faster than control samples, respectively. With an estimated price of less than half the cost of a shopping bag for titanium catalyst integration and a retention of the polymer’s tensile strength with a 2 wt% catalyst concentration, photocatalytic decomposition is a feasible, scalable method for the prevention and future reduction of polymer waste from realistic products littered in the environment.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Engineering Na‐Rich P2‐Type Layered Oxides Through Li/Ti Dual Doping for Oxygen Redox Activation and Superior Structural Stability

Sodium layered oxides Na x MO 2 (x ≤ 1 and M = transition metal ions) have gained significant interest as sodium-ion battery (NIB) cathodes owing to their high operating voltages and potential for higher energy density compared with polyanion and Prussian blue–type cathodes. However, their practical applications are often hindered by the irreversible structural transitions leading to capacity fading during cycling. The nature and substitution of transition metal ions define the material properties and electrochemical performance. In this study, through comprehensive electrochemical characterization combined with multi-scale structural and spectroscopical analyses, we demonstrate the synergistic impacts of Lithium and Titanium doping, which not only increases overall capacity by boosting cation and anion cooperative redox contributions but also improves the rate capability and cycling stability. Specifically, Li + doping enhances the available sodium inventory for extraction, while Ti 4+ disrupts Na + /vacancy ordering at lower voltages (< 4 V) and mitigates the detrimental P2→OP4/O2 phase transition during cycling. The combined effect of Lithium and Titanium doping promotes more charge localization on Oxygen, which activates reversible lattice oxygen redox reactions at elevated voltages, contributing additional capacity beyond conventional cationic redox. This work provides crucial insights into the design of high-performance, high-capacity P2-type layered cathode materials for sodium-ion batteries.

36 MATERIALS SCIENCE↗

DOE OSTI2023

In Situ Scattering Studies of Superconducting Vacancy‐Ordered Monoclinic TiO Thin Films

Abstract The structural and transport properties of vacancy‐ordered monoclinic superconducting titanium oxide (TiO) thin films grown by molecular beam epitaxy are investigated. The evolution of the crystal structure during growth is monitored by in situ synchrotron X‐ray diffraction. Long‐range ordering of Ti and O vacancies in the disordered cubic phase stabilizes the vacancy‐ordered monoclinic TiO phase. The reduced structural disorder arising from vacancy‐ordering is correlated with a superconductor‐metal transition (SMT) in contrast to the superconductor‐insulator transition (SIT) observed in cubic TiO, orthorhombic Ti 2 O 3 , and the Magneli γ − Ti 3 O 5 and γ − Ti 4 O 7 phase. Magnetoresistance measurements for the SIT phases indicate superconducting fluctuations persisting in the normal phase. These results confirm the role of disorder related to Ti and O vacancies and structural inhomogeneity in determining the electronic properties of the normal state of titanium oxide‐based superconductors.

Baksi, Merve↗