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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 109 records · Page 6
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

In Situ Study of Resistive Switching in a Nitride‐Based Memristive Device

Abstract Resistive switching (RS) devices with ultra‐low‐voltage threshold and reliable switching repeatability exhibits great potential applications in energy‐efficient data storage and neuromorphic computing. Understanding switching mechanisms at nanoscale is critical to design RS devices with improved performance. In this work, a lamella memristive device using focused ion beam (FIB) method based on the metal/TiO x /TiN/Si structure device is fabricated. In situ transmission electron microscopy (TEM) and current–voltage ( I–V ) characteristic demonstrate that the lamella device shows a volatile RS behavior with a threshold switching at ≈ ± 0.4 V. In situ scanning transmission electron microscopy (STEM) experiments with electron energy loss spectroscopy (EELS) reveal that the charge carriers such as oxygen vacancies migrate under positive/negative DC bias and modulate Schottky barriers at the top and bottom metal/semiconductor interfaces. The RS mechanism of the lamella device is based on the Schottky barriers modulation and Joule heating assisted electric field triggered thermal runaway (FTTR) occurred at the metal/semiconductor interfaces. The fundamental insights gained from this study presents a perspective on interface‐type RS devices processing and opens up new technological opportunities of fabricating ultra‐low‐energy memristive devices.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Stable Anode–Free All–Solid–State Lithium Battery through Tuned Metal Wetting on the Copper Current Collector

A stable anode-free all-solid-state battery (AF-ASSB) with sulfide-based solid-electrolyte (SE) (argyrodite Li 6 PS 5 Cl) is achieved by tuning wetting of lithium metal on “empty” copper current-collector. Lithiophilic 1 µm Li 2 Te is synthesized by exposing the collector to tellurium vapor, followed by in situ Li activation during the first charge. The Li 2 Te significantly reduces the electrodeposition/electrodissolution overpotentials and improves Coulombic efficiency (CE). During continuous electrodeposition experiments using half-cells (1 mA cm –2 ), the accumulated thickness of electrodeposited Li on Li 2 Te–Cu is more than 70 µm, which is the thickness of the Li foil counter-electrode. Full AF-ASSB with NMC811 cathode delivers an initial CE of 83% at 0.2C, with a cycling CE above 99%. Additionally, cryogenic focused ion beam (Cryo-FIB) sectioning demonstrates uniform electrodeposited metal microstructure, with no signs of voids or dendrites at the collector-SE interface. Electrodissolution is uniform and complete, with Li 2 Te remaining structurally stable and adherent. By contrast, an unmodified Cu current-collector promotes inhomogeneous Li electrodeposition/electrodissolution, electrochemically inactive “dead metal,” dendrites that extend into SE, and thick non-uniform solid electrolyte interphase (SEI) interspersed with pores. Density functional theory (DFT) and mesoscale calculations provide complementary insight regarding nucleation-growth behavior. Unlike conventional liquid-electrolyte metal batteries, the role of current collector/support lithiophilicity has not been explored for emerging AF-ASSBs.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Reactive Carbide‐Based Synthesis and Microstructure of NASICON Sodium Metal All Solid‐State Electrolyte

Reactive carbide precursor-based synthesis of NASICON-type NZSP (Na 1+x Zr 2 Si x P 3-x O 12 ) solid-state electrolyte (SSE) is demonstrated, in contrast to the established oxide-based approach. Exothermic decomposition of ZrC and SiC in air homogenizes microstructure, yielding 98% compact density after conventional sintering at 1200 °C. Quantitative stereology demonstrates that significant microstructural differences are present. Compacts of carbide-derived Carb-NZSP are 98% dense with a secondary zirconium oxide (ZrO 2 ) volume fraction of 0.2% ± 0.3%, versus 93% dense and 3% ± 1% for oxide-derived baseline. For Carb-NZSP, the secondary glassy phosphate phase is agglomerated, while for baseline, it is dispersed and percolated. Electrochemical testing combined with post-mortem analysis demonstrates how microstructural control of secondary phases is critical for dendrite suppression: Carb-NZSP critical current density (CCD) is 3.1 ± 0.8 mA cm −2 at 0.1 mAh cm −2 , versus 1.0 ± 0.7 mA cm −2 at 0.1 mAh cm −2 . Cryogenic focused ion beam (cryo-FIB) analysis demonstrates that in both materials, the porous 2D sheet-like sodium metal dendrites propagate around and subsume NZSP grains, likely following a path enriched with glassy phase and with porosity. Dendrites also flow around isolated zirconia particles. Phase field simulation reveals deflection of dendrites by mechanically tough zirconia, while brittle glassy phase accelerates dendrite growth, especially when finely distributed.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Fabrication and Characterization of Composite Membranes for the Concentration of Lithium Containing Solutions Using Forward Osmosis

In this study, an energy and highly time efficient, cost effective, and scalable forward osmosis (FO) composite polyvinylidene fluoride (PVDF) membrane is developed to concentrate lithium chloride recovered from naturally occurring geothermal brine resources. Dense thin robust defect-free Kynar-PVDF membranes are fabricated on porous PVDF hollow fiber supports. Various membrane fabrication parameters such as membrane thickness, coating solution concentration, cross-linker concentration, and curing temperature are studied to develop a defect-free dense membrane. Advanced characterization tools such as FIB-SEM, Raman, FTIR spectroscopy, and XRD are used to study the surface and cross-sectional morphology, chemistry of crosslinking, crystallinity and chemical structure of the dense PVDF membrane. FO is utilized to concentrate LiCl in the solution from 36 to 175 g L -1 with an average water transfer rate of 0.450 L m -2 h -1 (LMH) at 85 °C. Furthermore, the membrane showed stable performance for more than 550 h while maintaining the purity of the concentrated lithium chloride solution of >99.99 wt%. Overall, the results suggest that the FO-based technology is an innovative, time and energy efficient approach compared to the conventional technologies for concentration of battery grade LiCl for application in lithium ion batteries and other clean energy technologies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Accelerated Short Circuiting in Anode-Free Solid-State Batteries Driven by Local Lithium Depletion

“Anode-free” solid-state batteries (SSBs), which have no anode active material, can exhibit extremely high energy density (≈1500 Wh L -1 ). However, there is a lack of understanding of the lithium plating/stripping mechanisms at initially lithium-free solid-state electrolyte (SSE) interfaces because excess lithium metal is often used. Here, it is demonstrated that commercially relevant quantities of lithium (>5 mAh cm -2 ) can be reliably plated at moderate current densities (1 mA cm -2 ) using the sulfide SSE Li 6 PS 5 Cl. Investigations of lithium plating/stripping mechanisms, in conjunction with cryo-ocused ion beam (FIB) imaging, synchrotron tomography, and phase-field modeling, reveal that the cycling stability of these cells is fundamentally limited by the nonuniform presence of lithium during stripping. Local lithium depletion causes isolated lithium regions toward the end of stripping, decreasing electrochemically active area and resulting in high local current densities and void formation. This accelerates subsequent filament growth and short circuiting compared to lithium-excess cells. Despite this degradation mode, here it is shown that anode-free cells exhibit comparable Coulombic efficiency to lithium-excess cells, and improved resistance to short circuiting is achieved by avoiding local lithium depletion through retention of thicker lithium at the interface. These new insights provide a foundation for engineering future high-energy anode-free SSBs.

25 ENERGY STORAGE↗
DOE OSTI2023

Intermetallics Based on Sodium Chalcogenides Promote Stable Electrodeposition–Electrodissolution of Sodium Metal Anodes

Sodiophilic micro-composite films of sodium-chalcogenide intermetallics (Na 2 Te and Na 2 S) and Cu particles are fabricated onto commercial copper foam current collectors (Na 2 Te@CF and Na 2 S@CF). For the first time a controllable capacity thermal infusion process is demonstrated. Enhanced wetting by the metal electrodeposition leads to state-of-the-art electrochemical performance. For example, Na 2 Te@CF-based half-cells demonstrate stable cycling at 6 mA cm -2 and 6 mAh cm -2 , corresponding to 54 µm of Na electrodeposited/electrodissolved by geometric area. Sodium metal batteries with Na 3 V 2 (PO 4 ) 3 cathodes are stable at 30C (7 mA cm -2 ) and for 10 000 cycles at 5C and 10C. Cross-sectional cryogenic focused ion beam (cryo-FIB) microscopy details deposited and remnant dissolved microstructures. Sodium metal electrodeposition onto Na 2 Te@CF is dense, smooth, and free of dendrites or pores. On unmodified copper foam, sodium grows in a filament-like manner, not requiring cycling to achieve this geometry. Substrate–metal interaction critically affects the metal–electrolyte interface, namely the thickness and morphology of the solid electrolyte interphase. Density functional theory and mesoscale simulations provide insight into support-adatom energetics, nucleation response, and early-stage morphological evolution. On Na 2 Te sodium atomic dispersion is thermodynamically more stable than isolated clusters, leading to conformal adatom coverage of the surface.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Tuned Reactivity at the Lithium Metal–Argyrodite Solid State Electrolyte Interphase

Thin intermetallic Li 2 Te–LiTe 3 bilayer (0.75 µm) derived from 2D tellurene stabilizes the solid electrolyte interphase (SEI) of lithium metal and argyrodite (LPSCl, Li 6 PS 5 Cl) solid-state electrolyte (SSE). Tellurene is loaded onto a standard battery separator and reacted with lithium through single-pass mechanical rolling or transferred directly to SSE surface by pressing. State-of-the-art electrochemical performance is achieved, e.g., symmetric cell stable for 300 cycles (1800 h) at 1 mA cm -2 and 3 mAh cm -2 (25% DOD, 60 µm foil). Cryo-stage focused ion beam (Cryo-FIB) sectioning and Raman mapping demonstrate that the Li 2 Te–LiTe 3 bilayer impedes SSE decomposition. The unmodified Li–LPSCl interphase is electrochemically unstable with a geometrically heterogeneous reduction decomposition reaction front that extends deep into the SSE. Decomposition drives voiding in Li metal due to its high flux to the reaction front, as well as voiding in the SSE due to the associated volume changes. Analysis of cycled SSE found no evidence for pristine (unreacted) lithium metal filaments/dendrites, implying failure driven by decomposition phases with sufficient electrical conductivity that span electrolyte thickness. In conclusion, DFT calculations clarify thermodynamic stability, interfacial adhesion, and electronic transport properties of interphases, while mesoscale modeling examines interrelations between reaction front heterogeneity (SEI heterogeneity), current distribution, and localized chemo-mechanical stresses.

25 ENERGY STORAGE↗
DOE OSTI2024

Mechanical Milling – Induced Microstructure Changes in Argyrodite LPSCl Solid-State Electrolyte Critically Affect Electrochemical Stability

Microstructure of argyrodite solid-state electrolyte (SSE) critically affects lithium metal electrodeposition/dissolution. While the stability of unmodified SSE is mediocre, once optimized state-of-the-art electrochemical performance is achieved (symmetric cells, full cells with NMC811) without secondary interlayers or functionalized current collectors. Planetary mechanical milling in wet media (m-xylene) is employed to alter commercial Li 6 PS 5 Cl (LPSCl) powder. Quantitative stereology demonstrates how milling progressively refines grain and pore size/distribution in the SSE compact, increases its density, and geometrically smoothens the SSE-Li interface. Mechanical indentation demonstrates that these changes lead to reduced site-to-site variation in the compact's hardness. Milled microstructures promote uniform early-stage electrodeposition on foil collectors and stabilize solid electrolyte interphase (SEI) reactivity. Analysis of half-cells with bilayer electrolytes demonstrates the importance of microstructure directly contacting current collector, with interface roughness due to pore and grain size distribution being key. For the first time, short-circuiting Li metal dendrite is directly identified, employing 1.5 mm diameter “mini” symmetrical cell and cryogenic focused ion beam (cryo-FIB) electron microscopy. The branching sheet-like dendrite traverses intergranularly, filling the interparticle voids and forming an SEI around it. Importantly, mesoscale modeling reveals the relationship between Li-SSE interface morphology and the onset of electrochemical instability, based on underlying reaction current distribution.

25 ENERGY STORAGE↗
DOE OSTI2025

Mitigating Battery Cell Failure: Role of Ag‐Nanoparticle Fillers in Solid Electrolyte Dendrite Suppression

Abstract The development of solid‐state batteries (SSBs) with lithium Li metal anodes holds significant promise for enhancing the energy density and safety of next‐generation energy storage systems. However, their commercialization is hindered by challenges related to Li dendrite formation, which can lead to short circuits and battery failure. In this study, the role of Ag nanoparticles embedded within solid electrolytes (SE) is investigated in suppressing dendrite propagation. The results demonstrate that Ag nanoparticles effectively mitigate two key failure mechanisms: (1) dendrite growth within porous networks at low current densities and (2) stress intensification‐induced SE fracture at higher current densities (12 mA cm −2 ). Ex situ characterization using focused‐ion beam – scanning electron microscopy (FIB–SEM) and energy dispersive X‐ray spectroscopy (EDS,) reveals that Ag nanoparticles migrate alongside advancing Li dendrites, promoting homogeneous dendrite growth and reducing the likelihood of localized stress concentrations. Additionally, the incorporation of Ag nanoparticles is shown to facilitate a more uniform Li distribution toward the anode side, which can potentially enable the use of higher charging rates in SSBs. This study provides a new perspective on Li dendrite suppression and presents new opportunities for enhancing the performance and safety of SSBs.

Diallo, Mouhamad Said↗
DOE OSTI2023

Influence of Potassium Metal‐Support Interactions on Dendrite Growth

Abstract Combined synchrotron X‐ray nanotomography imaging, cryogenic electron microscopy (cryo‐EM) and modeling elucidate how potassium (K) metal‐support energetics influence electrodeposit microstructure. Three model supports are employed: O‐functionalized carbon cloth (potassiophilic, fully‐wetted), non‐functionalized cloth and Cu foil (potassiophobic, nonwetted). Nanotomography and focused ion beam (cryo‐FIB) cross‐sections yield complementary three‐dimensional (3D) maps of cycled electrodeposits. Electrodeposit on potassiophobic support is a triphasic sponge, with fibrous dendrites covered by solid electrolyte interphase (SEI) and interspersed with nanopores (sub‐10 nm to 100 nm scale). Lage cracks and voids are also a key feature. On potassiophilic support, the deposit is dense and pore‐free, with uniform surface and SEI morphology. Mesoscale modeling captures the critical role of substrate‐metal interaction on K metal film nucleation and growth, as well as the associated stress state.

Liu, Pengcheng↗
DOE OSTI2024

Interdependence of Support Wettability ‐ Electrodeposition Rate‐ Sodium Metal Anode and SEI Microstructure

Abstract This study examines how current collector support chemistry (sodiophilic intermetallic Na 2 Te vs. sodiophobic baseline Cu) and electrodeposition rate affect microstructure of sodium metal and its solid electrolyte interphase (SEI). Capacity and current (6 mAh cm −2 , 0.5–3 mA cm −2 ) representative of commercially relevant mass loading in anode‐free sodium metal battery (AF‐SMBs) are analyzed. Synchrotron X‐ray nanotomography and grazing‐incidence wide‐angle X‐ray scattering (GIWAXS) are combined with cryogenic ion beam (cryo‐FIB) microscopy. Highlighted are major differences in film morphology, internal porosity, and crystallographic preferred orientation e.g. (110) vs. (100) and (211) with support and deposition rate. Within the SEI, sodium fluoride (NaF) is more prevalent with Te−Cu versus sodium hydride (NaH) and sodium hydroxide (NaOH) with baseline Cu. Due to competitive grain growth the preferred orientation of sodium crystallites depends on film thickness. Mesoscale modeling delineates the role of SEI (ionic conductivity, morphology) on electrodeposit growth and onset of electrochemical instability.

Lo, Chang‐An↗
DOE OSTI2023

Influence of Potassium Metal-Support Interactions on Dendrite Growth

We report combined synchrotron X-ray nanotomography imaging, cryogenic electron microscopy (cryo-EM) and modeling elucidate how potassium (K) metal-support energetics influence electrodeposit microstructure. Three model supports are employed: O-functionalized carbon cloth (potassiophilic, fully-wetted), non-functionalized cloth and Cu foil (potassiophobic, nonwetted). Nanotomography and focused ion beam (cryo-FIB) cross-sections yield complementary three-dimensional (3D) maps of cycled electrodeposits. Electrodeposit on potassiophobic support is a triphasic sponge, with fibrous dendrites covered by solid electrolyte interphase (SEI) and interspersed with nanopores (sub-10 nm to 100 nm scale). Lage cracks and voids are also a key feature. On potassiophilic support, the deposit is dense and pore-free, with uniform surface and SEI morphology. Mesoscale modeling captures the critical role of substrate-metal interaction on K metal film nucleation and growth, as well as the associated stress state.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Alumina – Stabilized SEI and CEI in Potassium Metal Batteries

Aluminum oxide (Al 2 O 3 ) nanopowder is spin-coated onto both sides of commercial polypropene separator to create artificial solid-electrolyte interphase (SEI) and artificial cathode electrolyte interface (CEI) in potassium metal batteries (KMBs). Here, this significantly enhances the stability, including of KMBs with Prussian Blue (PB) cathodes. For example, symmetric cells are stable after 1,000 cycles at 0.5 mA/cm 2 –0.5 mAh/cm 2 and 3.0 mA/cm 2 –0.5 mAh/cm 2 . Alumina modified separators promote electrolyte wetting and increase ionic conductivity (0.59 vs. 0.2 mS/cm) and transference number (0.81 vs. 0.23). Cryo-stage focused ion beam (cryo-FIB) analysis of cycled modified anode demonstrates dense and planar electrodeposits, versus unmodified baseline consisting of metal filaments (dendrites) interspersed with pores and SEI. Alumina-modified CEI also suppresses elemental Fe crossover and reduces cathode cracking. Mesoscale modeling of metal – SEI interactions captures crucial role of intrinsic heterogeneities, illustrating how artificial SEI affects reaction current distribution, conductivity and morphological stability.

25 ENERGY STORAGE↗
DOE OSTI2024

3D‐Printed Carbon Nanoneedle Electrodes for Dopamine Detection in Drosophila

In vivo electrochemistry in small brain regions or synapses requires nanoelectrodes with long straight tips for submicron scale measurements. Nanoelectrodes can be fabricated using a Nanoscribe two-photon printer, but annealed tips curl if they are long and thin. We propose a new pulling-force strategy to fabricate a straight carbon nanoneedle structure. A micron-width bridge is printed between two blocks. The annealed structure shrinks during pyrolysis, and the blocks create a pulling force to form a long, thin, and straight carbon bridge. Parameterization study and COMSOL modeling indicate changes in the block size, bridge size and length affect the pulling force and bridge shrinkage. Electrodes were printed on niobium wires, insulated with aluminum oxide, and the bridge cut with focused ion beam (FIB) to expose the nanoneedle tip. Annealed needle diameters ranged from 400 nm to 5.25 μm and length varied from 50.5 μm to 146 μm. The electrochemical properties are similar to glassy carbon, with good performance for dopamine detection with fast-scan cyclic voltammetry. Nanoelectrodes enable biological applications, such as dopamine detection in a specific Drosophila brain region. Long and thin nanoneedles are generally useful for other applications such as cellular sensing, drug delivery, or gas sensing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Interdependence of Support Wettability - Electrodeposition Rate- Sodium Metal Anode and SEI Microstructure

Here, this study examines how current collector support chemistry (sodiophilic intermetallic Na 2 Te vs. sodiophobic baseline Cu) and electrodeposition rate affect microstructure of sodium metal and its solid electrolyte interphase (SEI). Capacity and current (6 mAh cm -2 , 0.5–3 mA cm -2 ) representative of commercially relevant mass loading in anode-free sodium metal battery (AF-SMBs) are analyzed. Synchrotron X-ray nanotomography and grazing-incidence wide-angle X-ray scattering (GIWAXS) are combined with cryogenic ion beam (cryo-FIB) microscopy. Highlighted are major differences in film morphology, internal porosity, and crystallographic preferred orientation e.g. (110) vs. (100) and (211) with support and deposition rate. Within the SEI, sodium fluoride (NaF) is more prevalent with Te-Cu versus sodium hydride (NaH) and sodium hydroxide (NaOH) with baseline Cu. Due to competitive grain growth the preferred orientation of sodium crystallites depends on film thickness. Mesoscale modeling delineates the role of SEI (ionic conductivity, morphology) on electrodeposit growth and onset of electrochemical instability.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Ternary Potassium‐Bismuth‐Telluride Intermetallic Support Promotes Electrochemical Stability in Potassium Metal Anodes

We employed accumulative roll bonding to fabricate self‐standing metallurgical composite of in situ formed alkaline potassium‐bismuth‐telluride intermetallic K 2 (Bi 2/6 Te 3/6 Vac 1/6 ) embedded in potassium metal. This newly discovered thermodynamically stable potassiophilic crystal, termed “KBT”, is fcc antifluorite with K 2 Te archetype. Symmetric cells achieve 880 h of cycling at 0.5 mA cm −2 and 0.5 mAh cm −2 . Potassium metal battery (KMB) with Prussian blue (PB) cathode in carbonate electrolyte retains 80% capacity after 200 cycles at 1C. In ether‐based electrolyte with organic cathode, it achieves 80% retention after 900 cycles at 2C. Combined synchrotron X‐ray nano‐tomography, cryogenic‐focused ion beam microscopy (Cryo‐FIB) and sputter‐down X‐ray photoelectron spectroscopy (XPS) demonstrate uniform electrodeposits, versus baseline of potassium filaments intermixed with pores and coarse SEI. Binary K 3 Bi‐K and K 2 Te‐K intermetallic supports also provide improved electrochemical performance, albeit to lesser extent. Multiscale simulation provides insight into role of support structure in adatom energetics, film nucleation, early‐stage SEI morphology and interfacial stability.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Working Principle of an Ionic Liquid Interlayer During Pressureless Lithium Stripping on Li 6.25 Al 0.25 La 3 Zr 2 O 12 (LLZO) Garnet‐Type Solid Electrolyte

Abstract Solid‐state‐batteries employing lithium metal anodes promise high theoretical energy and power densities. However, morphological instability occurring at the lithium/solid–electrolyte interface when stripping and plating lithium during cell cycling needs to be mitigated. Vacancy diffusion in lithium metal is not sufficiently fast to prevent pore formation at the interface above a certain current density during stripping. Applied pressure of several MPa can prevent pore formation, but this is not conducive to practical application. This work investigates the concept of ionic liquids as “self‐adjusting” interlayers to compensate morphological changes of the lithium anode while avoiding the use of external pressure. A clear improvement of the lithium dissolution process is observed as it is possible to continuously strip more than 70 μm lithium (i. e., 15 mAh cm −2 charge) without the need for external pressure during assembly and electrochemical testing of the system. The impedance of the investigated electrodes is analyzed in detail, and contributions of the different interfaces are evaluated. The conclusions are corroborated with morphology studies using cryo‐FIB‐SEM and chemical analysis using XPS. This improves the understanding of the impedance response and lithium stripping in electrodes employing liquid interlayers, acting as a stepping‐stone for future optimization.

Fuchs, Till↗
DOE OSTI2022

Inhibition of Micro-pitting by Tribofilm-Forming ZrO 2 Nanocrystal Lubricant Additives: A Micro-pitting Rig and Transmission Electron Microscope Study

The drive to reduce fuel consumption in transportation has encouraged the emergence of low viscosity lubricants to reduce viscous losses in the engine, drivetrain, and other components. However, viscosity reduction increases the risk of surface damage, thus motivating the development of new anti-wear (AW) additives. Capped ZrO 2 nanocrystals (NCs) in base oils have been shown to form AW tribofilms within microscale sliding contacts. However, the potential of ZrO 2 NCs to protect surfaces subjected to rolling-sliding contact from macroscale damage, such as micro-pitting, remains unexplored. Here, we explore the ability of ZrO 2 NCs to form protective tribofilms under harsh conditions using a micro-pitting rig (MPR), consisting of a three ring-on-roller configuration. The experiments were conducted in polyalphaolephin (PAO) base oil, with and without 5 nm diameter ZrO 2 NCs, at two levels of slide-to-roll ratio (SRR) (30% and 0%) and at variable test durations up to long durations (119 h). MPR results showed the use of ZrO 2 NCs gives rise to the formation of a tribofilm covering the roller surfaces and decreases the initiation and propagation of micro-pits compared to tests in pure PAO base stock. Transmission electron microscopy (TEM) performed on focused ion beam (FIB) milled cross-sectional samples of the roller surfaces revealed the growth of dense and 50–100 nm thick ZrO 2 -based tribofilms independent of (SRR), indicating the potential for robust micro-pitting fatigue protection. Nevertheless, small cracks localized within the near surface region of the roller tested at the most severe conditions (30% SRR and 119 h) were observed. The initiation of these cracks was directly related to the presence of manganese sulphide (MnS) inclusions in the steel, revealed using TEM combined with energy dispersive spectroscopy (EDS). Furthermore, the results highlight the benefits of the protective tribofilms formed by ZrO 2 NCs and suggest approaches for further optimizing their use.

36 MATERIALS SCIENCE↗