Tailored Ni(OH) 2 /CuCo/Ni(OH) 2 Composite Interfaces for Efficient and Durable Urea Oxidation Reaction
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36 MATERIALS SCIENCE↗
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The General Isothermal Oxidation Behavior of Cu-8Cr-4Nb
Oxidation kinetics of Cu-8Cr-4Nb was investigated by TGA (thermogravimetric) exposures between 500 and 900-C (at 25-50 C intervals) and the oxide scale morphologies examined by microscopy and micro-analysis. Because Cu-8Cr-4Nb is comprised of fine Cr2Nb precipitates in a Cu matrix, the results were interpreted by comparison with the behavior of copper (OFHC) and 'NARloy-Z' (a rival candidate material for thrust cell liner applications in advanced rocket engines) under the same conditions. While NARloy-Z and Cu exhibited identical oxidation behavior, Cu-8Cr-4Nb differed markedly in several respects: below approx. 700 C its oxidation rates were significantly lower than those of Cu; At higher temperatures its oxidation rates fell into two categories: an initial rate exceeding that of Cu, and a terminal rate comparable to that of Cu. Differences in oxide morphologies paralleled the kinetic differences at higher temperature: While NARloy-Z and Cu produced a uniform oxide scale of Cu2O inner layer and CuO outer layer, the inner (Cu2O) layer on Cu-8Cr-4Nb was stratified, with a highly porous/spongy inner stratum (responsible for the fast initial kinetics) and a dense/blocky outer stratum (corresponding to the slow terminal kinetics). Single and spinel oxides of Nb and Cr were found at the interface between the oxide scale and Cu-8Cr-4Nb substrate and it appears that these oxides were responsible for its suppressed oxidation rates at the intermediate temperatures. No difference was found between Cu-8Cr-4Nb oxidation in air and in oxygen at 1.0 atm.
Thomas-Ogbuji, L. U.↗
Microstructure and Oxidation of a MAX Phase/Superalloy Hybrid Interface
Corrosion resistant, strain tolerant MAX phase coatings are of interest for turbine applications. Thin Cr2AlC MAX phase wafers were vacuum diffusion bonded to an advanced turbine disk alloy, LSHR, at 1100 C. The interface, examined by optical and scanning electron microscopy, revealed a primary diffusion zone consisting of ~ 10 micrometers of beta-Ni(Co)Al, decorated with various NiCoCrAl, MC and M3B2 precipitates. On the Cr2AlC side, an additional ~40 micrometers Al-depletion zone of Cr7C3 formed in an interconnected network with the beta-Ni(Co)Al. Oxidation of an exposed edge at 800 C for 100 h produced a fine-grained lenticular alumina scale over Cr2AlC and beta-Ni(Co)Al, with coarser chromia granules over the Cr7C3 regions. Subsequent growth of the diffusion layers was only ~ 5 micrometers in total. A residual stress of ~ 500 MPa was estimated for the MAX phase layer, but no interfacial damage was observed. Subsequent tests for 1000 h reveal similar results.
heat resistant alloys↗
Crystallographic and TEM Features of a TBC/Ti2AlC MAX Phase Interface after 1300°C Burner Rig Oxidation
A FIB/STEM interfacial study was performed on a TBC/Ti 2 AlC MAX phase system, oxidized in an aggressive burner rig test (Mach 0.3 at 1300 °C for 500 h). The 7YSZ TBC, α-Al 2 O 3 TGO, and MAXthal 211 TM Ti 2 AlC base were variously characterized by TEM/STEM, EDS, SADP, and HRTEM. The YSZ was a mix of “clean” featureless and “faulted” high contrast grains. The latter exhibited ferro-elastic domains of high Y content tetragonal t″ variants. No martensite was observed. The TGO was essentially a duplex α-Al 2 O 3 structure of inner columnar plus outer equiaxed grains. It maintained a perfectly intact, clean interface with the Ti 2 AlC substrate. The Ti 2 AlC substrate exhibited no interfacial Al-depletion zone but, rather, numerous faults along the basal plane of the hexagonal structure. These are believed to offer a means of depleting Al by forming crystallographic, low-Al planar defects, proposed as Ti 2.5 AlC 1.5 . These characterizations support and augment prior optical, SEM, and XRD findings that demonstrated remarkable durability for the YSZ/Ti 2 AlC MAX phase system in aggressive burner tests.
TI2AlC↗
Interface magnetism and anomalous Hall effect in La 0.7 Sr 0.3 MnO 3 /SrIrO 3 bilayers
Epitaxial interfaces combining 3d and 5d transition metal oxides are a fertile playground to examine the interplay between topology and electron correlations. In this work, we explore magnetism and transport of bilayers combining ferromagnetic La 0.7 Sr 0.3 MnO 3 and the strong spin-orbit coupling material SrIrO 3 . We have found an interfacial magnetic proximity effect driving an intrinsic contribution to the anomalous Hall effect of topological origin. The interfacial proximity interaction is enabled by the Mn-O-Ir bonding reconstruction and depends on layer sequence. While bilayers with the La 0.7 Sr 0.3 MnO 3 on top featuring a robust Mn magnetism at the interface show the intrinsic AHE contribution, it is absent in bilayers with the inverted layer sequence (SrIrO 3 layer on top) showing strongly suppressed magnetism at the interface. These results illustrate the leading role of interfacial atomic reconstructions on the interplay between topology and correlations at 3d/5d oxide interfaces. This finding may be of interest in future oxide topological spintronics and spin-orbitronics.
36 MATERIALS SCIENCE↗
Thermo-Oxidative Stability of Graphite/PMR-15 Composites: Effect of Fiber Surface Modification on Composite Shear Properties
Experiments were conducted to establish a correlation between the weight loss of a polyimide (PMR- 15) matrix and graphite fibers and the in-plane shear properties of their unidirectional composites subjected to different isothermal aging times up to 1000 hr at 316 C. The role of fiber surface treatment on the composite degradation during the thermo-oxidative aging was investigated by using A4 graphite fibers with three surface modifications: untreated (AU-4), surface treated (AS-4), and surface treated and sized with an epoxy-compatible sizing (AS-4G). The weight loss of the matrix fibers, and composites was determined during the aging. The effect of thermal aging was seen in all the fiber samples in terms of weight loss and reduction in fiber diameter. Calculated values of weight loss fluxes for different surfaces of rectangular unidirectional composite plates showed that the largest weight loss occurred at those cut surfaces where fibers were perpendicular to the surface. Consequently, the largest amount of damage was also noted on these cut surfaces. Optical observation of the neat matrix and composite plates subjected to different aging times revealed that the degradation (such as matrix microcracking and void growth) occurred in a thin surface layer near the specimen edges. The in-plane shear modulus of the composites was unaffected by the fiber surface treatment and the thermal aging. The shear strength of the composites with the untreated fibers was the lowest and it decreased with aging. A fracture surface examination of the composites with untreated fibers suggested that the weak interface allowed the oxidation reaction to proceed along the interface and thus expose the inner material to further oxidation. The results indicated that the fiber-matrix interface affected the composite degradation process during its thermal aging and that the the weak interface accelerated the composite degradation.
Madhukar, Madhu S.↗
Stressed Oxidation Life Prediction for C/SiC Composites
The residual strength and life of C/SiC is dominated by carbon interface and fiber oxidation if seal coat and matrix cracks are open to allow oxygen ingress. Crack opening is determined by the combination of thermal, mechanical and thermal expansion mismatch induced stresses. When cracks are open, life can be predicted by simple oxidation based models with reaction controlled kinetics at low temperature, and by gas phase diffusion controlled kinetics at high temperatures. Key life governing variables in these models include temperature, stress, initial strength, oxygen partial pressure, and total pressure. These models are described in this paper.
Levine, Stanley R.↗
Emergent Phenomena at Mott Interfaces – a Time- and Depth-Resolved Approach (Final Technical Report)
This is the final technical report for Award DE-SC0019297, Emergent Phenomena at Mott Interfaces – a Time- and Depth-Resolved Approach. This research program aimed to address the scientific questions related to the emergence and control of non-equilibrium electronic phases of matter in strongly correlated Mott oxides and their interfaces. We were focusing specifically on exploiting the interfaces in heterostructures and superlattices, containing Mott oxides CaMnO 3 and LaNiO 3 because in such systems, precise control of electronic and magnetic structure in the ground state can be achieved through dimensionality, heterostructuring, interface termination, and lattice strain. We utilized advanced x-ray spectroscopic and scattering techniques, to investigate these phenomena. Additionally, we used intense THz electric-field pulses generated by a femtosecond laser to directly modify the electronic structure and magnetic states of the ultrathin LaNiO 3 and CaMnO 3 layers in such heterostructures, with the objectives of disentangling, understanding, and harnessing control over the intricate competing interactions responsible for two-dimensional magnetism and metal-insulator transition at the interfaces.
36 MATERIALS SCIENCE↗
Measuring the Thermodynamics of the Alloy/Scale Interface
A method is proposed for the direct measurement of the thermodynamic properties of the alloy and oxide compound at the alloy/scale interface observed during steady-state oxidation. The thermodynamic properties of the alloy/scale interface define the driving force for solid-state transport in the alloy and oxide compound. Accurate knowledge of thermodynamic properties of the interface will advance our understanding of oxidation behavior. The method is based on the concept of local equilibrium and assumes that an alloy+scale equilibrium very closely approximates the alloy/scale interface observed during steady-state oxidation. The thermodynamics activities of this alloy+scale equilibrium are measured directly by Knudsen effusion-cell mass spectrometer (KEMS) using the vapor pressure technique. The theory and some practical considerations of this method are discussed in terms of beta-NiAl oxidation.
Copland, Evan↗
XPS study of interface formation of CVD SiO2 on InSb
The interfacial chemistry of CVD SiO2 films deposited on thin native oxides grown on InSb substrates is examined using X-ray photoemission spectroscopy (XPS) and a relatively benign chemical etching technique for depth profiling. An intensity analysis of XPS spectra is used to derive the compositional structure of the interfaces obtained in the SiO2/native oxide/InSb system. Peak positions in these spectra are used to follow the change in substrate surface potential during the etch sequence, and to establish the chemical nature of the species formed during deposition and subsequent processing. Reaction of the substrate with oxygen resulted in an In-rich native oxide and 1-2 monolayers of excess elemental Sb at the native-oxide/substrate interface, incompletely oxidized silane reduced the native oxide, leaving less than 1 monolayer of elemental In at the SiO2/native oxide interface. Etch removal of this thin In-rich layer leads to a change in the substrate surface potential of 0.06 eV, corresponding to a net increase in positive charge. The results are consistent with simple thermodynamic considerations; they are also compared to previously reported studies of deposited dielectrics on III-V compound semiconductors.
Vasquez, R. P.↗
Enhancing Acidic Oxygen Evolution Activity by Controlling Oxidation State of Iridium
Iridium oxides with high oxidation states have been reported to be effective in enhancing the acidic oxygen evolution reaction (OER) performance. Herein, we develop ultrasmall IrO x nanoparticles (NPs) over titanium nitride (TiN), which undergoes surface oxidation under oxidative conditions to form oxygen-modified TiN (oxi-TiN), enabling the formation of highly oxidized Ir δ+ (δ > 4). This IrO x /oxi-TiN catalyst delivers higher Ir mass activity than commercial IrO 2 , while comparable stability is maintained. The superior OER activity of IrO x /oxi-TiN is further demonstrated in a proton exchange membrane water electrolyzer (PEMWE), requiring only 1.88 V to reach 3 A cm −2 , achieving the U.S. Department of Energy 2025 target (1.90 V at 3 A cm −2 ). In situ X-ray absorption spectroscopy (XAS) confirms that the superior OER activity of IrO x /oxi-TiN originates from highly oxidized Ir δ+ under OER conditions. Further, density functional theory (DFT) calculations reveal a general correlation between the oxidation state of Ir and OER overpotential. Specifically, the introduction of interfacial oxygen at the Ir/TiN interface increases the oxidation state of deposited Ir δ+ from δ < 4 to δ > 4, decreasing the OER overpotential. This study highlights the critical role of high oxidation states of Ir δ+ in enhancing OER activity, providing guidance for the development of advanced acidic OER catalysts.
In situ measurements↗
Enhancing Acidic Oxygen Evolution Activity by Controlling Oxidation State of Iridium
Iridium oxides with high oxidation states have been reported to be effective in enhancing the acidic oxygen evolution reaction (OER) performance. In this work, we develop ultrasmall IrO x nanoparticles (NPs) over titanium nitride (TiN), which undergoes surface oxidation under oxidative conditions to form oxygen‐modified TiN (oxi‐TiN), enabling the formation of highly oxidized Ir δ+ (δ > 4). This IrO x /oxi‐TiN catalyst delivers higher Ir mass activity than commercial IrO 2 , while comparable stability is maintained. The superior OER activity of IrO x /oxi‐TiN is further demonstrated in a proton exchange membrane water electrolyzer (PEMWE), requiring only 1.88 V to reach 3 A cm −2 , achieving the U.S. Department of Energy 2025 target (1.90 V at 3 A cm −2 ). In situ X‐ray absorption spectroscopy (XAS) confirms that the superior OER activity of IrO x /oxi‐TiN originates from highly oxidized Ir δ+ under OER conditions. Density functional theory (DFT) calculations reveal a general correlation between the oxidation state of Ir and OER overpotential. Specifically, the introduction of interfacial oxygen at the Ir/TiN interface increases the oxidation state of deposited Ir δ+ from δ < 4 to δ > 4, decreasing the OER overpotential. This study highlights the critical role of high oxidation states of Ir δ+ in enhancing OER activity, providing guidance for the development of advanced acidic OER catalysts.
58 GEOSCIENCES↗
Experimental observations of the chemistry of the SiO2/Si interface
Changes in silicon surface preparation prior to thermal oxidation are shown to leave a signature by altering the final SiO2/Si interface structure. Surface analytical techniques, including XPS, static SIMS, ion milling, and newly developed wet-chemical profiling procedures are used to obtain detailed information on the chemical structure of the interface. The oxides are shown to be essentially SiO2 down to a narrow transitional interface layer (3-7 A). A number of discrete chemical species are observed in this interface layer, including different silicon bonds (e.g., C-, OH-, H-) and a range of oxidation states of silicon (0 to +4). The effect of surface preparation and the observed chemical species are correlated with oxide growth rate, surface-state density, and flatband shifts after irradiation.
Grunthaner, F. J.↗
Some TEM observations of Al2O3 scales formed on NiCrAl alloys
The microstructural development of Al2O3 scales on NiCrAl alloys has been examined by transmission electron microscopy. Voids were observed within grains in scales formed on a pure NiCrAl alloy. Both voids and oxide grains grew measurably with oxidation time at 1100 C. The size and amount of porosity decreased towards the oxide-metal growth interface. The voids resulted from an excess number of oxygen vacancies near the oxidemetal interface. Short-circuit diffusion paths were discussed in reference to current growth stress models for oxide scales. Transient oxidation of pure, Y-doped, and Zr-doped NiCrAl was also examined. Oriented alpha-(Al, Cr)2O3 and Ni(Al, Cr)2O4 scales often coexisted in layered structures on all three alloys. Close-packed oxygen planes and directions in the corundum and spinel layers were parallel. The close relationship between oxide layers provided a gradual transition from initial transient scales to steady state Al2O3 growth.
Smialek, J.↗
Controlling Interfacial Charge Separation Energetics and Kinetics
The overall goal is to probe electron transfer kinetics of the Marcus inverted region at interfaces. This project specifically uses a dye‐semiconductor interface with a reversible electron transfer reagent in solution where the semiconductor conduction band and electron transfer reagent ideally have a potential energy difference firmly within the Marcus inverted region. The goals of this project are: (Goal 1) Identify dye design elements that give dyes with low energy ground‐state oxidation potentials while retaining desirable electron transfer kinetics at the semiconductor interface. (Goal 2) Identify dye designs with excited‐state oxidation potentials set to fixed energies through molecular design while the dye ground‐state oxidation potentials are varied to allow for the evaluation of varied electron transfer reagents/redox shuttles (RS) with different free energies for electron transfer. (Goal 3) Within the context of the functionality identified in goals 1 and 2, goal 3 seeks to design dyes with features maximizing charge carrier lifetimes by minimizing recombination losses at metal oxide interfaces with high voltage systems. (Goal 4) Probe electron transfer kinetics in a high voltage‐dye sensitized solar cell with both the oxidized dye and RS firmly within the Marcus inverted region with regard to the TiO2 CB. (Goal 5) Identify tailored sensitizer/redox shuttle pairs with desirable electron transfer kinetics in defined spectral regions capable of “banding off” incident solar irradiation to give high voltage multijunction systems capable of exceeding the Shockley‐Queisser limit and powering catalytic processes.
14 SOLAR ENERGY↗
First-Principles study of interface capture of Ni during high-temperature oxidation of NiCr alloys
The formation of precipitated phases of less reactive metals within an oxide scale during alloy oxidation can disrupt its structural integrity, significantly compromising the protective function of the oxide. To better understand this phenomenon, it is crucial to investigate the atomic-level diffusion mechanisms that drive precipitate formation. In this study, we employ first-principles calculations to examine the diffusion and aggregation of Ni atoms across the NiCr/Cr 2 O 3 interface during the high-temperature oxidation of NiCr alloys. Our results reveal that, in the absence of Cr vacancies, Ni atoms predominantly remain within the NiCr substrate, with minimal migration toward the Cr 2 O 3 layer. However, when Cr vacancies are present at both the NiCr/Cr 2 O 3 interface and within the Cr 2 O 3 bulk, Ni atoms exhibit a strong propensity to migrate from the NiCr substrate into the Cr 2 O 3 bulk, where they aggregate into Ni-rich regions with a corundum structure. This study provides valuable atomic-level insights into the diffusion and aggregation of less-reactive metals at the alloy/oxide interface, enhancing our understanding of solute capture and its contribution to the degradation of oxidation resistance in alloys.
Chen, Jianmin [Xiangtan University (China)] (ORCID↗
Electron escape depth variation in thin SiO2 films measured with variable photon energy
A double crystal monochromator at the Stanford Synchrotron Radiation Laboratory is used to study the Si/SiO2 interface, using photon energies of hv = 1950-3700 eV. This photon energy range allows interfaces to be observed through oxide layers 50 A thick or more. Variations in electron escape depth and/or oxide density as a function of distance from the interface are observed over the entire kinetic energy range (100-3600 eV). These differences are attributed to a strained oxide layer near the interface.
Hecht, M. H.↗
Charge Disproportionation at Twisted SrTiO 3 Bilayer Interface Driven by Local Atomic Registry
The interplay of lattice, orbital, and charge degrees of freedom in complex oxide materials has hosted a plethora of exotic quantum phases and physical properties. Recent advances in the synthesis of freestanding complex oxide membranes and twisted heterostructures assembled from membranes provide diverse opportunities for discovery using moiré design with local lattice control. To this end, we designed moiré crystals at the coincidence site lattice condition, providing commensurate structure within the moiré supercell arising from the multiatom complex oxide unit cell. We fabricated such twisted bilayers from freestanding SrTiO 3 membranes and used depth-sectioning-based electron microscopic methods to investigate ordered charge states at the moiré interface. By selectively imaging SrTiO 3 atomic planes at different depths through the bilayer, we clearly resolved the moiré periodic structure at the twisted interface and found that it exhibits lattice-dependent charge disproportionation in the local atomic registry within the moiré supercell. Density functional modeling of the twisted oxide interface predicts that these moiré phenomena are accompanied by a two-dimensional flat band that can drive exceptional electronic phases. Our work provides a robust strategy for controlling moiré periodicity in twisted oxides and paves pathways to exploit the extraordinary functionalities via moiré lattice-driven charge-orbital correlation.
charge disproportionation↗