Integrating Experimental and Computational Analyses for Mechanical Characterization of Titanium Carbide/Aluminum Metal Matrix Composites.

This study investigates the mechanical properties of titanium carbide/aluminum metal matrix composites (AMMCs) using both experimental and computational methods. Through accumulative roll bonding (ARB) and cryorolling (CR) processes, AA1050 alloy surfaces were reinforced with TiCp particles to create the Al-TiCp composite. The experimental analysis shows significant improvements in tensile strength, yield strength, elastic modulus, and hardness. The finite element analysis (FEA) simulations, particularly the microstructural modeling of RVE-1 (the experimental case model), align closely with the experimental results observed through scanning electron microscopy (SEM). This validation underscores the accuracy of the computational models in predicting the mechanical behavior under identical experimental conditions. The simulated elastic modulus deviates by 5.49% from the experimental value, while the tensile strength shows a 6.81% difference. Additionally, the simulated yield strength indicates a 2.85% deviation. The simulation data provide insights into the microstructural behavior, stress distribution, and particle-matrix interactions, facilitating the design optimization for enhanced performance. The study also explores the influence of particle shapes and sizes through Representative Volume Element (RVE) models, highlighting nuanced effects on stress-strain behavior. The microstructural evolution is examined via transmission electron microscopy (TEM), revealing insights regarding grain refinement. These findings demonstrate the potential of Al-TiCp composites for lightweight applications.

Microstructure and Mechanical Properties of AA1050/AA6061 Laminated Composites Fabricated through Three-Cycle Accumulative Roll Bonding and Subsequent Cryorolling.

In this study, AA1050/AA6061 laminated composites were prepared by three-cycle accumulative roll bonding (ARB) and subsequent rolling. The effects of the rolling process on the microstructure evolution and mechanical properties of AA1050/AA6061 laminated composites were systematically investigated. The results indicate that the mechanical properties of the laminated composites can be effectively improved by cryorolling compared with room-temperature rolling. The microstructure analysis reveals that cryorolling can suppress the necking of the hard layer to obtain a flat lamellar structure. Moreover, the microstructure characterized by transmission electron microscopy shows that cryorolling can inhibit the dynamic recovery and significantly refine the grain size of the constituent layers. Meanwhile, the tensile fracture surface illustrates that AA1050/AA6061 laminated composites have the optimal interfacial bonding quality after cryorolling. Therefore, the laminated composites obtain excellent mechanical properties with the contribution of these factors.

Liquid-Metal Solvents for Designing Hierarchical Nanoporous Metals at Low Temperatures.

Metallic nanoarchitectures hold immense value as functional materials across diverse applications. However, major challenges lie in effectively engineering their hierarchical porosity while achieving scalable fabrication at low processing temperatures. Here we present a liquid-metal solvent-based method for the nanoarchitecting and transformation of solid metals. This was achieved by reacting liquid gallium with solid metals to form crystalline entities. Nanoporous features were then created by selectively removing the less noble and comparatively softer gallium from the intermetallic crystals. By controlling the crystal growth and dealloying conditions, we realized the effective tuning of the micro-/nanoscale porosities. Proof-of-concept examples were shown by applying liquid gallium to solid copper, silver, gold, palladium, and platinum, while the strategy can be extended to a wider range of metals. This metallic-solvent-based route enables low-temperature fabrication of metallic nanoarchitectures with tailored porosity. By demonstrating large-surface-area and scalable hierarchical nanoporous metals, our work addresses the pressing demand for these materials in various sectors.

Large volume tomography using plasma FIB-SEM: A comprehensive case study on black silicon.

The xenon plasma focused ion beam and scanning electron microscopy (PFIB-SEM) system is a promising tool for 3D tomography of nano-scale materials, including nanotextured black silicon (BSi), whose topography is difficult to measure with conventional microscopy techniques. Advantages of PFIB-SEM include high material removal rates, precise control of milling parameters and automated slice-and-view procedures. However, there is no universal sample preparation procedure nor is there an established ideal workflow for the PFIB-SEM slice-and-view process. This work demonstrates that specimen preparation, including the orientation of the volume of interest, is critical for the quality of the final reconstructed 3D model. It thoroughly explores three unique configurations incrementally optimized for higher total throughput. All three sampling configurations are applied to a resin-embedded BSi sample to determine the most favourable workflow and highlight each approach's advantages and disadvantages. The reconstructed 3D models of the BSi surface obtained are shown to be qualitatively closer to the topography measured directly by SEM. The height distribution data extracted from the rendered 3D models reveal a higher structure depth compared to that obtained from an atomic force microscopy measurement. Furthermore, the work demonstrates how samples with different rigidity react to long-term ion-beam interaction, as both amorphous (resin) and crystalline (Si) material is present in the tested specimen. This study improves the understanding of sample-beam interaction and broadens the utility of the 3D PFIB-SEM for more complicated sample structures.

Modulating nitric oxide-generating activity of zinc oxide by morphology control and surface modification.

Zinc oxide (ZnO) has emerged as a promising material for nitric oxide (NO) delivery owing to its intrinsic enzyme-mimicking activities to catalyze NO prodrugs S-nitrosoglutathione (GSNO) and ß-gal-NONOate for NO generation. The catalytic performance of enzyme mimics is strongly dependent on their size, shape, and surface chemistry; however, no studies have evaluated the influence of the aforementioned factors on the NO-generating activity of ZnO. Understanding these factors will provide an opportunity to tune NO generation profiles to accommodate diverse biomedical applications. In this paper, for the first time, we demonstrate that the activity of ZnO towards catalytic NO generation is shape-dependent, resulting from the different crystal growth directions of these particles. We modified the surfaces of ZnO particles with zeolitic imidazolate framework (ZIF-8) by in situ synthesis and observed that ZnO/ZIF-8 retained 60% of its NO-generating potency. The newly formed ZnO/ZIF-8 particles were shown to catalytically decompose both endogenous (GSNO) and exogenous (ß-gal-NONOate and S-nitroso-N-acetylpenicillamine (SNAP)) prodrugs to generate NO at physiological conditions. In addition, we design the first platform that combines NO-generating and superoxide radical scavenging properties by encapsulating a natural enzyme, superoxidase dismutase (SOD), into ZnO/ZIF-8 particles, which holds great promise towards combinatorial therapy.

3D electron backscatter diffraction characterization of fine α titanium microstructures: collection, reconstruction, and analysis methods.

3D electron backscatter diffraction (3D-EBSD) is a method of obtaining 3-dimensional crystallographic data through serial sectioning. The recent advancement of using a Xe+ plasma focused ion beam for sectioning along with a complementary metal-oxide semiconductor based EBSD detector allows for an improvement in the trade-off between volume analyzed and spatial resolution over most other 3D characterization techniques. Recent publications from our team have focused on applying 3D-EBSD to understand microstructural phenomena in Ti-6Al-4V microstructures as a function of electron beam scanning strategies in electron beam powder bed fusion additive manufacturing. The microstructures resulting from this process have fine features, with α laths as small as 1 µm interwoven in a highly complex fashion, presenting a significant challenge to characterize. Over the course of these fundamental works, we have developed best-practice 3D-EBSD collection protocols and advanced methods for 3D data reconstruction and analysis of such microstructures which remain unpublished. These methods may be of interest to the 3D materials characterization community, especially considering the lack of standard commercial software tools. Thus, the current paper elaborates on the methods and analysis used to characterize fine titanium microstructures using 3D-EBSD and presents a detailed description of the new algorithms developed for probing the unique features therein. The new analyses include algorithms for identifying intervariant boundary types, classifying three-variant clusters, assigning grains to variants, and quantifying interconnectivity of branched α platelets.

Grain Growth Mechanism of Lamellar-Structure High-Purity Nickel via Cold Rolling and Cryorolling during Annealing.

High-purity (99.999%) nickel with lamellar-structure grains (LG) was obtained by room-temperature rolling and cryorolling in this research, and then annealed at different temperatures (75 °C, 160 °C, and 245 °C). The microstructure was characterized by transmission electron microscopy. The grain growth mechanism during annealing of the LG materials obtained via different processes was studied. Results showed that the LG high-purity nickel obtained by room-temperature rolling had a static discontinuous recrystallization during annealing, whereas that obtained by cryorolling underwent static and continuous recrystallization during annealing, which was caused by the seriously inhibited dislocation recovery in the rolling process under cryogenic conditions, leading to more accumulated deformation energy storage in sheets.

3D characterisation using plasma FIB-SEM: A large-area tomography technique for complex surfaces like black silicon.

This paper demonstrates an improved method to accurately extract the surface morphology of black silicon (BSi). The method is based on an automated Xe+ plasma focused ion beam (PFIB) and scanning electron microscope (SEM) tomography technique. A comprehensive new sample preparation method is described and shown to minimize the PFIB artifacts induced by both the top surface sample-PFIB interaction and the non-uniform material density. An optimized post-image processing procedure is also described that ensures the accuracy of the reconstructed 3D surface model. The application of these new methods is demonstrated by applying them to extract the surface topography of BSi formed by reactive ion etching (RIE) consisting of 2 µm tall needles. An area of 320 µm2 is investigated with a controlled slice thickness of 10 nm. The reconstructed 3D model allows the extraction of critical roughness characteristics, such as height distribution, correlation length, and surface enhancement ratio. Furthermore, it is demonstrated that the particular surface studied contains regions in which under-etching has resulted in overhanging structures, which would not have been identified with other surface topography techniques. Such overhanging structures can be present in a broad range of BSi surfaces, including BSi surfaces formed by RIE and metal catalyst chemical etching (MCCE). Without proper measurement, the un-detected overhangs would result in the underestimation of many critical surface characteristics, such as absolute surface area, electrochemical reactivity and light-trapping.

3D electron backscatter diffraction study of α lath morphology in additively manufactured Ti-6Al-4V.

Titanium alloys exhibit complex, multi-phase microstructures which form during liquid-solid and solid-solid phase transformations. These phase transformations govern the microstructural evolution and are potentially more complex during additive manufacturing due to large thermal gradients and inhomogeneities. The prototypical fundamental unit of titanium microstructures are the α laths, and investigations into their three-dimensional morphology may provide new insights. A prior ß-grain boundary, 3-variant clusters and interconnected laths were studied in 3D in electron-beam printed Ti-6Al-4V using a plasma FIB. These key features are of interest for studying variant selection in additive manufacturing.

Formation of micro-spherulitic barite in association with organic matter within sulfidized stromatolites of the 3.48 billion-year-old Dresser Formation, Pilbara Craton.

The shallow marine and subaerial sedimentary and hydrothermal rocks of the ~3.48 billion-year-old Dresser Formation are host to some of Earth's oldest stromatolites and microbial remains. This study reports on texturally distinctive, spherulitic barite micro-mineralization that occur in association with primary, autochthonous organic matter within exceptionally preserved, strongly sulfidized stromatolite samples obtained from drill cores. Spherulitic barite micro-mineralization within the sulfidized stromatolites generally forms submicron-scale aggregates that show gradations from hollow to densely crystallized, irregular to partially radiating crystalline interiors. Several barite micro-spherulites show thin outer shells. Within stromatolites, barite micro-spherulites are intimately associated with petrographically earliest dolomite and nano-porous pyrite enriched in organic matter, the latter of which is a possible biosignature assemblage that hosts microbial remains. Barite spherulites are also observed within layered barite in proximity to stromatolite layers, where they are overgrown by compositionally distinct (Sr-rich), coarsely crystalline barite that may have been sourced from hydrothermal veins at depth. Micro-spherulitic barite, such as reported here, is not known from hydrothermal systems that exceed the upper temperature limit for life. Rather, barite with near-identical morphology and micro-texture is known from zones of high bio-productivity under low-temperature conditions in the modern oceans, where microbial activity and/or organic matter of degrading biomass controls the formation of spherulitic aggregates. Hence, the presence of micro-spherulitic barite in the organic matter-bearing Dresser Formation sulfidized stromatolites lend further support for a biogenic origin of these unusual, exceptionally well-preserved, and very ancient microbialites.

Author Correction: Chemical nature of alkaline polyphosphate boundary film at heated rubbing surfaces.

A correction to this article has been published and is linked from the HTML and PDF versions of this paper. The error has been fixed in the paper.

Superstrength of nanograined steel with nanoscale intermetallic precipitates transformed from shock-compressed martensitic steel.

An increasing number of industrial applications need superstrength steels. It is known that refined grains and nanoscale precipitates can increase strength. The hardest martensitic steel reported to date is C0.8 steel, whose nanohardness can reach 11.9 GPa through incremental interstitial solid solution strengthening. Here we report a nanograined (NG) steel dispersed with nanoscale precipitates which has an extraordinarily high hardness of 19.1 GPa. The NG steel (shock-compressed Armox 500T steel) was obtained under these conditions: high strain rate of 1.2 µs-1, high temperature rise rate of 600 Kµs-1 and high pressure of 17 GPa. The mean grain size achieved was 39 nm and reinforcing precipitates were indexed in the NG steel. The strength of the NG steel is expected to be ~3950 MPa. The discovery of the NG steel offers a general pathway for designing new advanced steel materials with exceptional hardness and excellent strength.

Chemical nature of alkaline polyphosphate boundary film at heated rubbing surfaces.

Alkaline polyphosphate has been demonstrated to be able to reduce significant wear and friction of sliding interfaces under heavy loads (>1 GPa) and elevated temperature (800 °C and above) conditions, e.g. hot metal manufacturing. The chemical composition and fine structure of polyphosphate lubricating film is not well understood as well as the role of alkaline elements within the reaction film at hot rubbing surface. This work makes use of the coupling surface analytical techniques on the alkaline polyphosphate tribofilm, XANES, TOF-SIMS and FIB/TEM. The data show the composition in gradient distribution and trilaminar structure of tribofilm: a shorter chain phosphate overlying a long chain polyphosphate that adheres onto oxide steel base through a short chain phosphate. The chemical hardness model well explains the anti-abrasive mechanism of alkaline polyphosphate at elevated temperatures and also predicts a depolymerisation and simultaneous cross-linking of the polyphosphate glass. The role of alkaline elements in the lubrication mechanism is especially explained. This work firstly serves as a basis for a detailed study of alkaline polyphosphate tribofilm at temperature over 600 °C.

Subtle Interplay between Localized Magnetic Moments and Itinerant Electrons in LaAlO3/SrTiO3 Heterostructures.

Clarification of the role of magnetic ordering and scattering in two-dimensional electron gas has become increasingly important to understand the transport and magnetic behavior in the LaAlO3 (LAO)/SrTiO3 (STO) heterostructures. In this work, we report the sheet resistance of the LAO/STO heterostructures as functions of temperature, magnetic field, and field orientation. An unexpected resistance minimum was discovered at ∼10 K under a sufficiently high in-plane magnetic field. An anisotropic magnetoresistance (MR) is clearly identified, indicating the presence of magnetic scattering which may be related to the interaction between itinerant electrons and localized magnetic moments in the LaAlO3/SrTiO3 heterostructures. It is believed that the high concentration of oxygen vacancies induced by the ultralow oxygen partial pressure during the deposition process plays a predominant role in the occurrence of the anisotropic MR.

A combined experimental-numerical approach for determining mechanical properties of aluminum subjects to nanoindentation.

A crystal plasticity finite element method (CPFEM) model has been developed to investigate the mechanical properties and micro-texture evolution of single-crystal aluminum induced by a sharp Berkovich indenter. The load-displacement curves, pile-up patterns and lattice rotation angles from simulation are consistent with the experimental results. The pile-up phenomenon and lattice rotation have been discussed based on the theory of crystal plasticity. In addition, a polycrystal tensile CPFEM model has been established to explore the relationship between indentation hardness and yield stress. The elastic constraint factor C is slightly larger than conventional value 3 due to the strain hardening.

A new insight into ductile fracture of ultrafine-grained Al-Mg alloys.

It is well known that when coarse-grained metals undergo severe plastic deformation to be transformed into nano-grained metals, their ductility is reduced. However, there are no ductile fracture criteria developed based on grain refinement. In this paper, we propose a new relationship between ductile fracture and grain refinement during deformation, considering factors besides void nucleation and growth. Ultrafine-grained Al-Mg alloy sheets were fabricated using different rolling techniques at room and cryogenic temperatures. It is proposed for the first time that features of the microstructure near the fracture surface can be used to explain the ductile fracture post necking directly. We found that as grains are refined to a nano size which approaches the theoretical minimum achievable value, the material becomes brittle at the shear band zone. This may explain the tendency for ductile fracture in metals under plastic deformation.

Enhanced cellular preservation by clay minerals in 1 billion-year-old lakes.

Organic-walled microfossils provide the best insights into the composition and evolution of the biosphere through the first 80 percent of Earth history. The mechanism of microfossil preservation affects the quality of biological information retained and informs understanding of early Earth palaeo-environments. We here show that 1 billion-year-old microfossils from the non-marine Torridon Group are remarkably preserved by a combination of clay minerals and phosphate, with clay minerals providing the highest fidelity of preservation. Fe-rich clay mostly occurs in narrow zones in contact with cellular material and is interpreted as an early microbially-mediated phase enclosing and replacing the most labile biological material. K-rich clay occurs within and exterior to cell envelopes, forming where the supply of Fe had been exhausted. Clay minerals inter-finger with calcium phosphate that co-precipitated with the clays in the sub-oxic zone of the lake sediments. This type of preservation was favoured in sulfate-poor environments where Fe-silicate precipitation could outcompete Fe-sulfide formation. This work shows that clay minerals can provide an exceptionally high fidelity of microfossil preservation and extends the known geological range of this fossilization style by almost 500 Ma. It also suggests that the best-preserved microfossils of this time may be found in low-sulfate environments.

A deformation mechanism of hard metal surrounded by soft metal during roll forming.

It is interesting to imagine what would happen when a mixture of soft-boiled eggs and stones is deformed together. A foil made of pure Ti is stronger than that made of Cu. When a composite Cu/Ti foil deforms, the harder Ti will penetrate into the softer Cu in the convex shapes according to previously reported results. In this paper, we describe the fabrication of multilayer Cu/Ti foils by the roll bonding technique and report our observations. The experimental results lead us to propose a new deformation mechanism for a hard metal surrounded by a soft metal during rolling of a laminated foil, particularly when the thickness of hard metal foil (Ti, 25 µm) is much less than that of the soft metal foil (Cu, 300 µm). Transmission Electron Microscope (TEM) imaging results show that the hard metal penetrates into the soft metal in the form of concave protrusions. Finite element simulations of the rolling process of a Cu/Ti/Cu composite foil are described. Finally, we focus on an analysis of the deformation mechanism of Ti foils and its effects on grain refinement, and propose a grain refinement mechanism from the inside to the outside of the laminates during rolling.

Pt-Al2O3 interfaces in cofired ceramics for use in miniaturized neuroprosthetic implants.

A core element to miniaturized, hermetic encapsulations for neuroprosthetic implants with high numbers of stimulation channels is the creation of electrical feedthroughs. Platinum (Pt) and alumina (Al2 O3 ) are necessary to connect the sealed electronics to external components including electrode arrays that provide a neural interface function, as well as to sources of power or data. Combined with laser micro-processing, high-density feedthrough arrays were created with up to 2500 channels per cm(2) . The chemistry, micro structure, and crystallography of the Pt-Al2 O3 interface created by the cofiring of Pt particles and Al2 O3 particulate in binder were studied by transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS) and selective area electron diffraction (SAED) to determine the nature of the Pt-Al2 O3 bond. While Pt-Al2 O3 interfaces only occurred in cases where the different grains were in distinct orientations where the crystal lattices matched, the addition of glass additives allowed for bonding nonmatching orientations by devitrification to form Pt-glass-Al2 O3 interfaces. The conditions for the formation of both mechanisms were determined, and it was shown that higher order crystal planes than previously described can be matched. Analyzing the lattice matches in detail showed the ability of the material compound to compensate for mismatches by the formation of dislocations, out-of-angle matching, lattice distortion, and the existence of semi-coherent interfaces in case of integer misfit ratios to create domain matching.