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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.

Materials of a gradient structure have been shown to possess both high strength and high ductility. To date, materials of a gradient structure can only be produced in small quantities. In this paper, we report a novel 'cyclic skin-pass rolling' (CSPR) technique capable of producing sheets of gradient structure in large quantities. Both experimental and analytical/numerical investigations are reported. In the experiments on aluminium sheets, the outer layer was subjected to 40 passes of CSPR with a reduction ratio of 1% per pass. After CSPR, the sample surface shows an ultrafine-grained microstructure with a mean grain size of 206 nm, while the annealed microstructure is retained in the core of the sample. Compared with cold-rolled aluminium sheets fabricated with the same total reduction ratio, CSPR-processed aluminium sheets have the same yield stress but improved uniform elongation (2.4 times). The scanning electron microscopy was used to study the fracture surface, and The transmission electron microscopy to examine the microstructure near the fracture end, in order to analyse the improvement in ductility. In addition, the finite element method was used to simulate the roll-sample contact pressure and strain distribution as well as residual stress on the sheet surface during CSPR, and to better understand the mechanism leading to improvement of ductility of the sheets by the CSPR technique.

Compact oxide scale at a high speed steel (HSS) work roll surface during hot rolling process can act as an effective solid lubricant and a protective layer for better product surface quality. In this study, considering practical hot rolling process time, microstructure and surface roughness of three oxide scales on a HSS work roll have been systematically characterized with a help of scanning electron microscopy (SEM), atomic force microscopy (AFM), and transmission electron microscopy (TEM). It has been found that growth of the oxide scale follows a parabolic rate law and the dominant oxide phase is hematite. In addition, surface roughness increases dramatically when the oxidation time is less than 30 min and then changes slightly, when the HSS specimens were isothermally oxidized at 600 °C in a dry air. Residual stress evolutions with oxidation time have also been examined in details using X-ray diffraction (XRD) method. Measurement of microhardness at the HSS specimen surface revealed that development of defects and decrease of compressive residual stress in the oxide layer lead to a slight decrease in the microhardness.

In the present paper, a systematic study on the deformation behaviour of an oxidized high speed steel (HSS) during nanoindentation has been conducted. Specimens cut from a HSS work roll were oxidized first to develop the oxide layer with thickness close to that built up on a HSS work roll surface during hot rolling in industry. Then, nanoindentation tests with three typical peak loads from low to high (namely 2 mN, 20 mN, and 200 mN) were conducted on the oxide scale surface. Porosity in oxide scale and its surface morphology features were examined by transmission electron microscopy (TEM) and scanning electron microscopy (SEM), respectively. In addition, a finite element model was developed and verified by comparing with the experimental measured load-depth curves. With the developed model, for the first time, a systematic investigation has been done to understand the effects of nanoindentation depth (from 10 nm to 1250 nm), friction coefficient (from 0 to 0.6) and initial porosity of oxide scale (from 0 to 20%) during nanoindentation on the deformation behaviours of both oxide scale and HSS substrate. It has been found an obvious size effect and three regions can be divided according to nanoindentation depth, based on the evolution of mechanical property, porosity in oxide scale, and plastic deformations in both oxide scale and HSS substrate. This study also revealed that friction has a slight influence during nanoindentation and almost the same results were obtained when the friction coefficient is larger than 0.3. By contrast, a large influence of porosity in oxide scale was observed.

Thickness dependence of magnetic properties of LaAlO3 (LAO)/SrTiO3 (STO) heterostructures is systematically studied. It is found that the magnetic moment is rather robust at elevated temperatures in the samples grown under ultralow PO2 of 1 × 10−8 Torr, indicating room-temperature ferromagnetism in the LaAlO3/SrTiO3 heterostructures. Spin-glass-like behavior is observed in the LAO/STO heterostructures with the LAO thickness ranging from 5 to 90 unit cells (2–35.2 nm). As the LAO layer becomes thicker, the blocking temperature of spin-glass-like behavior decreases and magnetic moment weakens, which may be related to the reduced density of oxygen vacancies at the interfacial TiO2 layer. It is believed that the well-controlled magnetism by tuning the LAO thickness may open an avenue for the potential application of spintronics with LaAlO3/SrTiO3 heterostructures.

The mechanical properties of the Ti-6Al-4V alloy are significantly determined by the process used for manufacture. In this study, the mechanical properties of the Ti-6Al-4V alloy manufactured using cold rolling, asymmetric rolling and asymmetric cryorolling were characterized by subjecting it to the tensile test and the microhardness test. The evolution in the microstructure was studied using scanning electron microscopy, transmission electron microscopy as well as energy dispersive X-ray spectrometry. Results show that the Ti-6Al-4V alloy sheets subjected to asymmetrical cryorolling with low rolling speed ratio between the upper and lower rolls have the highest tensile strength and microhardness. The tensile stress of the alloy samples after cold rolling was found to be 1008 MPa, 1046 MPa after asymmetric rolling, and 1113 MPa after asymmetric cryorolling. The highest Vickers hardness (HV395) is achieved by asymmetric cryorolling. We discuss the mechanical behavior using the criteria of grain size, size of second phase as well as dislocation density.

Grain growth and grain refinement behavior during deformation determine the strength and ductility of ultrafine-grained materials. We used asymmetric cryorolling to fabricate ultrafine-grained copper sheets with an average grain width of 230 nm and having a laminate structure. The sheets show a high-true failure strain of 1.5. Observation of the microstructure at the fracture surface reveals that ultrafine laminate-structured grains were simultaneously transformed into both equiaxed nanograins and coarse grains under tensile deformation at room temperature.

The microstructure evolution and mechanical properties of ultrafine-grained (UFG) Al sheets subjected to accumulative roll bonding (ARB) and subsequent cryorolling was studied. Cryorolling can suppress the dynamic softening of UFG Al sheets subjected to ARB at room temperature. After the third ARB pass, the grains are slightly refined as the number of ARB passes increases. However, the grains are significantly refined further during cryorolling. The grain size of 460 nm achieved after the third ARB pass is reduced to 290 nm after two cryorolling passes with total reduction ratio 80%. Sheets subjected to ARB + cryorolling show improved mechanical properties compared to only ARB-processed sheets due to a change in the fraction of high-angle boundaries and elongated grains. The deformation mechanism for ultrafine grains at room temperature is determined by grain boundary sliding or dislocation-based recovery, while it is governed by dislocation glide at cryogenic temperature.

Grain growth and grain refinement behavior during deformation determine the strength and ductility of ultrafine-grained materials. We used asymmetric cryorolling to fabricate ultrafine-grained copper sheets with an average grain width of 230 nm and having a laminate structure. The sheets show a high-true failure strain of 1.5. Observation of the microstructure at the fracture surface reveals that ultrafine laminate-structured grains were simultaneously transformed into both equiaxed nanograins and coarse grains under tensile deformation at room temperature.

The microstructure evolution and mechanical properties of ultrafine-grained (UFG) Al sheets subjected to accumulative roll bonding (ARB) and subsequent cryorolling was studied. Cryorolling can suppress the dynamic softening of UFG Al sheets subjected to ARB at room temperature. After the third ARB pass, the grains are slightly refined as the number of ARB passes increases. However, the grains are significantly refined further during cryorolling. The grain size of 460 nm achieved after the third ARB pass is reduced to 290 nm after two cryorolling passes with total reduction ratio 80%. Sheets subjected to ARB + cryorolling show improved mechanical properties compared to only ARB-processed sheets due to a change in the fraction of high-angle boundaries and elongated grains. The deformation mechanism for ultrafine grains at room temperature is determined by grain boundary sliding or dislocation-based recovery, while it is governed by dislocation glide at cryogenic temperature.

Grain growth and grain refinement behavior during deformation determine the strength and ductility of ultrafine-grained materials. We used asymmetric cryorolling to fabricate ultrafine-grained copper sheets with an average grain width of 230 nm and having a laminate structure. The sheets show a high-true failure strain of 1.5. Observation of the microstructure at the fracture surface reveals that ultrafine laminate-structured grains were simultaneously transformed into both equiaxed nanograins and coarse grains under tensile deformation at room temperature.

The microstructure evolution and mechanical properties of ultrafine-grained (UFG) Al sheets subjected to accumulative roll bonding (ARB) and subsequent cryorolling was studied. Cryorolling can suppress the dynamic softening of UFG Al sheets subjected to ARB at room temperature. After the third ARB pass, the grains are slightly refined as the number of ARB passes increases. However, the grains are significantly refined further during cryorolling. The grain size of 460 nm achieved after the third ARB pass is reduced to 290 nm after two cryorolling passes with total reduction ratio 80%. Sheets subjected to ARB + cryorolling show improved mechanical properties compared to only ARB-processed sheets due to a change in the fraction of high-angle boundaries and elongated grains. The deformation mechanism for ultrafine grains at room temperature is determined by grain boundary sliding or dislocation-based recovery, while it is governed by dislocation glide at cryogenic temperature.

Grain growth and grain refinement behavior during deformation determine the strength and ductility of ultrafine-grained materials. We used asymmetric cryorolling to fabricate ultrafine-grained copper sheets with an average grain width of 230 nm and having a laminate structure. The sheets show a high-true failure strain of 1.5. Observation of the microstructure at the fracture surface reveals that ultrafine laminate-structured grains were simultaneously transformed into both equiaxed nanograins and coarse grains under tensile deformation at room temperature.

The microstructure evolution and mechanical properties of ultrafine-grained (UFG) Al sheets subjected to accumulative roll bonding (ARB) and subsequent cryorolling was studied. Cryorolling can suppress the dynamic softening of UFG Al sheets subjected to ARB at room temperature. After the third ARB pass, the grains are slightly refined as the number of ARB passes increases. However, the grains are significantly refined further during cryorolling. The grain size of 460 nm achieved after the third ARB pass is reduced to 290 nm after two cryorolling passes with total reduction ratio 80%. Sheets subjected to ARB + cryorolling show improved mechanical properties compared to only ARB-processed sheets due to a change in the fraction of high-angle boundaries and elongated grains. The deformation mechanism for ultrafine grains at room temperature is determined by grain boundary sliding or dislocation-based recovery, while it is governed by dislocation glide at cryogenic temperature.

The discovery of magnetism at the LaAlO3/SrTiO3 heterostructures has attracted a lot of interests in regards to the origin of magnetic properties appearing in this nonmagnetic system. In this paper, the existence of a robust ferromagnetic state in the LaAlO3/SrTiO3 heterostructures is demonstrated. The oxygen vacancy dependence of magnetic phenomena demonstrates the correlation between the magnetic properties and the oxygen vacancies. The strong ferromagnetism can be also manipulated by controlling the partial pressure of oxygen during the film deposition process. The well-controlled magnetism may open an avenue for the applications of magnetic storage and spintronics with the 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.

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.

2014 Elsevier B.V. Monolayer TiCN and multilayer TiCN/Ti coatings were deposited on the surface of Ti using the Filtered Arc Deposition System (FADS). Nanoindentation tests were performed on both coatings. The multilayer TiCN/Ti coating exhibited better ductility than the monolayer TiCN coating. The lattice constants of the coatings were characterized by X-ray diffraction. Transmission Electron Microscopy (TEM) was used to investigate the fracture behavior of the coatings. Inter-columnar, inclined and lateral cracks were found to be the dominant crack modes in the monolayer TiCN coatings while small bending crack and radial crack were the dominant crack modes in the multilayer TiCN/Ti coatings. The Finite Element Method (FEM) was used to simulate the indentation process. It was found that the Ti interlayer in the multilayer TiCN/Ti coating could efficiently suppress the fracture, which is responsible for the improved ductility of the multilayer TiCN/Ti coating.

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.

2014 Elsevier B.V. Monolayer TiCN and multilayer TiCN/Ti coatings were deposited on the surface of Ti using the Filtered Arc Deposition System (FADS). Nanoindentation tests were performed on both coatings. The multilayer TiCN/Ti coating exhibited better ductility than the monolayer TiCN coating. The lattice constants of the coatings were characterized by X-ray diffraction. Transmission Electron Microscopy (TEM) was used to investigate the fracture behavior of the coatings. Inter-columnar, inclined and lateral cracks were found to be the dominant crack modes in the monolayer TiCN coatings while small bending crack and radial crack were the dominant crack modes in the multilayer TiCN/Ti coatings. The Finite Element Method (FEM) was used to simulate the indentation process. It was found that the Ti interlayer in the multilayer TiCN/Ti coating could efficiently suppress the fracture, which is responsible for the improved ductility of the multilayer TiCN/Ti coating.

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.

2014 Elsevier B.V. Monolayer TiCN and multilayer TiCN/Ti coatings were deposited on the surface of Ti using the Filtered Arc Deposition System (FADS). Nanoindentation tests were performed on both coatings. The multilayer TiCN/Ti coating exhibited better ductility than the monolayer TiCN coating. The lattice constants of the coatings were characterized by X-ray diffraction. Transmission Electron Microscopy (TEM) was used to investigate the fracture behavior of the coatings. Inter-columnar, inclined and lateral cracks were found to be the dominant crack modes in the monolayer TiCN coatings while small bending crack and radial crack were the dominant crack modes in the multilayer TiCN/Ti coatings. The Finite Element Method (FEM) was used to simulate the indentation process. It was found that the Ti interlayer in the multilayer TiCN/Ti coating could efficiently suppress the fracture, which is responsible for the improved ductility of the multilayer TiCN/Ti coating.

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.

2014 Elsevier B.V. Monolayer TiCN and multilayer TiCN/Ti coatings were deposited on the surface of Ti using the Filtered Arc Deposition System (FADS). Nanoindentation tests were performed on both coatings. The multilayer TiCN/Ti coating exhibited better ductility than the monolayer TiCN coating. The lattice constants of the coatings were characterized by X-ray diffraction. Transmission Electron Microscopy (TEM) was used to investigate the fracture behavior of the coatings. Inter-columnar, inclined and lateral cracks were found to be the dominant crack modes in the monolayer TiCN coatings while small bending crack and radial crack were the dominant crack modes in the multilayer TiCN/Ti coatings. The Finite Element Method (FEM) was used to simulate the indentation process. It was found that the Ti interlayer in the multilayer TiCN/Ti coating could efficiently suppress the fracture, which is responsible for the improved ductility of the multilayer TiCN/Ti coating.

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.

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.

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.

In this study polyphosphate lubricant was introduced into steel rolling process. The friction coefficient reduced from 0.463 to 0.238 by the presence of polyphosphate lubricant as compared with unlubricated condition, calculated from 2-high Hille 100 rolling mill tests. A tribofilm of similar to 100 nm can be observed on the strip surface, greatly improving the surface finish. This tribofilm well adhered on the oxide layer/steel base by the interfacial reactions. Laser-scanning confocal microscope well confirmed the reactions of polyphosphate lubricant with the oxide scales occurring. Furthermore, a feasible mechanism the composition and structure of this lubricant during thermal reaction was proposed when exposed to different temperatures. (C) 2015 Elsevier B.V. All rights reserved.

Polyphosphate inorganic polymer is evaluated as a high-performance lubricant for steel/steel contacts at 600, 700, and 800 degrees C. In situ thermal tests of this lubricant indicate that liquid lubrication at the rubbing interface is occurring. Tribological testing indicates the molten polyphosphate is effective as a lubricant and, reduces friction and wear of the sliding steel/steel tribo pair substantially. The lubricated steel/steel pair shows desirable tribological performance that correlates closely with the temperature-dependent hierarchical structure of the tribo-interface under the combination of pressure, shear, and temperature. Morphological observation of worn surfaces and interfaces of steel discs is achieved using scanning electron microscopy and transmission electron microscopy (TEM). Compositional analysis and elemental distribution are performed using X-ray photoelectron spectroscopy and energy dispersive X-ray on a scanning TEM. These enable the tribochemical reactions at the rubbing surface and the formation mechanism of the hierarchical tribo-interface to be understood.

We report an abnormally high residual dislocation density in aluminium in an Al/Ti/Al laminate annealed at 873 K for seven days. The residual dislocation density reaches 7.5 x 1014 m−2, higher than that in aluminum after severe plastic deformation processes such as accumulative roll bonding and high-pressure torsion. It is proposed that the high residual dislocation density may result from obstruction of the movement of TiAl3 nanoparticles by the grain boundary and Ti atoms conglomerating at vacancies distributed in the aluminium matrix at a high temperature for a sufficient time to allow a relatively stable crystal.

In this paper, an extended accumulative roll bonding (ARB) technique, called the 'Four-Layer Accumulative Roll Bonding (FL-ARB)' technique, is presented for the first time. This technique has been employed to produce ultrafine-grained commercial pure aluminum sheets with success. After three FL-ARB passes, the grain size of pure aluminum was seen to reduce to 380 nm. The bonding strength of the sheets after rolling has also been discussed. Theoretical calculations showed that the bonding strength of sheets processed by the FL-ARB technique can be 2-2.2 times greater than that by the traditional ARB technique. The main advantages of the FL-ARB technique are (a) improvement of the interface bonding, with increasing deformation in each pass, (b) applicability of the technique at room temperature to process most metals, and (c) generation of the largest equivalent strain in the workpiece with the same number of passes, compared with other severe plastic deformation techniques.

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 mm) is much less than that of the soft metal foil (Cu, 300 mm). 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.

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.

An asymmetric cryorolling technique was used to reduce the thickness of an Al-Mg-Si alloy sheet from 1.5 mm to 0.19 mm. The samples were subsequently aged for 48 h at 100 degrees celcius. The hardness and tensile strength of both rolled and aged sheets increased with the number of passes up to the sixth pass, but the tensile stress decreased after the seventh pass. Investigation of the microstructure of the sheets showed that the grain size after seven passes was about 235 nm and revealed the presence of Fe-Cr-Mn-Si particles in the samples. The deformation of Fe-Cr-Mn-Si particles and sheet thickness affects the ductility when the sheet thickness is less than 0.4 mm, and the strength when the thickness is less than 0.2 mm.

In this paper, a high temperature pin-on-disc configuration was used to simulate the contact established between a high-speed steel (HSS) work roll and a hot strip material in hot rolling, in which the pin represented the HSS roll and the disc represented a strip steel. The pin surfaces were oxidised due to the heat transfer from the disc while they were in contact. This work focused on the contact behaviour of the oxide scale in the roll bite during hot rolling while the testing temperature was close to the rolling temperature, the Hertzian pressure was similar to the contact pressure and the sliding speed was close to those in the roll bite. The coefficient of friction during the tests was monitored and recorded in-situ. It was found that the evolution of the coefficient of friction could be divided into three stages. Associated with the evolution of the coefficient of friction, the morphologies and micro-structures on the surface of pin were characterised by means of SEM, FIB and TEM techniques to study the tribological behaviour of oxide scale in contacts. The results indicated that the wear mechanism of pin surface varies in different stages. At the stages I and II, the oxide scale on the pin surface is significantly deformed. At the stage III, which the coefficient of friction is stable, the wear mechanism is a mixture of adhesion, abrasion and oxidation. The oxide transfer from the mild carbon steel disc to HSS pin significantly contributed to the scale formed on the HSS pin surface.

This paper reports a new technique that combines the features of Accumulative Roll Bonding (ARB) and Asymmetric Rolling (AR). This technique has been developed to enable production of ultra-thin bimetallic foils. Initially, 1.5 mm thick AA1050 and AA6061 foils were roll-bonded using ARB at 2006C, with 50% reduction. The resulting 1.5 mm bimetallic foil was subsequently thinned to 0.04 mm through four AR passes at room temperature. The speed ratio between the upper and lower AR rolls was 151.3. The tensile strength of the bimetallic foil was seen to increase with reduction in thickness. The ductility of the foil was seen to reduce upon decreasing the foil thickness from 1.5 mm to 0.14 mm, but increase upon further reduction in thickness from 0.14 mm to 0.04 mm. The grain size was about 140 nm for the AA6061 layer and 235 nm for the AA1050 layer, after the third AR pass.

An asymmetric cryorolling technique was used to reduce the thickness of an Al-Mg-Si alloy sheet from 1.5 mm to 0.19 mm. The samples were subsequently aged for 48 h at 100 degrees celcius. The hardness and tensile strength of both rolled and aged sheets increased with the number of passes up to the sixth pass, but the tensile stress decreased after the seventh pass. Investigation of the microstructure of the sheets showed that the grain size after seven passes was about 235 nm and revealed the presence of Fe-Cr-Mn-Si particles in the samples. The deformation of Fe-Cr-Mn-Si particles and sheet thickness affects the ductility when the sheet thickness is less than 0.4 mm, and the strength when the thickness is less than 0.2 mm.

This paper reports a new technique that combines the features of Accumulative Roll Bonding (ARB) and Asymmetric Rolling (AR). This technique has been developed to enable production of ultra-thin bimetallic foils. Initially, 1.5 mm thick AA1050 and AA6061 foils were roll-bonded using ARB at 2006C, with 50% reduction. The resulting 1.5 mm bimetallic foil was subsequently thinned to 0.04 mm through four AR passes at room temperature. The speed ratio between the upper and lower AR rolls was 151.3. The tensile strength of the bimetallic foil was seen to increase with reduction in thickness. The ductility of the foil was seen to reduce upon decreasing the foil thickness from 1.5 mm to 0.14 mm, but increase upon further reduction in thickness from 0.14 mm to 0.04 mm. The grain size was about 140 nm for the AA6061 layer and 235 nm for the AA1050 layer, after the third AR pass.

In this paper, a high temperature pin-on-disc configuration was used to simulate the contact established between a high-speed steel (HSS) work roll and a hot strip material in hot rolling, in which the pin represented the HSS roll and the disc represented a strip steel. The pin surfaces were oxidised due to the heat transfer from the disc while they were in contact. This work focused on the contact behaviour of the oxide scale in the roll bite during hot rolling while the testing temperature was close to the rolling temperature, the Hertzian pressure was similar to the contact pressure and the sliding speed was close to those in the roll bite. The coefficient of friction during the tests was monitored and recorded in-situ. It was found that the evolution of the coefficient of friction could be divided into three stages. Associated with the evolution of the coefficient of friction, the morphologies and micro-structures on the surface of pin were characterised by means of SEM, FIB and TEM techniques to study the tribological behaviour of oxide scale in contacts. The results indicated that the wear mechanism of pin surface varies in different stages. At the stages I and II, the oxide scale on the pin surface is significantly deformed. At the stage III, which the coefficient of friction is stable, the wear mechanism is a mixture of adhesion, abrasion and oxidation. The oxide transfer from the mild carbon steel disc to HSS pin significantly contributed to the scale formed on the HSS pin surface.

Nanostructural Al 1050 sheets were produced using a novel method of asymmetric cryorolling under ratios of upper and down rolling velocities (RUDV) of 1.1, 1.2, 1.3, and 1.4. Sheets were rolled to about 0.17 mm from 1.5 mm. Both the strength and ductility of Al 1050 sheets increase with RUDVs. Tensile strength of Al sheets with the RUDV 1.4 is larger 22.3% of that for RUDV 1.1, which is 196 MPa. The TEM observations show the grain size is 360 nm when the RUDV is 1.1, and 211 nm for RUDV 1.4.

Nanostructural Al 1050 sheets were produced using a novel method of asymmetric cryorolling under ratios of upper and down rolling velocities (RUDV) of 1.1, 1.2, 1.3, and 1.4. Sheets were rolled to about 0.17 mm from 1.5 mm. Both the strength and ductility of Al 1050 sheets increase with RUDVs. Tensile strength of Al sheets with the RUDV 1.4 is larger 22.3% of that for RUDV 1.1, which is 196 MPa. The TEM observations show the grain size is 360 nm when the RUDV is 1.1, and 211 nm for RUDV 1.4.

Nanostructural Al 1050 sheets were produced using a novel method of asymmetric cryorolling under ratios of upper and down rolling velocities (RUDV) of 1.1, 1.2, 1.3, and 1.4. Sheets were rolled to about 0.17 mm from 1.5 mm. Both the strength and ductility of Al 1050 sheets increase with RUDVs. Tensile strength of Al sheets with the RUDV 1.4 is larger 22.3% of that for RUDV 1.1, which is 196 MPa. The TEM observations show the grain size is 360 nm when the RUDV is 1.1, and 211 nm for RUDV 1.4.

TiN monolayer and TiN/Ti multilayer thin films were deposited on commercially pure Ti substrates using a filtered arc deposition system (FADS). Surface topography and chemical composition have been characterized by atomic force microscopy (AFM) and X-ray diffraction (XRD), respectively. Fracture properties of coatings induced by nanoindentation have been investigated. Focused ion beam (FIB) and transmission electron microscopy (TEM) were used to identify the fracture modes. It was found that the TiN/Ti multilayer coating exhibited a higher pop-in force, which indicated good film ductility. Transmission electron microscope (TEM) observation showed that the small bending crack was the dominant crack in the TiN/Ti multilayer coating. The Ti layer shows that it could efficiently suppress the crack propagation, which was responsible for the improved ductility of the TiN/Ti multilayer coating.

Nanostructural Al 1050 sheets were produced using a novel method of asymmetric cryorolling under ratios of upper and down rolling velocities (RUDV) of 1.1, 1.2, 1.3, and 1.4. Sheets were rolled to about 0.17 mm from 1.5 mm. Both the strength and ductility of Al 1050 sheets increase with RUDVs. Tensile strength of Al sheets with the RUDV 1.4 is larger 22.3% of that for RUDV 1.1, which is 196 MPa. The TEM observations show the grain size is 360 nm when the RUDV is 1.1, and 211 nm for RUDV 1.4.

Jia, Z., Nomoto, K., Wang, Q., Kong, C., Sun, L., Zhang, L. C., . . . Kruzic, J. J. (2021). A self-supported high-entropy metallic glass with a nanosponge architecture for efficient hydrogen evolution under alkaline and acidic conditions. Advanced Functional Materials, 31(38), article 2101586. https://doi.org/10.1002/adfm.202101586