The nanogranular origin of friction and cohesion in shale—A strength homogenization approach to interpretation of nanoindentation results

An inverse micromechanics approach allows interpretation of nanoindentation results to deliver cohesive‐frictional strength behavior of the porous clay binder phase in shale. A recently developed strength homogenization model, using the Linear Comparison Composite approach, considers porous clay as a granular material with a cohesive‐frictional solid phase. This strength homogenization model is employed in a Limit Analysis Solver to study indentation hardness responses and develop scaling relationships for indentation hardness with clay packing density. Using an inverse approach for nanoindentation on a variety of shale materials gives estimates of packing density distributions within each shale and demonstrates that there exists shale‐independent scaling relations of the cohesion and of the friction coefficient that vary with clay packing density. It is observed that the friction coefficient, which may be interpreted as a degree of pressure‐sensitivity in strength, tends to zero as clay packing density increases to one. In contrast, cohesion reaches its highest value as clay packing density increases to one. The physical origins of these phenomena are discussed, and related to fractal packing of these nanogranular materials. Copyright © 2010 John Wiley & Sons, Ltd.     

Computational mechanics of the steel–concrete interface

Concrete cracking in reinforced concrete structures is governed by two mechanisms: the activation of bond forces at the steel–concrete interface and the bridge effects of the reinforcement crossing a macro‐crack. The computational modelling of these two mechanisms, acting at different scales, is the main objective of this paper. The starting point is the analysis of the micro‐mechanisms, leading to an appropriate choice of (measurable) state variables describing the energy state in the surface systems: on the one side the relative displacement between the steel and the concrete, modelling the bond activation; on the other hand, the crack opening governing the bridge effects. These displacement jumps are implemented in the constitutive model using thermodynamics of surfaces of discontinuity. On the computational side, the constitutive model is implemented in a discrete crack approach. A truss element with slip degrees of freedom is developed. This degree of freedom represents the relative displacement due to bond activation. In turn, the bridge effect is numerically taken into account by modifying the post‐cracking behaviour of the contact elements representing discrete concrete cracks crossed by a rebar. First simulation results obtained with this model show a good agreement in crack pattern and steel stress distribution with micro‐mechanical results and experimental results. Copyright © 2001 John Wiley & Sons, Ltd.     

The nanogranular nature of shale

Despite their ubiquitous presence as sealing formations in hydrocarbon bearing reservoirs affecting many fields of exploitation, the source of anisotropy of this earth material is still an enigma that has deceived many decoding attempts from experimental and theoretical sides. Sedimentary rocks, such as shales, are made of highly compacted clay particles of sub-micrometer size, nanometric porosity and different mineralogy. In this paper, we present, for the first time, results from a new experimental technique that allows one to rationally assess the elasticity content of the highly heterogeneous clay fabric of shales from nano- and microindentation. Based on the statistical analysis of massive nanoindentation tests, we find (1) that the in-situ elasticity content of the clayfabric at a scale of a few hundred to thousands nanometers is almost an order of magnitude smaller than reported clay stiffness values of clay minerals, and (2) that the elasticity and the anisotropy scale linearly with the clay packing density beyond a percolation threshold of roughly 50%. Furthermore, we show that the elasticity content sensed by nano- and microindentation tests is equal to the one that is sensed by (small strain) velocity measurements. From those observations, we conclude that shales are nanogranular composite materials, whose mechanical properties are governed by particle-to-particle contact and by characteristic packing densities, and that the much stiffer mineral properties play a secondary role.     

Nanochemo-mechanical signature of organic-rich shales: a coupled indentation–EDX analysis

The organic–inorganic nature of organic-rich source rocks poses several challenges for the development of functional relations that link mechanical properties with geochemical composition. With this focus in mind, we herein propose a method that enables chemo-mechanical characterization of this highly heterogeneous source rock at the micron and submicron length scale through a statistical analysis of a large array of energy-dispersive X-ray spectroscopy (EDX) data coupled with nanoindentation data. The ability to include elemental composition to the indentation probe via EDX is shown to provide a means to identify pure material phases, mixture phases, and interfaces between different phases. Employed over a large array, the statistical clustering of this set of chemo-mechanical data provides access to the properties of the fundamental building blocks of clay-dominated organic-rich source rocks. The versatility of the approach is illustrated through the application to a large number of source rocks of different origin, chemical composition, and organic content. We find that the identified properties exhibit a unique scaling relation between stiffness and hardness. This suggests that organic-rich shale properties can be reduced to their elementary constituents, with several implications for the development of predictive functional relations between chemical composition and mechanical properties of organic-rich source rocks such as the intimate interplay between clay-packing, organic maturity, and mechanical properties of porous clay/organic phase.     

Dating of soil layers in a young floodplain using iron oxide crystallinity

Dating of fluvial deposits is essential for a more quantitative understanding of landscape evolution and soil development in floodplain environments. We collected soil layers in defined depth intervals down to 60 cm along a substrate age gradient in a floodplain of the Danube River near Vienna, Austria. Depth profiles of fallout ¹³⁷Cs were used to assess short-term sedimentation, and optically stimulated luminescence (OSL) dating was used to attribute sediment deposits to time periods between the early last millennium BC and the 18th century AD. In the studied soils, the ratio of oxalate- to dithionite-extractable iron (Fe_o/Fe_d), which indicates the degree of iron oxide crystallinity, progressively decreased from ratios greater than 0.5 to values less than 0.2 with increasing soil age and proved to be a reliable indicator of soil maturity. We linked the observed Fe_o/Fe_d ratios to the radiometric and OSL ages in a chronofunction, which allows to approximately date soil layers that lack an independent age control. The soil ages calculated with this chronofunction accurately reflected their geomorphological position, resulted in consistent age trends with depth, and highlighted the active morphodynamics of the studied floodplain. The chronofunction was further validated by dating a soil profile near the studied chronosequence that contained an archaeological find dated to the La Tène period (5th to 1st century BC).     

Rate-independent fracture toughness of gray and black kerogen-rich shales

The objective of this investigation is to characterize the influence of the loading rate, scratch speed, mineralogy, morphology, anisotropy, and total organic content on the scratch toughness of organic-rich shale. We focus our study on a gray shale, Toarcian shale (Paris basin, France) and a black shale, Niobrara shale (northeastern Colorado, USA). Microscopic scratch tests are performed for varying scratch speeds and loading rates. We consider several orientations for scratch testing. For all gas shale specimens, the scratch toughness is found to increase with increasing scratch speed. In the asymptotic regime of high speeds, there is a convergence toward a single constant value irrespective of the loading rate. To understand this evolution of the scratch toughness, a nonlinear fracture mechanics model is built that integrates fracture dissipation with the various forms of viscous processes. In particular, a coupling is shown between the fracture energy and the viscoelastic characteristics. An inverse approach which combines scratch and indentation testing makes it possible to represent all tests in a single curve and retrieve the rate-independent fracture toughness of kerogen-rich shale materials. The presence of organic matter drastically alters the creep and fracture properties at the microscopic length-scale. The fracture behavior is anisotropic with the divider orientation yielding the highest fracture toughness value and the short transverse orientation yielding the lowest fracture toughness. Elucidating the fracture-composition-morphology relationships in organic-rich shale will promote advances in science and engineering for energy-related applications such as hydraulic fracturing in unconventional reservoirs or \(\hbox {CO}_2\) sequestration in depleted reservoirs.     

Marine and estuarine reservoir effects in central Queensland,Australia: Determination of ΔR values

As a component of archaeological investigations on the central Queensland coast, a series of five marine shell specimens live‐collected between A.D. 1904 and A.D. 1929 and 11 shell/charcoal paired samples from archaeological contexts were radiocarbon dated to determine local ΔR values. The object of the study was to assess the potential influence of localized variation in marine reservoir effect in accurately determining the age of marine and estuarine shell from archaeological deposits in the area. Results indicate that the routinely applied ΔR value of −5 ± 35 for northeast Australia is erroneously calculated. The determined values suggest a minor revision to Reimer and Reimer's (2000) recommended value for northeast Australia from ΔR = +11 ± 5 to +12 ± 7, and specifically for central Queensland to ΔR = +10 ± 7, for near‐shore open marine environments. In contrast, data obtained from estuarine shell/charcoal pairs demonstrate a general lack of consistency, suggesting estuary‐specific patterns of variation in terrestrial carbon input and exchange with the open ocean. Preliminary data indicate that in some estuaries, at some time periods, a ΔR value of more than −155 ± 55 may be appropriate. In estuarine contexts in central Queensland, a localized estuary‐specific correction factor is recommended to account for geographical and temporal variation in ¹⁴C activity. © 2002 Wiley Periodicals, Inc.