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Title: Micromechanical characterization of shales through nanoindentation and energy dispersive x-ray spectrometry

Shales are heterogeneous sedimentary rocks which typically comprise a variable mineralogy (including compacted clay particles sub-micrometer in size), silt grains, and nanometer sized pores collectively arranged with transversely isotropic symmetry. Moreover, a detailed understanding of the micro- and sub-microscale geomechanics of these minerals is required to improve models of shale strength and stiffness properties. In this paper, we propose a linked experimental–computational approach and validate a combination of grid nanoindentation and Scanning Electron Microscopy (SEM) with Energy and Wavelength Dispersive X-ray Spectrometry (EDS/WDS) at the same spatial locations to identify both the nano-mechanical morphology and local mineralogy of these nanocomposites. The experimental parameters of each method are chosen to assess a similar volume of material. By considering three different shales of varying mineralogy and mechanical diversity, we show through the EMMIX statistical iterative technique that the constituent phases, including highly compacted plate- or sheet-like clay particles, carbonates, silicates, and sulfides, have distinct nano-mechanical morphologies and associated indentation moduli and hardness. Nanoindentation-based strength homogenization analysis determines an average clay packing density, friction coefficient, and solid cohesion for each tested shale sample. Comparison of bulk to microscale geomechanical properties, through bulk porosimetry measurements, reveals a close correspondence between bulk and microscale claymore » packing densities. Determining the mechanical microstructure and material properties is useful for predictive microporomechanical models of the stiffness and strength properties of shale. Furthermore, the experimental and computational approaches presented here also apply to other chemically and mechanically complex materials exhibiting nanogranular, composite behavior.« less
 [1] ; ORCiD logo [2] ; ORCiD logo [3] ;  [4] ;  [5] ;  [5] ;  [6]
  1. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Structural Dynamics
  2. LGM Consultants Engineering Services, Tarrytown, NY (United States)
  3. North Carolina State Univ., Raleigh, NC (United States). Dept. of Civil, Construction, and Environmental Engineering
  4. CSIRO Energy, Clayton, VIC (Australia). Ian Wark Lab.
  5. Australian Resources Research Centre, Kensington, WA (Australia)
  6. Univ. of Melbourne (Australia). Dept. of Chemical and Biomolecular Engineering
Publication Date:
Report Number(s):
Journal ID: ISSN 2352-3808; PII: S2352380816300843
Grant/Contract Number:
Accepted Manuscript
Journal Name:
Geomechanics for Energy and the Environment
Additional Journal Information:
Journal Volume: 9; Journal Issue: C; Journal ID: ISSN 2352-3808
Research Org:
Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
Sponsoring Org:
USDOE National Nuclear Security Administration (NNSA)
Country of Publication:
United States
36 MATERIALS SCIENCE; 58 GEOSCIENCES; Micromechanical characterization; Shale; Nanoindentation; Energy and wavelength dispersive x-ray spectrometry; Scanning electron microscopy; Strength homogenization; Cathodoluminescence
OSTI Identifier: