Nanomechanics and pore structure evolution in organic-rich shale reservoirs during high-temperature treatment: A multi-scale analysis of microscopic stability
Abstract
To address the challenges of conflicting macroscopic mechanical tests and the inability to reveal complex nanoscale mechanisms during deep shale thermal modification, this study comprehensively investigates the microstructural and nanomechanical evolution of Longmaxi shale under heat treatment. This involves the innovative combination of gas adsorption, atomic force microscope high-resolution mapping, and multi-level spatial statistical analysis to systematically elucidate the spatial evolution of the pore structure of shale, surface morphology, and nanomechanical properties. The findings reveal a unique hardening-softening-rehardening three-stage pattern: From 25-400 °C, the average reduced modulus increases due to dehydration; from 400-600°C, organic matter pyrolysis significantly decreases the modulus, with intense atomic force microscope topographic uplift; from 600-900 °C, the modulus slightly increases again due to structural collapse and pore network regeneration. Local indicators of spatial association analysis shows that this macro evolution stems from synergistic microscopic phase space reshaping. Crucially, the mesopore volume increases most significantly in the 400-500°C range, and it exhibits its most notable increase. Considering energy efficiency and feasibility, this study demonstrates for the first time that 400-500 °C is an ideal temperature window for effective organic matter pyrolysis and nanopore optimization from a nanoscale spatial distribution and geometric stability perspective. This work provides crucial micromechanical mechanism support and precise temperature guidance for deep shale thermal modification, significantly outperforming the temperature ranges from traditional macroscopic experiments and filling the gap in macro-nanoscale mechanical discrepancies and spatial feature analysis.
Document Type: Original article
Cited as: Chen, Q., Tang, X., Shi, Y., Zhang, R., Shang, F. Nanomechanics and pore structure evolution in organic-rich shale reservoirs during high-temperature treatment: A multi-scale analysis of microscopic stability. Advances in Geo-Energy Research, 2025, 17(3): 241-255. https://doi.org/10.46690/ager.2025.09.06
Keywords:
Shale reservoir, thermal treatment, atomic force microscopy, geometric stability, spatial statisticsReferences
Allan, A. M., Clark, A. C., Vanorio, T., et al. On the evolution of the elastic properties of organic-rich shale upon pyrolysis-induced thermal maturation. Geophysics, 2016, 81(3): 263-281.
Anselin, L. Local indicators of spatial association-LISA. Geographical Analysis, 1995, 27(2): 93-115.
Bai, F., Sun, Y., Liu, Y., et al. Evaluation of the porous structure of Huadian oil shale during pyrolysis using multiple approaches. Fuel, 2017, 187(1): 1-8.
Brunauer, S., Emmett, P. H., Teller, E. Adsorption of gases in multimolecular layers. Journal of the American Chemical Society, 1938, 60(2): 309-319.
Cai, J., Wood, D., Hajibeygi, H., et al. Multiscale and multiphysics influences on fluids in unconventional reservoirs: Modeling and simulation. Advances in Geo-Energy Research, 2022a, 6(2): 91-94.
Cai, J., Zhao, L., Zhang, F., et al. Advances in multiscale rock physics for unconventional reservoirs. Advances in Geo-Energy Research, 2022b, 6(4): 271-275.
Cai, Z., Zhao, L., Ma, J., et al. Evolution of the elastic properties of lacustrine organic shales under different thermal maturity conditions. Science China Earth Sciences, 2025, 68: 781-802.
Chen, X., Tang, X., Liu, C., et al. Implications of temperature for the modification of high-overmature shale reservoirs: Experimental and numerical analysis. SPE Journal, 2024, 29(8): 4218-4231.
Chen, X., Tang, X., Zhang, R., et al. Changes in shale microstructure and fluid flow under high temperature: Experimental analysis and fluid-structure interaction simulation. Petroleum Science, 2025, 22(4): 1699-1711.
Cheng, B., Li, S., Xu, J., et al. Gaseous hydrocarbons cracking in shale: Mechanism, impact and resource significance. Earth-Science Reviews, 2025, 270: 105211.
Cliff, A. D., Ord, J. K. Spatial Autocorrelation. London, UK, Pion, 1973.
Dai, J., Raza, A., Wang, T., et al. Impact of CO2-Brine-Shale interaction on wettability change at reservoir temperature and pressure via AFM characterization. Energy & Fuels, 2024, 38(21): 21042-21051.
Derjaguin, B., Muller, M., Toporov, Y. P. Effect of contact deformations on the adhesion of particles. Journal of Colloid and Interface Science, 1975, 53(2): 314-326.
Dickinson, L. R., Suijkerbuijk, B. M. J. M., Berg, S., et al. Atomic force spectroscopy using colloidal tips functionalized with dried crude oil: A versatile tool to investigate oil-mineral interactions. Energy & Fuels, 2016, 30(11): 9193-9202.
Emmanuel, S., Eliyahu, M., Day-Stirrat, R. J., et al. Impact of thermal maturation on nano-scale elastic properties of organic matter in shales. Marine and Petroleum Geology, 2016, 70: 175-184.
Emmanuel, S., Ruarri, J. M. E., Stirrat, D., et al. Softening of organic matter in shales at reservoir temperatures. Petroleum Geoscience, 2017, 23(2): 262-269.
Feng, G., Zhang, L., Yan, J., et al. Lithofacies-based analysis of pore structure characteristics and controlling factors of shale reservoirs: A case study of the second member of the Kongdian Formation in the Cangdong Sag, Bohai Bay Basin, China. Marine and Petroleum Geology, 2025, 182: 107575.
Giergiel, M., Zapotoczny, B., Czyzynska-Cichon, I., et al. AFM image analysis of porous structures by means of neural networks. Biomedical Signal Processing and Control, 2022, 71: 103097.
Goodarzi, M., Rouainia, M., Aplin, A., et al. Predicting the elastic response of organic-rich shale using nanoscale measurements and homogenisation methods. Geophysical Prospecting, 2017, 65(6): 1597-1614.
Graham, S. P., Rouainia, M., Aplin, A. C., et al. Geomechanical characterisation of organic-rich calcareous shale using AFM and nanoindentation. Rock Mechanics and Rock Engineering, 2021, 54: 303-320.
Griffith, A. A. VI. The phenomena of rupture and flow in solids. Philosophical Transactions of the Royal Society of London, 1921, 221(582-593): 163-198.
Hou, Y., Yu, R., Li, J., et al. Molecular structure characterization of kerogen in contact metamorphic shales: Insights into the effect of graphitization on organic matter pores. AAPG Bulletin, 2024, 108(4): 633-662.
Iqbal, M. A., Rezaee, R., Smith, G., et al. Shale lithofacies controls on porosity and pore structure: An example from Ordovician Goldwyer Formation, Canning Basin, Western Australia. Journal of Natural Gas Science and Engineering, 2021, 89: 103888.
Jiang, X., Han, X., Cui, Z. New technology for the comprehensive utilization of Chinese oil shale resources. Energy, 2007, 32(5): 772-777.
Karamov, T., White, V., Idrisova, E., et al. Alterations of carbonate mineral matrix and kerogen micro-structure in domanik organic-rich shale during anhydrous pyrolysis. Minerals, 2022, 12(7): 870.
Khatibi, S., Ostadhassan, M., Tuschel, D., et al. Raman spectroscopy to study thermal maturity and elastic modulus of kerogen. International Journal of Coal Geology, 2018, 185(2): 103-118.
Li, C., Ostadhassan, M., Guo, S., et al. Application of peakforce tapping mode of atomic force microscope to characterize nanomechanical properties of organic matter of the Bakken Shale. Fuel, 2018, 233: 894-910.
Li, J., Li, X., Wu, K., et al. Thickness and stability of water film confined inside nanoslits and nanocapillaries of shale and clay. International Journal of Coal Geology, 2017, 179(15): 253-268.
Li, J., Shan, X., Song, X., et al. Evaluation of the organic matter product of Huadian oil shale during pyrolysis using multiple approaches: Guidance for the in situ conversion of oil shale. Journal of Analytical and Applied Pyrolysis, 2022, 167: 105656.
Li, Z., Duan, Y., Peng, Y., et al. A laboratory study of microcracks variations in shale induced by temperature change. Fuel, 2020, 280(15): 118636.
Liang, Z., Jiang, Z., Xue, Z., et al. Molecular structure and evolution mechanism of shale kerogen: Insights from thermal simulation and spectroscopic analysis. Journal of Analytical and Applied Pyrolysis, 2024, 181: 106648.
Liu, Q., Chen, T., Zhang, H., et al. Experimental investigation of permeability evolution in deep reservoirs under true triaxial stress: A review. Gas Science and Engineering, 2025, 144: 205739.
Loucks, R. G., Reed, R. M., Ruppel, S. C., et al. Spectrum of pore types and networks in mudrocks and a descriptive classification for matrix-related mudrock pores. AAPG Bulletin, 2012, 96: 1071-1098.
Lovric, M. International Encyclopedia of Statistical Science. Berlin, Germany, Springer, 2025.
Mazumder, M., Bal, A., Tripathy, A., et al. Multiscale assessment of transformation in pore system of shale during combustion: An insight into poromechanical response and sorption dynamics. Energy & Fuels, 2024, 38(18): 17510-17524.
Moran, P. A. P. Notes on continuous stochastic phenomena. Biometrika, 1950, 37(1-2): 17-23.
Paruchuri, A., Wang, Y., Gu, X., et al. Machine learning for analyzing atomic force microscopy (AFM) images generated from polymer blends. Digital Discovery, 2024, 3(12): 2533-2550.
Saif, T., Lin, Q., Bijeljic, B., et al. Microstructural imaging and characterization of oil shale before and after pyrolysis. Fuel, 2017, 197: 562-574.
Song, D., Wu, C., Tuo, J. Relationships between organic structure carbonization and organic pore destruction at the overmatured stage: Implications for the fate of organic pores in marine shales. Energy & Fuels, 2022, 36(13): 6906-6921.
Song, Y., Li, Z., Jiang, Z., et al. Progress and development trend of unconventional oil and gas geological research. Petroleum Exploration and Development, 2017, 44(4): 675-685.
Sun, C., Nie, H., Su, H., et al. Porosity, permeability and rock mechanics of Lower Silurian Longmaxi Formation deep shale under temperature-pressure coupling in the Sichuan Basin, SW China. Petroleum Exploration and Development, 2023, 50(1): 85-98.
Sun, Q., Zhang, W., Qian, H. Effects of high temperature thermal treatment on the physical properties of clay. Environmental Earth Sciences, 2016, 75, 610.
Vishal, V., Rizwan, M., Mahanta, B., et al. Temperature effect on the mechanical behavior of shale: Implication for shale gas production. Geosystems and Geoenvironment, 2022, 1(4): 100078.
Vranjes-Wessely, S., Misch, D., Kiener, D., et al. High-speed nanoindentation mapping of organic matter-rich rocks: A critical evaluation by correlative imaging and machine learning data analysis. International Journal of Coal Geology, 2021, 247(1): 103847.
Wang, J., Zhang, Y., Liu, J., et al. Shale weak cementation model and elastic modulus prediction based on nanoindentation experiment. Petroleum Science, 2025, 22(5): 2123-2141.
Wang, L., Zhao, Y., Yang, D. Evolution of permeability and mesostructure of oil shale exposed to high-temperature water vapor. Fuel, 2021, 290(15): 119786.
Wang, Q., Wang, T., Zhong, P., et al. Study of the surface pore structure and micromechanical properties of the Longmaxi shale. Petroleum Science Bulletin, 2023a, 8(5): 626-636. (in Chinese)
Wang, Y., Cheng, H. Advances in microscopic pore structure characterization of fine-grained mudrocks. Energy & Fuels, 2023, 37(3): 1495-1510.
Wang, Z., Ma, Z., Zheng, L., et al. Dynamic evolution characteristics of the “source-reservoir” integration of gray marl and its geological significance to unconventional gas: Insights from pyrolysis experiments. Petroleum Science, 2023b, 20(2): 705-720.
Yan, H., Zhou, T., Zhou, X., et al. Non-monotonic evolution and spatial reorganization mechanism of thermally induced micro-damage in sandstone. Advances in Geo-Energy Research, 2025, 17(2): 135-148.
Zargari, S., Wilkinson, T. M., Packard, C. E., et al. Effect of thermal maturity on elastic properties of kerogen. Geophysics, 2016, 81(2): M1-M6.
Zhang, H., Jia, X., Wu, J., et al. Impact of inherent minerals on isothermal pyrolysis of oil shale: Characteristics and kinetics. Journal of Analytical and Applied Pyrolysis, 2025, 191: 107231.
Zhang, L., Yang, D., Zhao, K., et al. Investigation of high-temperature effects on the strengthening and degradation of mechanical property in sandstone. Applied Energy, 2024, 357(1): 122532.
Zhang, Y., Lebedev, M., Al-Yaseri, A., et al. Nanoscale rock mechanical property changes in heterogeneous coal after water adsorption. Fuel, 2018, 218: 23-32.
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