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The marine shale within the Sichuan Basin constitutes China's significant shale gas production, featuring old formation age, high degree of thermal evolution, multiple tectonic movements, and complex structural conditions. However, there are significant differences in the shale gas preservation conditions and reservoir quality in different areas, limiting future large-scale exploration and development. Pore structure significantly influences shale reservoir quality, gas content, and exploration of shale gas occurrence, migration, and enrichment mechanisms. The influence of structural-dominated preservation conditions on shale pore structures is essential to comprehend for effective shale gas exploitation. This study employs field-emission scanning electron microscopy in conjunction with other techniques (low-temperature N2 adsorption, low-temperature CO2 adsorption, and nuclear magnetic resonance) for detailed analyses of the pore structure across varied structural zones, revealing the influence of structural attributes, fault systems, depth of burial, and formation pressure on pore architecture, and examining the relationship between pore structure and shale gas preservation conditions. The results show that stable structural condition is conducive to the development and preservation of shale pores. Structural compression causes inorganic and organic pores to become narrow and elongated due to shrinkage, with a significant increase in microfractures. The porosity of shale with stable structural conditions exhibits markedly increased porosity compared to samples under structural compressions. Under conditions of similar TOC and mineral composition, the pore size distribution (PSD), pore volume (PV), and specific surface area (SSA) of shale after structural compression are significantly lower than those of samples with stable structural conditions. As the burial depth increases, the shale porosity shows a decreasing trend, but the decrease is limited. Burial depth significantly impacts the SSA and PV of high-TOC samples (3%-6%). As the burial depth increases, both SSA and PV show a significant decreasing trend. When the burial depth reaches 4000 m, SSA and PV tend to concentrate. The formation pressure coefficient is an important factor for the development and preservation of shale pores, and porosity is positively correlated with the formation pressure coefficient. Increased formation pressure coefficient indicates superior preservation conditions and enhanced pore development. [ABSTRACT FROM AUTHOR]

The Wufeng-Longmaxi Formation shales with burial depths > 3 500 m in the southern Sichuan Basin are believed to have large shale gas potentials. However, the reservoir properties and gas-in-place (GIP) contents of these shales exhibit variations across different sublayers. In this study, a set of Wufeng-Longmaxi shales with burial depths of 4 000–4 200 m was derived from the Well Y101H2 in the Luzhou area, and the differences in geological and geochemical characteristics, porosity, water saturation and GIP content of various sublayer shales were investigated. The results indicate that the TOC content and effective porosity of the upper (LMX1-4) and lower (LMX1-3) sublayer shales of the first member of the Longmaxi Formation are better than those of the Wufeng Formation (WF) shales, which results in the LMX1-4 and LMX1-3 shales having higher GIP contents than the WF shales. The GIP contents of the LMX1-3 shales are higher than those of the LMX1-4 shales, and this is likely because the organic matter of the LMX1-3 shales had more aquatic organisms and was preserved in a stronger reductive environment, which leads to a stronger gas generation potential. In contrast to the middle-shallow LMX1-4 shales in the Sichuan Basin, the deep LMX1-4 shales in the Luzhou area have advantageous reservoir properties and GIP contents, and thus it is promising to synchronously exploit the deep LMX1-4 and LMX1-3 shales in some regions of the southern Sichuan Basin. [ABSTRACT FROM AUTHOR]

In the Luzhou Block of the southern Sichuan Basin, the deep Longmaxi shales have become important exploration targets in recent years. However, the water-bearing properties of these shales are still unclear, which significantly limits evaluations of reservoir pore structures and gas-in-place (GIP) contents. In this study, twelve fresh shale core samples were collected at the well site, and the pore water (CPW) and equilibrium water (CEW) contents, as well as the pore structures of the shales, were analyzed under both as-received and dried conditions. The results indicate that the deep shales have low water-bearing extents with a pore water content (CPW) of 3.82–16.67 mg/g, and that both the organic matter (OM) and inorganic matter (IM) pores can be used for pore water storage. The extent of influence of pore water on nonmicropores and IM pore structures is more significant than that on micropores and OM pore structures. Meanwhile, the pore water obviously reduces the retention effects of nanopores and may block nanopores with pore widths < 0.5 nm. An average of 40% of pore spaces were taken up by pore water in the studied deep shales in the Luzhou Block, and the residual pore surface area and pore volume of the shales were mainly contributed from micropores and nonmicropores, respectively. [ABSTRACT FROM AUTHOR]

Fluid charging and formation pressure evolution are of great significance for shale gas exploration and development. Taking the Longmaxi formation shale in southeast Chongqing as the research object, the fluid activity and pressure evolution process were studied by means of thin section observation, fluid inclusion analysis and testing, and basin numerical simulation. The results show that the area of the southeast of Chongqing, the Longmaxi formation of dike filling minerals, is mainly quartz vein and calcite part of the veins and arteries, and vein body captures the rich organic inclusions in minerals, sees fgas-liquid two-phase brine inclusions and methane inclusions, combining with the temperature and salinity of brine inclusions, and shows that the area has experienced two phases of oil and gas filling, the first period of gas-liquid fluid. The second stage is gas fluid. Combined with burial history and thermal maturation history, it is found that the filling time of oil and gas is late Cretaceous and Paleocene, respectively. In the Cretaceous, the pressure coefficient of Longmaxi formation reached the maximum value of 2.2 and remained above 1.5 overpressure after pressure unloading in the later period. In terms of the frequency of inclusions, the charging amount of the first stage is relatively large, and the charging time corresponds to the peak period of the palaeo-formation pressure. At the same time, fluid charging can timely supplement the pressure after unloading, which is conducive to high and stable production of shale gas. [ABSTRACT FROM AUTHOR]

The characterization of organic nanopores across the entire range is essential for gas storage and productivity evaluation of marine shale. To achieve a precise and comprehensive analysis of organic nanopore properties, an integration method of helium ion microscope (HIM) and scanning electron microscope (SEM), as well as focused ion beam-HIM (FIB-HIM) and FIB-SEM, was proposed. This integration method extends the organic pore imaging and quantitative analysis to below 10 nm. Results demonstrate that organic pores below 10 nm significantly impact the evaluation of shale gas storage and productivity by contributing to the porosity and specific surface area and altering pore size distribution and connectivity characteristics. The surface porosity increases by 10.73%, while the specific surface area increases by 76% according to the integration method. The integrated pore size distribution converts the unimodal PSD from the stitched SEM mosaic to a multimodal PSD, supporting the multi-stage formation mode of organic nanopores: larger bubble pores appear with oil generation at the early stage, while smaller spongy pores appear with gas generation at the later stage. The organic pores revealed by FIB-HIM have higher coordination numbers and a higher proportion of inner-connected volume, showing the more complex connectivity characteristics. Despite limitations due to heterogeneity and inadequate resolution, these novel insights by the integration method highlight the importance of exploring organic pores at the nanoscale and have the potential to inform further research in this field. • Organic nanopore size distribution in marine shale is corrected to a multimodal curve by the integration of HIM and SEM. • Organic nanopores beyond the SEM resolution significantly impact the evaluation of shale gas storage and productivity. • The integration of HIM and SEM provides more accurate and representative characteristics of organic pores in marine shale. [ABSTRACT FROM AUTHOR]

In order to improve the seepage channels in shale, soaking operation is often conducted after fracturing to carry out full shale hydration by the fracturing fluid. Previous research has mainly focused on the changes in the overall pore volume of shale due to hydration, but there is a lack of understanding on the volume changes of varied-size pores during the hydration process. In this study, a nuclear magnetic resonance (NMR) measurement method was carried out to obtain the size distribution of the pores in the shale in its unaltered state using ethanol as the saturation medium. Subsequently, through experiments, the shale core was saturated with fracturing fluid, and the dynamic changes in the pore size distribution under hydration were monitored using the low-field NMR technique. In addition, the relationships between the type of clay, the salinity of the fracturing fluid and the volume changes of varied-size pore were analyzed. The results of this study indicate that when the shale and fracturing fluid underwent hydration, the increase in the volumes of varied-size pores was concentrated in a certain pore-size area. This pore -size area was related to the type of clay that the shale contained. There was a strong correlation between the mixed-layer illite-smectite content and the increase in the small meso-pore volume. And the same between the illite content and the increase in the micro-pore volume. The saline fracturing fluid had an inhibitory effect on the shale hydration, mainly in the micro-pore domain. The results of this study is significant to optimize the selection of shale gas reservoirs and fracturing fluids for use in soaking measures. • A NMR method was proposed to obtain the unaltered pore-size distributions in shale. • The relationship between the type of clay and increasing pore-size was obtained. • The inhibitory effect of high-salinity solution mainly occurs in the micro-pores. [ABSTRACT FROM AUTHOR]

Currently, Luzhou in the Sichuan Basin is a focal point for shale-gas exploration and development in China. However, a lack of detailed research on the mineral composition of the Wufeng Formation-Longmaxi Formation (WF-LF) shale is hindering the extraction of deep-buried shale gas in the Luzhou shale play. Herein, a field emission scanning electron microscope (FESEM) equipped with the Advanced Mineral Identification and Characterization System (AMICS) software was employed to analyze the mineral composition of the WF-LF shale from six wells in Luzhou. Quartz was the dominant mineral type, (16.9–87.21%, average 51.33%), followed by illite, calcite, dolomite, and pyrite. Our study revealed that (1) quartz content showed a moderate positive correlation with the total organic carbon (TOC) content, indicating that the quartz found in the shale is mostly of biological origin; and (2) the sum content of siliceous minerals and carbonaceous minerals was moderately positively correlated with the brittleness index (BRIT) in well SS1H2-7 and in the well group of RS8 and RS5, indicating that the siliceous minerals and carbonaceous minerals had an active effect on reservoir compressibility. Finally, according to the mineralogical features of each sublayer, we identified four types of reservoirs to determine their scope for exploration. [ABSTRACT FROM AUTHOR]

In this study, shale cores from 20 wells in the S1l11-1 sublayer of Longmaxi Formation buried in shallow shale (<3500 m) and deep shale (>3500 m) in the southern Sichuan Basin, China were collected to compare their pore structures and gas-bearing properties using multiple experiments. Results showed that the deep layer has relatively lower brittle mineral content, which is disadvantageous in terms of the higher requirements it imposes on hydraulic fracturing. Results also showed that the most important factor controlling the differential enrichment of S1l11-1 shale gas in southern Sichuan Basin is porosity. Moreover, the porosity composition of shallow shale and deep shale has significant differences: the porosity of shallow shale is dominated by organic pores, while for deep shale, both organic and inorganic pores are important. The inorganic pores provide significant storage space for free gas in deep shale; their contribution warrants more attention. We also found that the difference in organic porosity of the shallow and deep shale samples resulted from large differences in pore development ability, while the highest inorganic porosity was concentrated near the optimal mineral composition when the content of quartz plus feldspar plus pyrite was about 70%. This study revealed the primary factor controlling the difference in gas content between shallow and deep shale and detailed the characteristics of microscopic pore structure, providing a basis for the exploration and development of deep shale gas in the Wufeng-Longmaxi Formation in the southern Sichuan Basin. [ABSTRACT FROM AUTHOR]

The permeability of shale in unconventional subsurface reservoirs under high-temperature and high effective stress conditions is of great significance for evaluating the extraction efficiency of shale gas and determining reservoir development programs. In this study, a series of permeability experiments using nitrogen gas were conducted on a sample from the lower Longmaxi Formation over a range of temperature (25–100 °C), effective stress (22.5–52.5 MPa), and pore pressure (0.5–8 MPa) conditions. The dynamic relationships between permeability and temperature, effective stress, and pore pressure are analyzed in detail. The results show that the apparent permeability decreases approximately linearly with increasing pore pressure, temperature, and effective stress. The absolute permeability also decreases with increasing temperature or effective stress. Upon increasing the reservoir depth by 1000 m , the permeability decreases by an average of approximately 25%. Approximately two-thirds of this decline is caused by changes in the effective stress and approximately one-third by changes in temperature. The Klinkenberg parameter is also found to be positively correlated with temperature and effective stress. The results herein provide important guidance for evaluating permeability changes and the extraction efficiency for deep shale gas development. • The shale permeability was measured at different pressure and temperature. • The Klinkenberg parameter is positively correlated with temperature and stress. • A model is developed to describe the gas permeability with respect to burial depth. [ABSTRACT FROM AUTHOR]

• High-pressure methane adsorption isotherms of 106 Wufeng-Longmaxi shales are measured. • Organic matter and clay are main compositions controlling factors of methane adsorption. • The isotherm of a shale is a linear superposition of those of its organic matter and clay. • V L , P L and ρ ads are found to be definite but different for unit organic matter and clay. • A quantitative composition-based model for adsorbed methane amount are proposed. The Wufeng-Longmaxi Formation shale in Sichuan Basin is the main strata of shale gas exploration and development in China. Adsorbed methane is an important part of the total shale gas content. The influence of shale composition on adsorption characteristics is complex, and it is difficult to obtain a comprehensive understanding without a sufficient amount of data. In this work, the total organic carbon (TOC), X-ray diffraction (XRD) mineral analysis, and the excess methane adsorption isotherms with pressure up to 50 MPa at 40 °C of 106 overmature shale samples with TOC of 0.8%-9.0% and clay content of 2%-58% that belong to Wufeng-Longmaxi formation from 10 shale gas wells in Sichuan Basin, China are experimentally investigated and analyzed. New correlations found between compositions and methane adsorption characteristic parameters guide the establishment of a composition-based methane adsorption model that the excess adsorption isotherm of shale is the content-weighted sum of equivalent unit-content excess isotherms for organic matter and clay. With this model, the differences of excess isotherms of these two compositions and the differences of clay-contribution to methane adsorption for different sublayers are disclosed. It is beneficial to improve the accuracy of shale reservoir evaluation of studied blocks under the condition of limited coring and deepening the understanding of the underlying mechanism of methane adsorption characteristics. [ABSTRACT FROM AUTHOR]