Pore Development Research Articles

Mechanism of the pore and molecular structure evolution of coal exposed to acid mine drainage (AMD)

In the post-extraction epoch, wastewater from mining activities, particularly acid mine drainage (AMD) residing in sulfur-laden coal terrains, assumes a pivotal role in the safety stewardship of decommissioned coal mines. This research aims to investigate the mechanism behind coal characteristic deterioration from prolonged exposure to AMD. Immersion assays were performed on coal samples across pH 2 to 5 to assess the impact of acid mine drainage. Subsequently, the pore and molecular architecture was appraised using microscopic methodologies. Computed Tomography (CT) findings elucidate that post-immersion, the porosity, and fissures proliferated longitudinally along the coal strata, engendering a marked amplification in surface porosity contiguous to pre-existing pores. This escalation in surface porosity was further accentuated in correlation with the intensification of AMD acidity. Nuclear Magnetic Resonance (NMR) data indicated a marginal augmentation in the content of both micropores and macropores within a tepid AMD milieu. However, in a more virulent AMD context, the proportion of micropores diminished, whereas that of macropores and pore throat size (PTS) experienced an upswing, thereby transmuting adsorptive pores into permeable conduits and consequently enhancing coal permeability. Scanning Electron Microscopy (SEM) corroborated the NMR outcomes; as AMD acidity transitioned from mild to severe, the coal matrix manifested many erosive pores, matrix layer disintegration, and an expansion in cleat width. Therefore, the microscopic pore evolution can be succinctly encapsulated as follows: in a mild AMD environment, dissolution of minerals predominates, generating erosive pores, whereas, in a more acidic AMD milieu, the matrix undergoes partial contraction, thereby augmenting pore volume, enhancing permeability, and inducing structural degradation. Additionally, Fourier Transform Infrared Spectroscopy (FTIR) analysis substantiated that AMD compromised the pore architecture and catalyzed the disintegration of coal macromolecules into lower molecular weight constituents. Therefore, AMD degrades coal macromolecules into smaller compounds, heightening matrix layer porosity and impairing coal characteristics. This research yields vital insights for the security and efficient management of abandoned mine excavations.

Production and characterization of activated carbon derived from orange peel for the adsorption of methylene blue dye

Activated carbon was produced from orange peel using H2SO4 and ZnCl2 as activating agents at a temperature of 400 oC. The impregnation was done in 1:1 (wt/v). FTIR analysis of the precursor and activated carbon shows different functional groups present in the precursor and activated carbon. The FTIR spectral also shows shifts in bands and changes in wave number between the precursor and activated carbon indicating chemical transformation during activation and carbonization. SEM analysis was used to study the internal structure and pores development of the activated carbon. The methylene blue adsorption capacity of the activated carbon was determined using standard methods. Langmuir and Freundlich adsorption isotherms were employed in determining the adsorption process and Pseudo first-order and Pseudo secondorder kinetics were employed in determining the rate of adsorption by the adsorbents.

Multiscale Fractal Characterization of Pore–Fracture Structure of Tectonically Deformed Coal Compared to Primary Undeformed Coal: Implications for CO2 Geological Sequestration in Coal Seams

The tectonically deformed coal (TDC) reservoirs with abundant gas resources and low permeability are expected to become one of the target coal seams for carbon dioxide geological storage-enhanced coalbed methane recovery (CO2-ECBM). The pore–fracture structure plays a crucial role in determining the effectiveness of CO2 storage. Fractal analysis provides a valuable approach to quantitatively describe the complex and heterogeneous pore–fracture structures across various scales in coal matrixes. Accordingly, the TDC samples in the Huainan–Huaibei coalfield and primary-undeformed coal (PUC) samples in the Qinshui Basin were selected for pore–fracture structure parameter tests using the mercury intrusion porosimetry (MIP) and low–temperature nitrogen adsorption (LNA) methods. Their multiscale pore–fracture parameters were analyzed using different fractal methods based on pore diameter. According to the fractal results, a multiscale classification standard for pore–fracture structures was devised in this study that is suitable for the controlling gas migration process. A parameter of 8 nm is set as the separating pore diameter for gas migration and storage. It was observed that the connectivity of migration pores (>8 nm) in TDC samples was stronger compared to PUC samples, reflected in larger pore volumes and smaller fractal dimensions. However, its complex development of seepage pores (150–300 nm) may hinder the flow of CO2 injection. As for the storage pores (<8 nm), the fractal dimension of the 2–8 nm pores in TDC was found to be similar to that of PUC but with larger pore volumes. The fractal dimension of the filling pores (<2 nm) in TDC samples was relatively lower, which facilitates efficient gas volume filling. Therefore, the pore–fracture structure of the TDC samples is found to be more advantages for CO2 injection and storage compared to the PUC. This suggests that TDC reservoirs holds promising geological potential for CO2-ECBM implementation.

Toward a Nanoscale‐Defect‐Free Ni‐Rich Layered Oxide Cathode Through Regulated Pore Evolution for Long‐Lifespan Li Rechargeable Batteries

AbstractNi‐rich layered oxides are envisioned as the most promising cathode materials for next‐generation lithium‐ion batteries; however, their practical adoption is plagued by fast capacity decay originating from chemo‐mechanical degradation. The intrinsic chemical–mechanical instability, inherited from atomic‐ and nanoscale defects generated during synthesis, is not yet resolved. Here, atomic‐ and nanoscale structural evolution during solid‐state synthesis of Ni‐rich layered cathode, Li[Ni0.92Co0.03Mn0.05]O2, is investigated using combined X‐ray/neutron scattering and electron/X‐ray microscopy. The multiscale analyses demonstrate the intertwined correlation between phase transition and microstructural evolution, with atomic‐scale defects derived from the decomposition of precursors leading to the creation of intra/inter‐granular pores. The nucleation and coalescence mechanism of pore defects during the synthesis of Ni‐rich layered cathodes are quantitatively revealed. Furthermore, a modified synthetic route is proposed to effectively circumvent the formation of nanoscale defects in Ni‐rich layered cathodes by facilitating uniform synthetic reactions, resulting in superior electrochemical and microstructural stability.

Kerogen structure and porosity in Woodford Shale before and after hydrous closed-system pyrolysis

Micro-plugs of the Upper Devonian to Lower Mississippian Woodford Shale from the Ardmore Basin in southern Oklahoma were analyzed before and after hydrous pyrolysis (300, 320, 330, and 340 °C for 24 h) by using a combination of μ-FTIR, CP-Py-GC/MS, BIB-SEM-EDS techniques to investigate kerogen transformation and evolution of pore space.Tasmanites and Leiosphaeridia in Woodford Shale are abundant macerals characterized by relatively long, unbranched alkyl chains, with an additional carboxyl component, and a minor contribution of aromatic structures based on μ-FTIR spectra results. The aliphatic νasCH2/ νasCH3 ratios show almost no correlation with pyrolysis temperatures, except for a minor increase of the ratio for both samples after pyrolysis at 330 °C, which may be attributed to cracking of C-C bonds next to a tertiary carbon atom. A decreasing aliphaticity and increasing aromaticity for alginite with increasing pyrolysis temperature and thus thermal maturity is indicated by the reduction of aliphatic CHx stretching bands and increasing γCH/ νCHx ratios. The relative abundance of olefinic bonding (νC=C) decreases in alginite compared to aromatic hydrogen (γCH) with higher pyrolysis temperature, and thus formation of monoaromatic rings is indicated by the condensation ratios (γCH/ νC=C); similar observations have been made on natural maturation series.This is in line with the CP-Py-GC/MS results on whole kerogen showing an increase of aromatic structures over aliphatic pyrolysis products with increasing thermal maturities, though with some differences between the two samples investigated. The differences are probably related to higher alginite/bituminite ratios in one of the samples, which also contain more N-compounds. In contrast, the other sample enriched in bituminite contains more S-compounds. Both FTIR spectra and EDS results document a loss of carbonyl/carboxyl C=O functional groups and/or O content with thermal maturation. The hydrocarbon generation potential parameter “A-Factor” (νCHx/ νCHx + νC=C), analyzed on alginite in this study, is rather consistent at different pyrolysis temperatures with a value of about 0.9 and with a slight tendency of higher values at higher pyrolysis temperatures.SEM observations show that there is no significant occurrence of microfractures in the initial samples and after pyrolysis at 300 °C, while microcracks and organic pores formed pore networks when pyrolysis temperature increased from 320 °C to 340 °C. Most of the newly generated cracks are parallel to the bedding. Mineral-filled Tasmanites cysts in Woodford Shale are silica-rich and may be related to the dissolution of siliceous tests (e.g., radiolarians).

3D microscale investigation of active deformation mechanisms of halite under conditions representative of underground hydrogen storage

To tackle the challenges raised by climate change, we need to rapidly switch our energy sources to low-carbon ones for all economic sectors. As renewable energies are intermittent, efficient energy carriers, such as hydrogen, will be needed to meet the energy demand. Green hydrogen is considered to be a promising energy vector for the future. However, in addition to problematics related to its production, safe and large scale storage solutions still need to be developed. The geological formations including saline aquifers and former depleted gas fields offer the largest storage capacities but are more adapted to seasonal or mid-to-long term storage. Conversely, underground salt caverns are well suited for storage/withdrawal cycles as short as daily cycling. These artificial structures, offering exceptional tightness, have already been used for decades for hydrocarbons storage but at seasonal storage/withdrawal cycles. The adaptation to short-term hydrogen storage still requires further studies to ensure the stability of the caverns under such loading conditions. Indeed, rapid cyclic loading conditions may impact the tightness and the integrity of the cavern [1, 6].
 Rock salt is polycrystalline material with an essentially viscoplastic behaviour, involving different micro-mechanisms such as crystal slip plasticity and grain boundary sliding. At mechanical loading conditions representative of those operated in storage caverns, the rock salt is characterized by non-linear viscous flow. The activation of grain boundary sliding is necessary to accommodate local plastic incompatibilities between neighbouring grains. It has been shown in uniaxial loading conditions but has not been verified in triaxial conditions yet [2, 4]. The presence of brine also affects the micro-mechanisms involved, with for example phenomena like dissolution-precipitation or diffusional mass transfer along grain boundaries, and can modify the mechanical behaviour [5].
 In our studies, we investigate the active micro-mechanisms in synthetic halite through in situ X-ray microcomputed tomography (XR-µCT) analysis and digital volume correlation (DVC) and damage quantification. To reproduce loading conditions representative of those in real salt caverns, we apply different confining pressures with a triaxial cell. This triaxial device, developed recently [3], is adapted to in situ XR-µCT tests. We study the development of damage networks and the evolution of pores during the deformation of rock salt under different confining pressures. Samples of halite are prepared by compaction of pure NaCl powder in dry and humid conditions. It gives samples with different brine contents and allows us to study the effect of brine on the deformation mechanims.
 An effect of brine is visible, as the cracks seem to appear earlier in the dry samples. On the µCT scans, cracks start to be visible for a lower strain in the case of dry samples compared to the case of wet samples. For a dry sample in uniaxial loading conditions, the cracks were already clearly visible and well formed in most of the sample at 1.3% axial strain. For a wet sample, very few cracks only start to become slightly visible in some areas at 1.45% axial strain. This could be due to the activity of mechanisms involving brine, such as dissolution-precipitation allowing for crack healing.
 The effect of the confining pressure is also noticeable. After unloading the wet sample and removing the confining pressure, we observed that the few cracks formed during the deformation of the sample opened up, indicating that the healing process was not
 complete. Dissolution and precipitation are kinetically slaw processes, which are mostly active at low strain rates. Therefore, further deformation experiments must also explore the effect of strain rate.
 Natural salt always contains some humidity. Therefore, the effect of brine in deformation and damage formation/healing mechanisms is important to understand, especially in the context of gas storage in salt caverns.

Shale Gas Exploration and Development Potential Analysis of Lower Cambrian Niutitang Formation and Lower Silurian Longmaxi Formation in Northwestern Hunan, South China, Based on Organic Matter Pore Evolution Characteristics

Shale gas production is obviously higher within the Silurian Longmaxi Formation than that of the Cambrian Niutitang Formation according to the drilling test results in the northwest Hunan area. To clarify the reasons behind this variation, core samples from the two sets of shales were studied for a comprehensive comparison and analysis of their organic matter (OM) pore structure. Methods were used, including the total organic carbon content test, the vitrinite reflectance test, X-ray diffraction, and focused ion-beam scanning electron microscopy (FIB-SEM). The results show that these two shales have similar reservoir characteristics, both with abundant organic matter and high content of brittle minerals. However, the Longmaxi shale with 2.3% to 3.0%Ro presents lower thermal maturity than the Niutitang shale with over 3.0%Ro. In the case of pore structure associated with OM, a huge difference exists between the two shales. The OM pore shape of the Longmaxi shale is very regular, being mostly round and oval, while the OM pore shape of the Niutitang shale is irregular, being flat with a thin middle and thick and elongated ends. An important factor affecting OM pore evolution is thermal maturity. In turn, the thermal maturity is controlled by the tectonic evolution process, especially the maximum paleo-burial depth. In conclusion, the paleo-burial depth of the Lower Cambrian Niutitang shale in northwest Hunan is too large, which leads to the excessive evolution of organic matter in the shale, and the physical and chemical properties are similar to graphite, which leads to the disappearance of OM pores. Shale gas has no effective reservoir space and is largely dispersed in geological history. At the same time, due to the insufficient hydrocarbon-generation evolution time of the Lower Silurian Longmaxi Formation shale in this area, the shale could not form enough gaseous hydrocarbons and a large amount of effective reservoir space (OM pores with regular shape and large pore size), and finally failed to become a gas reservoir. Therefore, the exploration and development potential of the marine shale gas of the Lower Cambrian Niutitang Formation and the Lower Silurian Longmaxi Formation in northwest Hunan is poor.

Differential Diagenesis and Pore Evolution Characteristics of Different Sedimentary Microfacies Reservoirs of Bioclastic Limestone: A Case Study of MB2-MC1 Section in X Oilfield in The Middle East

In order to clarify the differential diagenesis of different sedimentary microfacies of bioclastic limestone in Cretaceous M Formation in the Middle East and systematically analyze the characteristics of reservoir pore evolution, the data of regional geology, well logging, core, cast thin section, scanning electron microscope, three-dimensional CT and conventional porosity and permeability test are comprehensively used, taking MB2-MC1 section in X oilfield as an example, starting from the diagenesis and pore evolution of bioclastic-arene shoal, the characteristics of diagenesis of each sedimentary microfacies in different environments are analyzed, and the differential diagenesis, pore evolution process and its influence on physical properties are studied. It is showed that the reservoirs of MB2-MC1 section are mainly developed in the ramp shoal and platform margin shoal. The shoal facies can be further subdivided according to the type of bioclastic debris. The sedimentary microfacies determine the original fabric and bioclastic type of M Formation, and then control the diagenetic sequence and strength. Each sedimentary microfacies mainly experiences different degrees of mud crystallization and burrows in seawater environment, dissolution and cementation in atmospheric freshwater environment, compaction, pressure solution and dolomitization in burial environment. High energy microfacies have the characteristics of non-selective dissolution, mainly developing intergranular pores and intergranular dissolved pores. Medium energy microfacies have the characteristics of selective dissolution, mainly developing mould pores and intragranular pores. The medium-low energy microfacies have the characteristics of moderate cementation, moderate compaction and moderate-weak dolomitization, mainly developing intragranular pores and visceral foramen pores. The low energy microfacies have the characteristics of strong cementation, strong compaction and moderate dolomitization, mainly developing micropores, intercrystalline pores and visceral foramen pores, which are non-reservoirs.

Aluminum Foam Sandwich: Pore Evolution Mechanism Investigation and Engineering Preparing Optimization.

This paper employs an innovative investigation approach to study pore evolution in Al-Si-Mg-Cu alloy within aluminum foam sandwiches (AFS) by integrating data from heating-expansion ratio curves, in situ observation of synchronous radiation, and microscopic analysis of the matrix's microstructure at different stages. Additionally, the cavity design and plate type control for large-scale AFS production are explored. Findings categorize the precursor heating into three stages: rapid heating, solid-liquid transition, and stable foaming. During solid-liquid transition, the expansion rate experiences a sudden drop, associated with pore nucleation and edge cracking of precursors. Pores nucleate as elongated crack-like structures along the rolling direction, guided by the Mg-enriched regions. In stable foaming, these pores evolve, become spherical, and the matrix rapidly expands. Using square tubes for sealing on the preform cavity sides creates a dense edge zone during rolling, halting crack propagation into the powder core. Adopting edge sealing during foaming mitigates boundary effects, thereby improving AFS panel flatness.

Selective Photonic Gasification of Strained Oxygen Clusters on Graphene for Tuning Pore Size in the Å Regime.

Controlling the size of single-digit pores, such as those in graphene, with an Å resolution has been challenging due to the limited understanding of pore evolution at the atomic scale. The controlled oxidation of graphene has led to Å-scale pores; however, obtaining a fine control over pore evolution from the pore precursor (i.e., the oxygen cluster) is very attractive. Herein, we introduce a novel "control knob" for gasifying clusters to form pores. We show that the cluster evolves into a core/shell structure composed of an epoxy group surrounding an ether core in a bid to reduce the lattice strain at the cluster core. We then selectively gasified the strained core by exposing it to 3.2 eV of light at room temperature. This allowed for pore formation with improved control compared to thermal gasification. This is because, for the latter, cluster-cluster coalescence via thermally promoted epoxy diffusion cannot be ruled out. Using the oxidation temperature as a control knob, we were able to systematically increase the pore density while maintaining a narrow size distribution. This allowed us to increase H2 permeance as well as H2 selectivity. We further show that these pores could differentiate CH4 from N2, which is considered to be a challenging separation. Dedicated molecular dynamics simulations and potential of mean force calculations revealed that the free energy barrier for CH4 translocation through the pores was lower than that for N2. Overall, this study will inspire research on the controlled manipulation of clusters for improved precision in incorporating Å-scale pores in graphene.

Preparation of Activated Carbon from Korean Anthracite: Simultaneous Control of Ash Reduction and Pore Development

Anthracite stands as a valuable precursor for carbon materials, owing to its high carbon content. However, producing activated carbon from anthracite presents significant challenges due to its elevated ash content (23–40 wt%) and crystalline nature. The high ash content not only fails to contribute to the activation process but also obstructs pore formation on the carbon surface. To address these challenges, this study explores the preparation of activated carbon from anthracite using KOH activation. This method demonstrates remarkable efficacy in enhancing reactivity beyond the inherent physical properties of anthracite. In contrast to physical activation, the utilization of KOH as a chemical agent substantially enhances the specific surface area, resulting in a production yield of 62% and a specific surface area that reaches up to 1596 m2/g at a KOH/anthracite weight ratio of 4.0. Moreover, rinsing the activated sample with tap water achieves an ash removal rate of about 37.9%, surpassing twice the rate achieved through acid pretreatment (67.0%). A noteworthy observation from this study is the substantial reduction in the content of major ash components, such as silicon (Si) and aluminum (Al), both of which are prominent constituents in anthracite ash. Following KOH activation, their levels decrease by approximately 54% to 65%, respectively. These findings highlight the potential of utilizing available anthracite, even with elevated ash content, as a superior carbon material. Fundamentally, the KOH activation method serves a dual purpose: it effectively reduces ash content and promotes pore creation within a highly alkaline environment. This dual advantage positions the method as a promising approach for the production of top-tier activated carbon.

Factors Controlling the Pore Development of Low-Mature Marine–Continental Transitional Shale: A Case Study of the Upper Permian Longtan Shale, Western Guizhou, South China

The Upper Permian Longtan Shale is a significant reservoir in western Guizhou. To clarify the main factors controlling the low-mature marine–continental transitional shale pore development in western Guizhou, pore types were classified with scanning electron microscopy (SEM), and the pore developmental stages and morphological structures were quantitatively characterized by nitrogen adsorption isotherm analyses. Additionally, the qualitative or semi-quantitative relationships between the pore developmental stages and the main controlling factors were established via geochemical analysis. The results showed that the Longtan Shale pores include intergranular pores, intragranular pores, organic pores, and microfractures. The intergranular pore structures were categorized into ink-bottle, slit, layered, and irregular types. The intragranular pores were found to be of the elliptical, nearly circular, ink-bottle, and irregular varieties. The organic pores were categorized into elliptical, bubble-like, and irregular polygonal variants. The microfractures were only of the elongated type. The clay-mineral-related intergranular pores were the predominant pore type. The organic pores were found to be poorly developed. The mesopores were predominant, followed by macropores. The shale pore diameters ranged between 1 nm and 100 nm, and they are characterized by multiple peaks. The specific surface area (SSA) was primarily provided by nanopores in the range of 5 nm to 10 nm, such that the smaller pores provided a greater contribution to the SSA, and they are more conducive to shale gas adsorption and accumulation. Clay mineral content was the dominant internal factor controlling pore development and the SSA, with the illite–smectite mixed layer being the most obvious controlling factor. While too low or too high clay mineral content is adverse to macropore development, brittle mineral content, carbonate mineral content, and total organic carbon (TOC) content are adverse to pore development and the SSA. Thermal maturity has no remarkable control effect on pore volume and the SSA of non-organic pores.

Pore connectivity and microfracture characteristics of Longmaxi shale in the Fuling gas field: Insights from mercury intrusion capillary pressure analysis

Assessing the connectivity of pores and the characteristics of microfractures is essential for comprehending gas migration mechanisms and effectively implementing development strategies in deep shale gas plays. The Fuling gas field, a prominent shale gas reservoir in China, holds promise for deep shale development. This requires a better understanding of variations in pore connectivity among shale samples from different depths of the Fuling gas field. To achieve this goal, this study employs innovative methodologies based on mercury intrusion capillary pressure (MICP), a recognized technique for evaluating material pore structures. In this research, we conducted MICP tests on shale samples of varying sizes to examine variations in pore structure and quantify inaccessible pores. Additionally, repeated MICP tests were performed on the same sample to investigate the spatial distribution of residual mercury and distinguish different pore types associated with flow conduits and storage spaces. Furthermore, a directional MICP experiment was carried out to quantitatively characterize the degree of pore development and anisotropy of microfractures by considering the direction of mercury intruding the sample (parallel or perpendicular to lamination). Our findings revealed that deep shale samples exhibited a higher proportion of inaccessible pores compared to mid-deep ones. Regarding accessible pores, a greater proportion of connected pores was observed in the deep shale samples, while the mid-deep shale samples exhibited a lower proportion. The results from the directional MICP experiment indicated that samples with anisotropy in mercury intrusion volume possessed finer and denser microfractures. However, no evidence was found to correlate the ratio of dead-end and connected pores with sample anisotropy. Overall, this study presents a novel approach for experimentally evaluating pore connectivity and microfracture characteristics in shale reservoirs using MICP. The outcomes contribute to enhancing our understanding of shale gas migration mechanisms, particularly in deep ultra-low-permeability reservoirs, and hold significant implications for future developments in the field.

Effect of Pore Evolution on Thermal Diffusivity and Radiation Characteristics of Thermal Barrier Coatings after High-Temperature Exposures

Studying the impact of pores is crucial to enhancing the service performance of coatings, since they are a typical microstructure feature of thermal barrier coatings. In this paper, a coating prepared by the APS method was employed as the study object, and a scanning electron microscope and optical microscope were used to calculate the porosity after spraying or high-temperature exposures. Based on this, numerical calculations and simulations were used to evaluate the impacts of the pore structure and porosity on the heat conductivity and radiation characteristics of the coating. The results showed that, at high-temperature exposures, the horizontal pores inhibited thermal conductivity and radiation, but the column pores increased heat conductivity and radiation. The heat conductivity of the coating linearly decreased as the porosity increased, whereas the extinction coefficient increased, although at a slower and slower pace. When the porosity reached 15%, if the porosity was further increased, the thermal radiation energy did not change much, indicating that increasing the porosity would only block the heat radiation to a certain amount. This new and time-saving technique for materials research utilizing simulation and numerical computing may be utilized to optimize the microstructure of coatings to increase their service performance.

Pore Structure and Geochemical Characteristics of Alkaline Lacustrine Shale: The Fengcheng Formation of Mahu Sag, Junggar Basin

Shale oil and gas are currently the major fields of unconventional hydrocarbon exploration and development. The Fengcheng Formation (FF) shale in the Mahu Sag of the Junggar Basin is an alkaline lacustrine organic-rich shale with an extremely prospective shale oil potential. However, its strong heterogeneity and complex pore structure greatly influence the development of shale oil. It is significant to investigate the pore and geochemical characteristics of shale reservoirs for shale oil extraction. In this study, the pore structure and geochemical characteristics of FF have been investigated using core analysis, Rock-Eval pyrolysis, X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), mercury injection capillary pressure (MICP), low-temperature gas adsorption (LTGA), and X-ray computed tomography (X-ray CT). The results show that the shale of FF has moderate organic matter abundance, and the kerogen is mainly of Type II, which is now at the peak of oil generation. Shale minerals are mainly composed of carbonate (dolomite and calcite) and siliceous (quartz and feldspar) minerals, with extremely low clay mineral content. The pore types are mainly intergranular pores (inter-P), intragranular pores (intra-P), and microfractures associated with mineral particles. The pore space is contributed predominantly by micropores of 0.5–1.2 nm and mesopores of 10–50 nm, whereas macropores are underdeveloped. The pores are mostly ink bottle- and slit-shaped, and the pore connectivity is relatively poor. The pore development of shale in the FF is influenced by organic matter abundance, thermal maturity, mineral composition, etc. Organic matter content (TOC), thermal maturity (Ro), and carbonate minerals have a positive effect on pore development, and the pore volume (PV) increases with TOC, Ro, and carbonate minerals. While clay minerals show a negative effect, the PV decreases with clay minerals. Additionally, the influence of the clay mineral content on the pore morphology of shale should not be ignored. This study investigates the pore structure and geochemical characteristics of the alkaline lacustrine shale of FF in Mahu Sag, which is significant to deepen the understanding of alkaline lacustrine shale and to improve the production of shale oil.

Study on the evolution of microscopic pore structure of sandstone under freeze-thaw cycles

In cold regions, rocks undergo freeze-thaw (FT) cycles, leading to damage caused by the evolution of pores. This phenomenon significantly influences the rock mass stability. A comprehensive and accurate study of FT damage evolution in rock pores was conducted in this research. The microscopic morphology and pore size distribution (PSD) of sandstone samples subjected to FT cycles were measured utilizing scanning electron microscopy (SEM), nitrogen adsorption/desorption (NAD) method, and mercury intrusion porosimetry (MIP). Multifractal analysis was applied to explore the evolution of PSD. A gradual weakening of the cementation degree of mineral particles under FT cycles was observed based on SEM results, resulting in the formation of larger connected pores. A decrease of 37.3% in the number of pores was recorded after 40 cycles. According to NAD and MIP results, a greater effect on mesopores and large pores were found, with a minimal impact on micropores and transition pores. Multifractal characteristics were identified in the PSD of sandstone samples with different FT cycles. Initially, the connectivity of sandstone pores was found to decrease and then increase gradually after 10 cycles. Uneven PSD was observed to concentrate stress among pores, exacerbate frost heave damage, and drive the PSD towards a more uniform direction. It was concluded that the non-uniform degree of PSD does not consistently increase with FT cycles. The findings of this study can serve as a reference for further research on rock FT damage mechanisms.

Investigation of the oxidation mechanism of Si-Al2O3-fused mullite containing Ti2O3 composite

In this work, Si-Al2O3-fused mullite containing Ti2O3 composite was prepared and heat-treated at 1100 °C, 1300 °C and 1500 °C for 3 h respectively in an air atmosphere to explore its oxidation mechanism. The results show that the Si-Al2O3-fused mullite containing Ti2O3 composite has excellent oxidation resistance at evaluated temperatures. The reason for this is the formation of a complete oxide layer and a transition layer in the exterior to absorb and filter O2, allowing the interior without oxidation. The oxidation of Si and Ti2O3 in the exterior is accompanied by volume expansion. SiC and mullite are formed in the transition layer at 1300 °C. At 1500 °C, SiO2, mullite and Si2N2O are formed in the transition layer. O′-Sialon and Ti(C, N)ss are formed in the interior of the samples at both 1300 °C and 1500 °C. At 1100 °C, Si oxidizes to form SiO2 coating on the surface of Si particles. The industrial CT characterization of the pore evolution of the samples after oxidation is consistent with the oxidation mechanism. A reaction model is developed.

Study on the Characteristics of Pore Change in Tuff under the Frost and Salt Action Using High-Precision CT Scanning Equipment

Using high-precision CT scanning equipment, two series of tests on frost and salt weathering were conducted to investigate the characteristics of pore change in tuff. Experiments on frost and salt aging were performed with pieces of tuff from the same area of southeast China. One set of tuff samples was soaked in saturated sodium sulfate or magnesium sulfate solutions for 60 days. Another set of tuff samples were subjected to 60 freeze–thaw cycles after being submerged in saturated sodium sulfate or magnesium sulfate solutions for 48 h. Our study demonstrates that processes such as salt erosion and freeze–thaw affect the pore evolution of tuffs significantly. Tuff lost 1.56% of its mass after being submerged in magnesium sulfate solutions for 60 days, while tuff submerged in sodium sulfate solutions gained a negative 0.33% of its mass. After 60 freeze–thaw cycles, the mass loss of tuff samples immersed in sodium sulfate, magnesium sulfate, and distilled water solutions was 3.52%, 3.58%, and 3.82%, respectively. The average porosity of the magnesium sulfate and sodium sulfate test groups increased by 6.59% and 4.14%, respectively, when the number of days of salt erosion was extended from 10 to 60 days. The average porosity of tuff samples immersed in magnesium persulfate and sodium sulfate solutions increased by 2.25% and 2.18%, respectively, as the number of freeze–thaw cycles went from 10 to 60.

Radon exhalation characteristics after pyrolysis of long flame coal

Coal pyrolysis is a important method for classifying and utilizing coal resources and contributes to enhanced comprehensive resource utilization. However, In high-temperature areas such as coal pyrolysis, there is an abnormal phenomenon release of radioactive gas radon, understanding the relationship between temperature and radon exhalation characteristics, as well as the underlying mechanisms, holds great importance for assessing radon pollution in mining areas. After coal undergoes pyrolysis under high temperature conditions, its material composition, pore structure, water content, and other properties have changed. The pyrolysis products in different atmosphere environments have differences, and the characteristics of radon emission are also different. To address this, the present study conducted coal pyrolysis experiments in both aerobic and anaerobic environments, using long flame coal sourced from Yulin, China. The radon release concentration of the pyrolysis products was measured. The research findings indicate that during pyrolysis at elevated temperatures, the ratio of coal mass loss is constantly increasing. High temperatures promote the development of pores and fissures, and significant changes in coal properties at temperature thresholds (300 °C and 500 °C). The specific surface area, pore volume, and fracture ratio all display substantial increases, and the amplitude of change is greater under aerobic conditions. The fractal dimension of total pores and macropores shows continuous growth, while the specific surface area, pore volume, and fracture ratio exhibit a strong negative correlation with the radon emission rate of pyrolysis products. The expansion and penetration of pores and cracks, along with the release of a substantial amount of pyrolysis gas, accelerate the transformation, migration, and exhalation of radon, resulting in a negative correlation between the heat treatment temperature and the radon release rate of pyrolysis products. Under aerobic conditions, the radon release rate of pyrolysis products decreases more significantly.

The Influence of Chitosan on Water Absorption and Solubility of Calcium Phosphate Cement

Calcium phosphate cements are widely used biomaterials for bone regeneration due to their biological properties, such as biocompatibility, biodegradability, and bioactivity. The presence of chitosan in cement composition influences the resorption rate of the material and its mechanical properties. In the present work, the water absorption and solubility of a tricalcium phosphate bone cement, prepared with and without chitosan addition, was comparatively evaluated. The absorption and solubility properties were monitored for 21 days by immersing the samples in water at room temperature and then weighing them. A morphological analysis of the samples was carried out via scanning electron microscopy (SEM). The absorption dynamics and pore evolution were investigated with low-field nuclear magnetic resonance (NMR) relaxometry. It was demonstrated that the presence of chitosan accelerates the hardening dynamics, reduces water absorption, and influences the solubility and degradation behavior of the cement. It was also observed that, independent of the presence of chitosan, the polymerization process is not completed even after one hour, which influences the solubility process. It was also shown that the presence of chitosan reduces the amount of microcracks and improves the functional properties of the hardened cement.