Porous Structure Research Articles

Effect of N,N′-Methylenebisacrylamide on properties of porous semi-IPN hydrogels from Acrylamide, Maleic Acid, and its use for Urea absorption

Hydrogel is a three-dimensional polymer that can absorb large amounts of reagents while maintaining structural integrity. This material has been applied in many fields especially in smart agriculture. To improve the economic viability, the reusability of hydrogels in agricultural engineering over multiple cycles of adsorption and desorption is an urgent requirement. This can be solved if the crosslinker is used properly. Therefore, in this work, a series of porous semi-IPN hydrogels based on linear polyacrylamide, acrylamide, maleic acid, and N,N′-methylenebisacrylamide (MBA) were synthesized. The hydrogels were evaluated for the impact of MBA content on the characteristics and applicability as a urea fertilizer carrier. The chemical composition, morphology, mechanical, and rheological properties, swelling behavior, urea absorption and desorption of hydrogels with crosslinker content in the range of 0.5-2.0 % were investigated. The porous structure was confirmed by scanning electron microscopy images. Changing the MBA content significantly affected all characteristics of the hydrogels. In particular, increasing the MBA content decreased the equilibrium swelling ratios in all investigated environments. The maximum amount of urea loaded into the hydrogel was also reduced from 435.88 to 188.50 mg/g. This increase also changed the swelling mechanism from non-Fickian to Fickian, whereas the urea release mechanism changed from Fickian to non-Fickian. Finally, the hydrogels demonstrated stability in soil over multiple cycles of water absorption and release. This study provides valuable insights into designing a semi-IPN hydrogel with desired properties that meet the application requirements of modern farming techniques.

Three-Dimensional Printing of Metallic Parts by Means of Fused Filament Fabrication (FFF)

Obtaining metallic parts via Additive Manufacturing can yield several advantages over using other traditional manufacturing methods such as machining. Material extrusion (MEX) can handle complex shapes with porous structures and, at the present time, much low-end and desktop equipment is available. In the present work, different industrial and medical applications of metallic Fused Filament Fabrication (FFF) parts are presented. First, an overview of the process, equipment, and of the metal-filled filaments currently available is provided. Then, the properties of parts and different applications are shown. For example, metal-filled filaments with a low metal content that can be used to obtain plastic parts with metallic appearance (with either steel, copper, or bronze), and filaments with a high metallic content allow obtaining metallic parts with high mechanical strength after a sintering operation. The present contribution aims to be an up-to-date panorama for current industrial and medical results and lessons learnt from the application of FFF to obtain metallic parts.

Phase-field based shape optimization of uni- and multiaxially loaded nature-inspired porous structures while maintaining characteristic properties

AbstractTriply periodic minimal surfaces (TPMS) are highly versatile porous formations that can be defined by formulas. Computationally based, load-specific shape optimization enables tailoring these structures for their respective application areas and thereby enhance their potential. In this investigation, individual sheet-based gyroid structures with varying porosities are specifically optimized with respect to their stiffness. A modified phase-field method is employed to establish a simulation framework for the shape optimization process. Despite constant volume and the preservation of the periodicity of the unit cells, volume redistribution occurs through displacement of the interfaces. The phase-field-based optimization process is detailed using unidirectional loading on three gyroidal unit cells with porosities of 75 %, 80 %, and 85 %. Subsequently, the gyroidal unit cell with a porosity of 85 % is shape-optimized under multidirectional loading. A subsequent experimental validation of the unidirectionally loaded cells confirms that the shape-optimized structures exhibit, on average, higher stiffness than the non-optimized structures. The highest increase of 40 % in effective modulus is achieved with the gyroid structure having a porosity of 75 %, while maintaining minimal alteration to the surface-to-volume ratio and preserving periodicity. Additionally, the experimental data show that the optimization process resulted in a shift in the linear elasticity and plasticity range. In summary, the phase-field method proves to be a valid optimization technique for complex porous structures, allowing the preservation of characteristic properties.

Micro-CT Analysis of Pore Structure in Upland Red Soil Under Different Long-Term Fertilization Regimes

This study hypothesized that long-term fertilization alters the pore structure and aggregate stability in upland red soil. A long-term fertilization experiment in Qiyang, Hunan, was conducted with three treatments: no fertilization (CK), nitrogen–phosphorus–potassium fertilization (NPK), and nitrogen–phosphorus–potassium combined with pig manure (NPKOM). X-ray computed tomography (CT) scanning technology was used to assess three-dimensional pore structures at both the soil column (50 mm diameter and 50 mm height) and aggregate scales (diameter 3–5 mm), alongside the evaluation of the soil’s physical and chemical properties. Results showed that the soil organic carbon content (SOC) increased by 44.8% in NPK and 112.5% in NPKOM compared to CK. NPKOM improved the aggregate stability by 51.6%, whereas NPK had no significant effect. At the soil column scale, NPK increased the total porosity by 13.7% but reduced larger pores (>0.06 mm), whereas NPKOM decreased the total porosity by 7.8% and increased larger pores. At the aggregate scale, NPKOM increased the porosity for pores >0.098 mm by 7.6 times compared to CK and 9.5 times compared to NPK. In conclusion, long-term NPKOM significantly enhances the SOC and aggregate stability and promotes larger pore formation, unlike NPK, which mainly increases SOC but does not improve the soil structure.

Food Gels Based on Polysaccharide and Protein: Preparation, Formation Mechanisms, and Delivery of Bioactive Substances

Hydrogels have a unique three-dimensional network that can create a good environment for the loading of functional compounds; hence, they have considerable potential in the delivery of bioactive substances. Natural macromolecular substances (proteins, polysaccharides) have the features of low toxicity, degradability, and biosafety; thus, they can be employed in the manufacture of hydrogels in the food sector. With its customizable viscoelastic and porous structure, hydrogels are believed to be good bioactive material delivery vehicles, which can effectively load polyphenols, vitamins, probiotics, and other active substances to prevent their influence from the external environment, thereby improving its stability. In this research, the common raw materials, preparation methods, and applications in the delivery of bioactive elements of food gels were examined; this study aimed at presenting new ideas for the development and utilization of protein-based food gels.

A Pore-Scale Simulation of the Effect of Heterogeneity on Underground Hydrogen Storage

Using underground hydrogen storage technology has been recognized as an effective way to store hydrogen on a large scale, yet the physical mechanisms of hydrogen flow in porous media remain complex and challenging. Studying the heterogeneity of pore structures is crucial to enhance the efficiency of hydrogen storage. In order to better understand the pore-scale behavior of hydrogen in underground heterogeneous porous structures, this paper investigates the effects of wettability, pore–throat ratio, and pore structure heterogeneity on the behavior of the two-phase H2–brine flow using pore-scale simulations. The results show that the complex interactions between wettability, heterogeneity, and pore geometry play a crucial role in controlling the repulsion pattern. The flow of H2 is more obstructed in the region of the low pore–throat ratio, and the obstructive effect is more obvious when adjacent to the region of the high pore–throat ratio than that when adjacent to the region of the medium pore–throat ratio. In high-pore–throat ratio structures, the interfacial velocity changes abruptly as it passes through a wide pore and adjacent narrower throat. Interfacial velocities at the local pore scale may increase by several orders of magnitude, leading to non-negligible viscous flow effects. It is observed that an increase in the pore–throat ratio from 6.35 (low pore–throat ratio) to 12.12 (medium pore–throat ratio) promotes H2 flow, while an increase from 12.12 (medium pore–throat ratio) to 23.67 (high pore–throat ratio) negatively affects H2 flow. Insights are provided for understanding the role of the heterogeneity of pore structures in H2–brine two-phase flow during underground hydrogen storage.

Deep-Eutectic-Solvent-Decorated Metal–Organic Framework for Food and Environmental Sample Preparation

Deep eutectic solvent (DES) is distinguished by its unique solvent properties, chemical stability, and eco-friendly nature, which are pivotal in a spectrum of chemical processes. It enhances the sample preparation process by increasing efficiency and minimizing the environmental impact. Metal–organic frameworks (MOFs), which are porous structures formed through coordination bonds between metal ions and organic ligands, are defined by their adjustable pore dimensions, extensive surface areas, and customizable architectures. The integration of DES within MOF to create DES@MOF capitalizes on the beneficial attributes of both materials, augmenting MOFs’ stability and versatility while providing a multifunctional carrier for DES. This composite material is both highly stable and readily tunable, establishing it as a leading contender for applications in sample preparation for food and environmental samples. This comprehensive review explores the application of DES-decorated MOF in food and environmental sample preparation and highlights the expansive potential of DES@MOF in diverse fields. We provide a detailed analysis of the characteristics of DES@MOF and its individual components, methods for decorating MOFs with DES, the advantages of these composite materials in sample pretreatment, and their specific applications in food safety and environmental monitoring. DESs are employed to modify MOFs, offering a multitude of benefits that can substantially improve the overall performance and applicability of MOFs. The review also discusses current challenges and future directions in this field, offering valuable insights for further research and development. The synergistic effects of DES and MOFs offer new opportunities for applications in food safety and other areas, leading to the development of more efficient, sensitive, and environmentally friendly analytical methods. This collaboration paves the way for sustainable technologies and innovative solutions to complex challenges.

Effects of Soil Compaction Stress Combined with Drought on Soil Pore Structure, Root System Development, and Maize Growth in Early Stage

Soil compaction is a major environmental stress to root development and plant growth. Meanwhile, drought always results in increasing soil mechanical impedance, which in turn aggravates soil compaction stress. In this study, a column experiment with three levels of compaction stress (low, moderate, and severe) and two levels of soil water content (well-watered and drought,) was established to investigate the effects of soil compaction combined with drought on soil pore structure, root development, and maize growth properties. The results showed that soil compaction combined with soil water stress significantly affected the characteristics of soil pore structure. With the increase in soil compaction, the porosity, larger pores (>500 μm), and maximum pore diameter significantly decreased (p < 0.05) regardless of soil water status. Additionally, both pore morphology and network parameters also deteriorated under soil compaction with drought conditions. Soil compaction substantially affected the root length, root volume, root surface area, and root average diameter in the whole profile (p < 0.05). Compared to well-watered conditions, the effects of soil compaction on root characteristics under drought conditions were more obvious, which indicated that appropriate soil water content could alleviate compaction stress. The aboveground biomass and plant height showed a consistent trend with root traits under soil compaction stress regardless of water status. A Pearson’s correlation analysis showed that there were significant correlations between most soil pore parameters and maize growth traits. In addition, soil compaction showed a significant effect on both stomatal conductance and transpiration rate while soil water showed a significant effect on SPAD (Soil Plant Analysis Development).

Experimental Study on the Efficiency of Fracturing Integrated with Flooding by Slickwater in Tight Sandstone Reservoirs

Tight reservoirs, with their nanoscale pore structures and limited permeability, present significant challenges for oil recovery. Composite fracturing fluids that combine both fracturing and oil recovery capabilities show great potential to address these challenges. This study investigates the performance of a slickwater-based fracturing fluid, combined with a high-efficiency biological oil displacement agent (HE-BIO), which offers both production enhancement and environmental compatibility. Key experiments included tests on single-phase flow, core damage assessments, interfacial tension measurements, and oil recovery evaluations. The results showed that (1) the slickwater fracturing fluid effectively penetrates the rock matrix, enhancing oil recovery while minimizing environmental impact; (2) it causes substantially less damage to the reservoir compared to traditional guar gum fracturing fluid, especially in cores with little higher initial permeability; and that (3) oil recovery improves as HE-BIO concentration increases from 0.5% to 2.5%, with 2.0% as the optimal concentration for maximizing recovery rates. These findings provide a foundation for optimizing fracturing oil displacement fluids in tight sandstone reservoirs, highlighting the potential of the integrated fracturing fluid to enhance sustainable oil recovery.

Preparation and performance study of heparinized multi‐walled carbon nanotube/cellulose acetate hemodialysis membrane

AbstractCurrently, the incidence of kidney failure is increasing worldwide. Hemodialysis is the main method for the treatment of kidney diseases, and the continuous development of new hemodialysis membranes is the key to improve the treatment effect and the quality of life of patients. In this study, heparinized multi‐walled carbon nanotube/cellulose acetate (Hep/MWCNTs@CA) membranes were prepared by non‐solvent induced phase separation (NIPS). The morphology and pore structure of Hep/MWCNTs@CA membranes were characterized by scanning electron microscopy (SEM). The elongation at break and tensile strength of the membranes were characterized by a mechanical property universal tester. The results showed that mechanical properties of 0.1 wt% MWCNTs enhanced the membrane is best. The water contact angle test confirmed that MWCNTs can improve the membrane hydrophilicity, and combined with the adsorption test results for proteins, it was found that the hydrophilicity can reduce the adsorption of proteins to the composite membrane and improve the blood compatibility of the material. The dialysis performance of urea and lysozyme was tested by a self‐made simulated hemodialysis device, and the clearance rates of urea and lysozyme were 84% and 47.2%, respectively, which showed that the interfacial gap between MWCNTs and CA matrix can make the composite membrane retain a high retention rate of macromolecular proteins (92.3%) and further improved the clearance rate of small and medium molecular toxins. In addition, the good blood compatibility and biocompatible properties of the materials were confirmed by hemolysis, recalcification and cytotoxicity tests on Hep/MWCNTs@CA membranes. In conclusion, the prepared Hep/MWCNTs@CA holds great potential for application in the field of hemodialysis.

Comparison of Different Additives and Ages on Mechanical and Acoustic Behavior of Coal Gangue Cemented Composite

Cemented backfill represents a significant trend in mine filling methods; however, it often exhibits high brittleness and limited resistance to failure, which can restrict its practical application. This study investigates the mechanical properties and damage evolution of fiber-reinforced coal gangue cemented materials (CGCMs) at various curing times using uniaxial compressive tests, acoustic emission (AE) analysis, and scanning electron microscopy (SEM). Specimens were created with different fillers, including carbon fibers (CFs), steel fibers (SFs), and carbon black (CB), and subjected to uniaxial compression until failure. Control specimens without fillers were also tested for comparison. The microstructure of the specimens was examined using scanning electron microscopy (SEM). The findings indicate that (1) the compressive strength of filler-reinforced CGCMs increases between 7 and 14 days of curing but decreases thereafter, with CB significantly improving early-age strength; (2) specimens reinforced with CFs and SFs exhibit significantly enhanced toughness in their post-cracking response; (3) AE events during specific stages can effectively identify the reinforcing effects of CFs and SFs; (4) the presence of fillers improves resistance to shear cracks, with CFs and SFs being more effective than CB; and (5) adding CB results in a denser and more stable hydration product structure, while CFs and SFs lead to a more porous structure with increased cracking.

Multifunctional Electromagnetic Responsive Porous Materials Synthesized by Freeze Casting: Principles, Progress, and Prospects

AbstractFreeze casting is a solidification technique utilized in the fabrication of porous materials. However, the freeze casting process is quite complex, and significant challenges remain in precisely controlling the pore size and shape of porous structures. This study aims to investigate the customization of multifunctional electromagnetic wave (EMW) absorbers with 3D porous structures via freeze casting. This review initially presents the fundamental principles underlying the freeze casting technique and examines the correlation between internal and external factors during the preparation process and porosity. The emerging trends in constructing novel and intricate macroscopic structures through freeze casting are subsequently outlined. Furthermore, this review focuses on the fabrication of composites with various porous microstructures through freeze casting of low‐dimensional building blocks, and their EMW response and multifunctional properties. By regulating the internal and external influencing mechanisms of freeze casting, porous EMW absorption materials exhibit outstanding advantages such as electromagnetic property manipulation, controllable structure, high porosity, high specific surface area, lightweight, and flexibility. These features broaden their applications in electromagnetic shielding, mechanical property, radar stealth, thermal insulation and fire prevention, flexible sensors, antifreeze ability, etc. In addition, we discuss the challenges and prospects of high‐performance EMW absorbers using freeze casting techniques.

Effect of Synthesis Temperature on Performance of Phenazine-Based Cathode for Sodium Dual-Ion Batteries.

Organic materials have attracted much attention in the field of electrochemical energy storage due to their ecological sustainability, abundant resources and structural designability. However, low electrical conductivity and severe agglomeration of organic materials lead to poor discharge capacity and reaction kinetics in batteries. Herein, the morphology of the phenazine-based organic polymer poly(5,10-diphenylphenazine) (PDPPZ) was modified by varying the synthesis temperature. PDPPZ-165 °C with an exceptional porous structure provides abundant reaction channels for rapid charge transfer and diffusion that improves the reaction kinetics in sodium dual-ion batteries. Therefore, PDPPZ-165 °C cathode possesses excellent rapid charge-discharge capability delivering a specific capacity of 119.2 mAh g-1 at 40 C. Furthermore, a high specific capacity of 124.7 mAh g-1 can be provided even at a high loading of 16 mg cm-2 at 0.5 C with a capacity retention of 86.4 % after 500 cycles. This work could afford new insights for optimizing the performance of organic cathode materials in sodium dual-ion batteries.

Fabrication of Mesoporous SiO<sub>2</sub> Shells for Dye Adsorption Studies

The present work focuses on the fabrication of novel hybrid materials for toxic dye removal from an aqueous environment. Nanocarbon template (20-30 nm) was coated with tri-ethyl-orthosilicate (TEOS). The core-shell structure developed was further air pyrolyzed at 600 °C to produce mesoporous silica shells. The pore structures and characteristics of the material were evaluated using XRD, nitrogen adsorption studies, SEM, and TEM. Owing to the hierarchical porosity in range of 1-4 nm and 10-20 nm their adsorption studies were investigated for Phenol-Red. Dye adsorption studies performed revealed 98% removal efficiency with only 20 mg of adsorbent dose within 15 minutes.

Mullite Synthesis Using Porous 3D Structures Consisting of Nanofibrils of Aluminum Oxyhydroxide Chemically Modified with Ethoxysilanes

Nanocrystalline mullite was synthetized by annealing a highly porous 3D structure consisting of nanofibrous aluminum oxyhydroxides treated with ethoxysilanes. The chemical, structural, and phase transformations in the aluminosilicate nanosystem were studied in the temperature range between 100 and 1600 °C. The features of the solid-phase synthesis of mullite at the interface of crystalline alumina with a liquid silica layer are discussed. It was established that chemical modification of the alumina surface with ethoxysilanes significantly limits the interphase mass transport and delays the phase transformation of the amorphous oxide into γ-Al2O3, which begins at temperatures above 1000 °C, while the basic structural nanofibrils are already crystallized at ~850 °C. The formation of mullite was completed at temperatures ≥ 1200 °C, where the fraction of γ-Al2O3 sharply decreased.

Double Carbon‐Species Coated Porous Silicon Anode Induced by Interfacial Energy Reduction for Lithium‐Ion Batteries

The rapid development of electric vehicles necessitates high‐energy density Li‐ion batteries for extended range. Silicon is a promising alternative to graphite anodes due to its high capacity; however, its substantial volume expansion during cycling leads to continuous growth of the solid electrolyte interphase and significant capacity fading. This study addresses these issues by designing a porous Si structure combined with a double carbon‐species coating layer, induced by low interfacial energy in a scalable process. Carbon and graphene are located on Si surfaces, forming a close interface that maintains electrical contact, suppresses lithium consumption, and enhances charge transfer properties. The composite anode with a double carbon‐species coating on Si demonstrates rapid stabilization with increasing coulombic efficiency, achieving a specific capacity of 1,814 mAh g–1 at 0.2 C and a high‐rate capability of 1,356 mAh g–1 at 10C. Additionally, in a full‐cell configuration with LiFePO4, it recorded a specific capacity of 161 mAh g–1 at 0.2 C. These results show the potential of porous Si with a carbon‐graphene coating for stable, high‐capacity operation in Li‐ion batteries, offering new insights into high‐performance electrochemical systems. Moreover, the double carbon‐species coating derived from a scalable surface chemistry‐based process presents a realistic alternative for industrial applications.

Inverse Identification of Constituent Elastic Parameters of Ceramic Matrix Composites Based on Macro–Micro Combined Finite Element Model

Accurate material performance parameters are the prerequisite for conducting composite material structural analysis and design. However, the complex multiscale structure of ceramic matrix composites (CMCs) makes it extremely difficult to accurately obtain their mechanical performance parameters. To address this issue, a CMC micro-scale constituents (fiber bundles and matrix) elastic parameter inversion method was proposed based on the integration of macro–micro finite element models. This model was established based on the μCT scan data of a plain-woven CMC tensile specimen using the chemical vapor infiltration (CVI) process, which could reflect the real microstructure and surface morphology characteristics of the material. A BP neural network was used to predict the multiscale stiffness, considering the influence of the porous structure on the macroscopic stiffness of the material. The inversion process of the constituent elastic parameters was established using the trust-region algorithm combined with an improved error function. The inversion results showed that this method could accurately invert the CMC constituent elastic parameters with excellent robustness and anti-noise performance. Under four different degrees of deviation in the initial iteration conditions, the inversion error of all parameters was within 1%, and the maximum inversion error was only 2.16% under a 10% high noise level.

Controlling the Polarity of Metal–Organic Frameworks to Promote Electrochemical CO2 Reduction

AbstractThe addition of polar functional groups to porous structures is an effective strategy for increasing the ability of metal–organic frameworks (MOFs) to capture CO2 by enhancing interactions between the dipoles of the polar functional groups and the quadrupoles of CO2. However, the potential of MOFs with polar functional groups to activate CO2 has not been investigated in the context of CO2 electrolysis. In this study, we report a mixed‐ligand strategy to incorporate various functional groups in the MOFs. We found that substituents with strong polarity led to increased catalytic performance of electrochemical CO2 reduction for these polarized MOFs. Both experimental and theoretical evidence indicates that the presence of polar functional groups induces a charge redistribution in the micropores of MOFs. We have shown that higher electron densities of sp2‐carbon atoms in benzimidazolate ligands reduces the energy barrier to generate *COOH, which is simultaneously controlled by the mass transfer of CO2. Our research offers an effective method of disrupting local electron neutrality in the pores of electrocatalysts/supports to activate CO2 under electrochemical conditions.

Tailoring of the Properties of Amorphous Mesoporous Titanosilicates Active in Acetone Condensation

Amorphous mesoporous materials are promising as catalysts for processes involving or forming bulk molecules. In a reaction such as acetone condensation to form mesitylene, an effective catalyst should not only have a developed porous structure but also have active centers of acidic and basic types. The sol–gel approach allows one to obtain titanosilicates with such characteristics. This work demonstrates the possibility of controlling their properties by varying the conditions for the synthesis of titanosilicate gels. It has been established that controlling hydrolysis allows one to increase the activity of amorphous mesoporous titanosilicates by 10 times: from acetone conversion of 6% to 60%. It has been shown that the use of titanium acetylacetonate complexes in the synthesis of gels leads to an increase in the content of tetracoordinated Ti in the structure and contributes to an increase in the acidity of titanosilicates. During the condensation of acetone on the obtained mesoporous titanosilicates, high acetone conversion (60–79%) and mesitylene selectivity of up to 83% were achieved.

Phytic Acid Functionalized Hierarchical Porous Metal‐Organic Framework Microspheres for Efficient Extraction of Uranium from Seawater

AbstractUranium is a critical resource in the development of nuclear energy, and its extraction from natural seawater has been identified as a potential solution to address uranium resource shortages. In this study, hierarchical meso‐/micro‐ porous metal‐organic framework functionalized with phytic acid (PA) microspheres (denoted H‐UiO‐66‐PA) are rationally synthesized for efficient uranium extraction. This unique design allowed for a large adsorption capacity and fast adsorption kinetics, making it a promising material for uranium extraction. Due to the hierarchically porous structure, H‐UiO‐66‐NH2 materials not only provide more sites for grafting PA, and thus enhance the adsorption capacity, but also facilitate the rapid diffusion of uranyl ions which can quickly and effectively access the interior of the H‐UiO‐66‐PA adsorbent. Therefore, the obtained H‐UiO‐66‐PA can achieve an impressive absorption efficiency of 6.76 mg g−1 in actual seawater within 15 days. Meanwhile, the H‐UiO‐66‐PA possesses a good adsorption capacity for uranyl ions in the five adsorption/desorption cycles. This work proposes a feasible strategy for constructing functional hierarchical porous MOFs for uranium removal.