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34 pages, 13993 KiB  
Article
Multi-Scale Pore Structure of Terrestrial, Transitional, and Marine Shales from China: Insights into Porosity Evolution with Increasing Thermal Maturity
by Zhongrui Wu, Ralf Littke, Shuo Qin, Yahao Huang, Sheng He, Gangyi Zhai, Zhengqing Huang and Kaiming Wang
J. Mar. Sci. Eng. 2025, 13(3), 609; https://doi.org/10.3390/jmse13030609 - 19 Mar 2025
Cited by 2 | Viewed by 493
Abstract
Organic matter (OM)-hosted pores play a crucial role in unconventional shale reservoirs, with their development influenced by OM type and thermal maturity across terrestrial, transitional, and marine deposits. In this study, a comparative analysis of porosity and pore structures is presented using organic [...] Read more.
Organic matter (OM)-hosted pores play a crucial role in unconventional shale reservoirs, with their development influenced by OM type and thermal maturity across terrestrial, transitional, and marine deposits. In this study, a comparative analysis of porosity and pore structures is presented using organic petrographical, petrophysical, and mineralogical methods on organic-rich samples from diverse depositional environments. A pore evolution model for these sediments in different settings is proposed. Results show that kerogen particles in terrestrial shales at low and moderate thermal maturity (Dameigou Formation and Qingshankou Formation) are mostly nonporous. Transitional shales (Longtan Formation) contain vitrinite and inertinite, with only some inertinite exhibiting visible primary pores. In marine shales at higher maturity (late oil window; Dalong Formation), the interparticle pore space is occupied by solid bitumen, and secondary porosity is present at higher maturity, approaching the thermal gas generation stage. In over-mature marine shales (Wujiaping and Daye Formations), secondary pores are densely distributed within pyrobitumen. A negative correlation between organic carbon content and pore volume is observed in low-maturity lacustrine and transitional shales due to poorly developed kerogen-bound pores and interparticle pore occlusion by solid bitumen. However, over-mature marine shales exhibit a strong positive correlation due to extensive secondary porosity in pyrobitumen. Thus, pore evolution within OM is controlled by kerogen type and maturity. In oil-prone marine and lacustrine shales, secondary porosity in solid bitumen and pyrobitumen increases with thermal maturity. In contrast, terrestrial kerogen rarely forms solid bitumen and mainly develops micropores rather than mesopores at high maturity. Full article
(This article belongs to the Section Marine Energy)
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18 pages, 3191 KiB  
Article
Material Characterization and Technological Properties of Biocompatible Ti-12Al-42Nb Spherical Powder Alloy for Additive Manufacturing of Personal Medical Implants
by Alexander Anokhin, Andrey Kirsankin, Elena Kukueva, Alexander Luk’yanov, Maria Chuvikina, Elena Ermakova, Svetlana Strelnikova and Stepan Kupreenko
Metals 2025, 15(2), 147; https://doi.org/10.3390/met15020147 - 31 Jan 2025
Viewed by 970
Abstract
The paper focuses on material characterization and technology properties of a new Ti-12Al-42Nb spherical powder alloy for additive manufacturing of personal medical implants. The electrode induction melting inert gas atomization (EIGA) method was used to produce the powder alloy. The powder sphericity coefficient [...] Read more.
The paper focuses on material characterization and technology properties of a new Ti-12Al-42Nb spherical powder alloy for additive manufacturing of personal medical implants. The electrode induction melting inert gas atomization (EIGA) method was used to produce the powder alloy. The powder sphericity coefficient (PSC) was 1.02. Image J software was used to calculate the spherical degree by processing images sets from scanning electron microscopy (SEM) and optical microscopy (OM). SEM of particles cross-sections indicated internal thermal-induced porosity (TIP) with a 2.3 μm pore diameter. Particle size distribution was in the range from 15.72 μm (d10) to 64.48 μm (d100) as measured by laser particle analyzer. It was indicated that flowability and powder bulk density were 196 sec and 2.79 g/cm3, respectively. XRD analysis confirmed the beta phase of the powder alloy with no additional phases. X-ray fluorescence spectrometry confirmed the alloyed composition. Reducing and oxidative melting methods of analysis showed a slight amount of impurities: oxygen (0.0087 wt.%), nitrogen (0.03 wt.%), hydrogen (0.0012 wt.%), sulfur (0.0016 wt.%), and carbon (0.022 wt.%). Simultaneous thermal analysis (STA) was performed to indicate weight growth and losses and thermal effects in argon, nitrogen, and air as well as the oxidation of Al2O3, TiO2, and Nb2O5 on the surface layer of Ti-12Al-42Nb powder alloy particles. Different phase transformations of γAl2O3  θAl2O3  αAl2O3 and TiO2 rutile TiO2 anatase phase transformation were detected by STA in the oxidative layer. Full article
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16 pages, 5266 KiB  
Article
Ultra-Performance Liquid Chromatography-Quadrupole-Time-of-Flight-Mass Spectrometry-Based Analysis of Facial Physiological Parameters and Lipid Composition of Between Sensitive Skin of Women Aged 36–42 and 43–49 Year
by Yu Li, Rong Tang, Lizhi Yue and Congfen He
Life 2025, 15(2), 175; https://doi.org/10.3390/life15020175 - 25 Jan 2025
Viewed by 898
Abstract
Background: UPLC-Q-TOF-MS (Ultra-Performance Liquid Chromatography–Quadrupole Time-of-Flight Mass Spectrometry) is a high-precision, high-density technology for lipid analysis. Sensitive skin is a sub-stable condition, and it has been reported that the population of sensitive skin in China is predominantly female. Meanwhile, women with sensitive skin [...] Read more.
Background: UPLC-Q-TOF-MS (Ultra-Performance Liquid Chromatography–Quadrupole Time-of-Flight Mass Spectrometry) is a high-precision, high-density technology for lipid analysis. Sensitive skin is a sub-stable condition, and it has been reported that the population of sensitive skin in China is predominantly female. Meanwhile, women with sensitive skin have different physiological parameters as well as lipid compositions at different ages. The Yellow Emperor’s Classic of Internal Medicine states that the number of women’s life cycles is seven, that major changes are manifested every 7 years, and that aging begins at age 35. At present, the correlation between facial lipid composition and aging indicators of sensitive skin in women aged 36–42 and 43–49 years has not been reported. Objective: This study reveals the relationship between key lipid composition of the facial skin and the aging of sensitive skin in women aged 36–42 and 43–49 years. Methods: We used UPLC-Q-TOF-MS technology to study the changes in lipid composition in the sensitive skin of woman aged 36–42 and 43–49 years, using a multi-probe adapter system with different types of skin-testing probes to test physiological parameters. Three types of multivariate data—questionnaires, physiological indicators, and lipid composition—were used together to assess differences in aging in a population of women with sensitive skin at different ages. Results: 1. In the questionnaire part, the T1 group was more susceptible to sunburn and the T2 group was more susceptible to tanning. 2. In the physiological index part, the aging characteristics of facial skin in the T2 group were obvious, with the b-value, as well as the brown area size, being significantly higher than the T1 group, while the TWEL, sebum, R2 value, ITA value, pore count, and concentration of the red area were significantly lower than the T1 group. 3. In the lipid part, the total facial lipid content was higher in the T2 group, with a significantly higher GP lipid, and the 47 VIP lipids obtained were analyzed by ROC curves, narrowing down to six lipids, PS(2-OMe-21:0/0:0), PS(O-18:0/20:5 (5Z,8Z,11Z,14Z,17Z)), PA(O-16:0/20:5 (5Z,8Z,11Z,14Z,17Z)), PS (P-16:0/12:0, PA (O-16:0/22:2 (13Z,16Z)), and PC (19:3 (10Z,13Z,16Z)/0:0)), and all six lipids were higher in the T2 group. 4. In Spearman correlation analysis, PS(O-18:0/20:5(5Z,8Z,11Z,14Z,17Z)), PS(P-16:0/12:0), PS(2-OMe-21:0/0:0), PA(O-16:0/20:5(5Z,8Z,11Z,14Z,17Z)), and PC(19:3( 10Z,13Z,16Z)/0:0), which are five lipids and skin aging indicators (TWEL, sebum, ITA value, b-value, pore count, concentration of red area, and brown area size) were significantly correlated. Conclusions: Through correlation analysis, it was found that changes in the composition of skin surface lipids (SSLs) in both age groups have an important influence on facial physiological indicators (aging manifestations) and played an important role in furthering the understanding of sensitive skin aging. Therefore, these lipid components also provide theoretical support for the development of cosmetic ingredients that slow down the aging of sensitive skin. Full article
(This article belongs to the Section Physiology and Pathology)
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16 pages, 6667 KiB  
Article
Nanoscale Pore Evolution of Terrestrial Shale with Thermal Maturation Level Increase Induced by Hydrous Pyrolysis
by Haiyan Hu, Wangpeng Li, Yifan Yang and Shuai Chen
Processes 2025, 13(1), 246; https://doi.org/10.3390/pr13010246 - 16 Jan 2025
Cited by 1 | Viewed by 836
Abstract
A series of terrestrial shale samples with different thermal maturities were subjected to hydrous artificial pyrolysis to study the evolution of terrestrial shale pores. The original shale was obtained from the terrestrial interval of a core sample, the total organic carbon (TOC) content [...] Read more.
A series of terrestrial shale samples with different thermal maturities were subjected to hydrous artificial pyrolysis to study the evolution of terrestrial shale pores. The original shale was obtained from the terrestrial interval of a core sample, the total organic carbon (TOC) content was 8.34 wt%, and the vitrinite reflectance (Ro) was 5.31%. The original shale core was cut into eight parts, which were heated at temperatures of 300, 350, 400, 420, 450, 500, 550, and 600 °C to obtain samples with different thermal maturities. The pore size distribution (PSD), pore volume (PV), specific surface area (SSA), and pore types were investigated via CO2 and N2 adsorption tests and field emission scanning electron microscopy (FE-SEM). Many organic matter (OM) pores and mineral pores were observed via FE-SEM with increasing thermal maturity. The total PV and SSA increased until the sample reached 500 °C and then decreased, and the mesopore volume followed this trend. The micropore volume first decreased, increased until the sample reached 500 °C, and then decreased; the macropore volume increased to a peak in the sample pyrolyzed at 420 °C and then remained stable. Pores with sizes ranging from 10 to 30 nm were the predominant contributors to the shale pore volume. The SSA was affected by pores with diameters less than 20 nm, which accounted for approximately 54% of the SSA. The rate of OM conversion influenced pore creation. Full article
(This article belongs to the Special Issue Advances in Enhancing Unconventional Oil/Gas Recovery, 2nd Edition)
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21 pages, 5790 KiB  
Article
Sealing Effects on Organic Pore Development in Marine Shale Gas: New Insights from Macro- to Micro-Scale Analyses
by Qiumei Zhou, Hao Xu, Wen Zhou, Xin Zhao, Ruiyin Liu and Ke Jiang
Energies 2025, 18(1), 193; https://doi.org/10.3390/en18010193 - 5 Jan 2025
Cited by 1 | Viewed by 789
Abstract
The physics of how organic pores change under high thermal evolution conditions in overmature marine shale gas formations remains unclear. In this study, systematic analyses at the macro- to micro-scales were performed to reveal the effects of the sealing capacity on organic pore [...] Read more.
The physics of how organic pores change under high thermal evolution conditions in overmature marine shale gas formations remains unclear. In this study, systematic analyses at the macro- to micro-scales were performed to reveal the effects of the sealing capacity on organic pore development. Pyrolysis experiments were conducted in semi-closed and open systems which provided solid evidence demonstrating the importance of the sealing capacity. Low-maturity marine shale samples from the Dalong Formation were used in the pyrolysis experiments, which were conducted at 350 °C, 400 °C, 450 °C, 500 °C, 550 °C, and 600 °C. The pore characteristics and geochemical parameters of the samples were examined after each thermal simulation stage. The results showed that the TOC of the semi-closed system decreased gradually, while the TOC of the open system decreased sharply at 350 °C and exhibited almost no change thereafter. The maximum porosity, specific surface area, and pore volume of the semi-closed system (10.35%, 2.99 m2/g, and 0.0153 cm3/g) were larger than those of the open system (3.87%, 1.97 m2/g, and 0.0059 cm3/g). In addition, when the temperature was 600 °C, the pore diameter distribution in the open system was 0.001–0.1 μm, while the pore diameter distribution in the semi-closed system was 0.001–10 μm. The pore volumes of the macropores and mesopores in the semi-closed system remained larger than those in the open system. The pore volumes of the micropores in the semi-closed and open systems were similar. The pyrolysis results indicated that (1) the pressure difference caused by the sealing capacity controls organic pore development; (2) organic pores developed in the semi-closed system, and the differences between the two systems mainly occurred in the overmature stage; and (3) the differences were caused by changes in the macropore and mesopore volumes, not the micropore volume. It was concluded that the sealing capacity is the key factor for gas pore generation in the overmature stage of marine shale gas reservoirs when the organic matter (OM) type, volume, and thermal evolution degree are all similar. The macropores and mesopores are easily affected by the sealing conditions, but the micropores are not. Finally, the pyrolysis simulation results were validated with the Longmaxi shale and Qiongzhusi shale properties. The Longmaxi shale is similar to semi-closed system, and the Qiongzhusi shale is similar to open system. Two thermal evolution patterns of organic pore development were proposed based on the pyrolysis results. This study provides new insights into the evolution patterns of organic pores in marine shale gas reservoirs. Full article
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20 pages, 11238 KiB  
Article
Analysis of Nanostructures and Wettability of Marine Shale in Southern China, Based on Different Fractal Models
by Yang Wang, Baoyuan Zhong, Yunsheng Zhang, Yanming Zhu and Meng Wang
Fractal Fract. 2025, 9(1), 12; https://doi.org/10.3390/fractalfract9010012 - 29 Dec 2024
Cited by 2 | Viewed by 896
Abstract
The wetting behavior of shale oil and gas on shale surfaces is determined by the interplay of organic matter (OM), mineral composition, and the intricate pore network structure of the shale. In this paper, the sensitivity responses of the Frenkel–Halsey–Hill (FHH), Neimark (NM), [...] Read more.
The wetting behavior of shale oil and gas on shale surfaces is determined by the interplay of organic matter (OM), mineral composition, and the intricate pore network structure of the shale. In this paper, the sensitivity responses of the Frenkel–Halsey–Hill (FHH), Neimark (NM), and Wang–Li (WL) fractal models to marine shale with varying material components are analyzed, based on liquid nitrogen adsorption experiments and fractal theory. The wettability evolution model of shale with different maturity stages is established to reveal the heterogeneity characteristics of wettability in shale with complex pore structures. Results show that the NM and WL models offer distinct advantages in evaluating the reservoir structure of shale oil and gas resources. The existence of large-diameter pores is conducive to the homogeneous development of the pore structure. The coupling relationship between pore volume, pore size and pore specific surface affects the fractal characteristics of the pore structure. For highly overmature shale, with an increase in fractal dimension, the wettability of shale changes from neutral-wet to water-wet. For ultramature shale, the higher heterogeneity of the pore structure leads to larger contact angles, causing the wettability to transition gradually from water-wet to oil-wet. In addition, the sensitivity analysis of wettability to fractal structure parameters is examined from the perspective of OM maturation and evolution. Full article
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16 pages, 7632 KiB  
Article
The Control of Isolated Kerogen on Pore Structure and Heterogeneity in Marine-Continental Transitional Shale: A Case Study on the Taiyuan Formation, Northern Ordos Basin
by Zhengxi Gao, Ke Miao, Yushan Zuo, Fuhua Shang, Shuang Gao, Wentian Mi, Yuan Gao, Qing Li and Haidong Li
Processes 2024, 12(11), 2395; https://doi.org/10.3390/pr12112395 - 30 Oct 2024
Viewed by 1032
Abstract
Accurately determining the pore structure and heterogeneity characteristics of marine-continental transitional shale in the Taiyuan Formation is crucial for evaluating the shale gas resources in the northern Ordos Basin. However, the studies on pore characteristics and heterogeneity of marine-continental transitional shales and isolated [...] Read more.
Accurately determining the pore structure and heterogeneity characteristics of marine-continental transitional shale in the Taiyuan Formation is crucial for evaluating the shale gas resources in the northern Ordos Basin. However, the studies on pore characteristics and heterogeneity of marine-continental transitional shales and isolated kerogen are limited. This study collected Taiyuan Formation shale in the northern Ordos Basin, and corresponding kerogen isolated from shale and used N2 and CO2 adsorption experiment and Frenkel–Halsey–Hill and Volume-Specific Surface Area model to investigate the pore structure and heterogeneity of both. The results show that the isolated kerogen is dominated by micropores, and the micropore’s specific surface area and volume are 4.7 and 3.5 times the corresponding shale, respectively. In addition, the microporous heterogeneity of the isolated kerogen is stronger than that of shale, while the mesoporous heterogeneity is exactly the opposite. Meanwhile, the micropores fractal dimension Dm is positively correlated with organic matter (OM) content, while mesopores fractal dimension D1 and D2 are negatively linearly correlated with TOC content and have no significant relationship with clay mineral and quartz content (but show a significant positive correlation with illite and illite/smectite mixed layer). Isolated kerogen plays an important role in the pore (especially micropores) heterogeneity of shale, while other minerals (such as clay minerals) have a controlling effect on the mesopores heterogeneity of shale. Compared with marine shale, the marine-continental transitional shale of the Taiyuan Formation has a lower fractal dimension and better connectivity, which is conducive to shale gas seepage and migration. The final result can provide a significant basis for the reserve evaluation and the optimization of desert areas in the marine-continental transitional shale gas in the northern Ordos Basin. Full article
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83 pages, 5867 KiB  
Review
Fouling of Reverse Osmosis (RO) and Nanofiltration (NF) Membranes by Low Molecular Weight Organic Compounds (LMWOCs), Part 1: Fundamentals and Mechanism
by Yasushi Maeda
Membranes 2024, 14(10), 221; https://doi.org/10.3390/membranes14100221 - 17 Oct 2024
Cited by 6 | Viewed by 6229
Abstract
Reverse osmosis (RO) and nanofiltration (NF) are ubiquitous technologies in modern water treatment, finding applications across various sectors. However, the availability of high-quality water suitable for RO/NF feed is diminishing due to droughts caused by global warming, increasing demand, and water pollution. As [...] Read more.
Reverse osmosis (RO) and nanofiltration (NF) are ubiquitous technologies in modern water treatment, finding applications across various sectors. However, the availability of high-quality water suitable for RO/NF feed is diminishing due to droughts caused by global warming, increasing demand, and water pollution. As concerns grow over the depletion of precious freshwater resources, a global movement is gaining momentum to utilize previously overlooked or challenging water sources, collectively known as “marginal water”. Fouling is a serious concern when treating marginal water. In RO/NF, biofouling, organic and colloidal fouling, and scaling are particularly problematic. Of these, organic fouling, along with biofouling, has been considered difficult to manage. The major organic foulants studied are natural organic matter (NOM) for surface water and groundwater and effluent organic matter (EfOM) for municipal wastewater reuse. Polymeric substances such as sodium alginate, humic acid, and proteins have been used as model substances of EfOM. Fouling by low molecular weight organic compounds (LMWOCs) such as surfactants, phenolics, and plasticizers is known, but there have been few comprehensive reports. This review aims to shed light on fouling behavior by LMWOCs and its mechanism. LMWOC foulants reported so far are summarized, and the role of LMWOCs is also outlined for other polymeric membranes, e.g., UF, gas separation membranes, etc. Regarding the mechanism of fouling, it is explained that the fouling is caused by the strong interaction between LMWOC and the membrane, which causes the water permeation to be hindered by LMWOCs adsorbed on the membrane surface (surface fouling) and sorbed inside the membrane pores (internal fouling). Adsorption amounts and flow loss caused by the LMWOC fouling were well correlated with the octanol-water partition coefficient (log P). In part 2, countermeasures to solve this problem and applications using the LMWOCs will be outlined. Full article
(This article belongs to the Collection Featured Reviews in Membrane Science)
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18 pages, 32054 KiB  
Article
Study on the Process of Preparing Aluminum Foam Sandwich Panel Precursor by Friction Stir Welding
by Yu Zhang and Qiu Pang
Materials 2024, 17(20), 4981; https://doi.org/10.3390/ma17204981 - 11 Oct 2024
Cited by 1 | Viewed by 975
Abstract
In recent years, high-performance lightweight and multifunctional aluminum foam sandwiches (AFSs) can be successfully applied to spacecraft, automobiles, and high-speed trains. Friction stir welding (FSW) has been proposed as a new method for the preparation of AFS precursors in order to improve the [...] Read more.
In recent years, high-performance lightweight and multifunctional aluminum foam sandwiches (AFSs) can be successfully applied to spacecraft, automobiles, and high-speed trains. Friction stir welding (FSW) has been proposed as a new method for the preparation of AFS precursors in order to improve the cost-effectiveness and productivity of the preparation of AFS. In this study, the AFS precursors were prepared using the FSW process. The distribution of foaming agents in the AFS precursors and the structure and morphology of AFS were observed using optical microscopy (OM), scanning electron microscopy (SEM), and X-ray energy dispersive spectroscopy (EDS). The effects of the temperature and material flow on the distribution of the foaming agent during the FSW process were analyzed through experimental study and numerical simulation using ANSYS Fluent 19.0 software. The results show that the uniform distribution of the foaming agent in the matrix and excellent densification of AFS precursor can be prepared when the rotation speed is 1500 r/min, the travel speed is 25 mm/min, the tool plunge depth is 0.2 mm, and the tool moves along the retreating side (RS). In addition, the experimental and numerical simulations show that increasing the welding temperature improves the uniformity of foaming agent distribution and the area of AFS precursor prepared by single welding, shortening the thread length inhibits the foaming agent from reaching the upper sandwich plate and moving along the RS leads to a more uniform distribution of the foaming agent. Finally, the AFS with porosity of 74.55%, roundness of 0.97, and average pore diameter of 1.192 mm is prepared. Full article
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19 pages, 7766 KiB  
Article
Pore Space Characteristics and Migration Changes in Hydrocarbons in Shale Reservoir
by Yiqian Qu, Siqi Ouyang, Jianwen Gao, Jian Shi, Yiying Wu, Yuting Cheng, Zhen Zhou, Zhou Lyu, Wei Sun and Hanning Wu
Fractal Fract. 2024, 8(10), 588; https://doi.org/10.3390/fractalfract8100588 - 4 Oct 2024
Cited by 6 | Viewed by 1604
Abstract
The pore structure and mineral characteristics affect the accumulation and migration of hydrocarbons in shale, which determines the production capacity of shale oil. In this study, shale samples from the Chang 7 member of the Ordos Basin in China were selected to investigate [...] Read more.
The pore structure and mineral characteristics affect the accumulation and migration of hydrocarbons in shale, which determines the production capacity of shale oil. In this study, shale samples from the Chang 7 member of the Ordos Basin in China were selected to investigate the pore space characteristics, the effect of hydrocarbon accumulation on pore heterogeneity, and the hydrocarbon migration changes based on fractal theory, and a series of experiments were conducted involving X-ray diffraction (XRD), total organic carbon (TOC), Soxhlet extraction, and low-temperature nitrogen (N2) and carbon dioxide (CO2) adsorption. Then, the factors affecting extraction efficiency in shale pores were discussed. The interparticle pores contributed most to the accumulation of shale oil, and the organic matter (OM) pores contributed positively to the adsorption of hydrocarbons. The accumulation of hydrocarbons in the pore space did not increase the heterogeneity of the shale pore structure. The contents, states, and positions of hydrocarbons changed during the extraction process. Hydrocarbons were redistributed on the pore surface after Soxhlet extraction, and the heterogeneity of hydrocarbon adsorption and pore surface roughness were improved. Some heavy hydrocarbons and adsorbed components were pyrolyzed, resulting in the gradual escape of the adsorbed layer in the large pores. However, the free oil in the small pores diffused to the large pores and reaggregated on the surface, restoring a stable adsorption layer. The extraction rate was closely related to the pore throat structure and the wettability of mineral surfaces. The configuration between pores and throats had a crucial influence on the extraction rate. A high proportion of meso-pores, which effectively connect micro- and macro-pores, had a higher diffusion efficiency and a higher extraction rate. The OM pores with high energy adsorption were located in the micro-pores, and the shale oil existed in a dissolved state with high mobile capacity. The wettability of mineral surfaces affected the adsorption behavior during extraction, and strong oil wetting promoted hydrocarbon re-adsorption in clay minerals, so that the volume of micro-pores was smaller after extraction. Full article
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27 pages, 6545 KiB  
Article
Compositional and Microstructural Investigations of Prehistoric Ceramics from Southern Romania (Middle Neolithic Pottery)
by Rodica-Mariana Ion, Ancuta-Elena Pungoi, Lorena Iancu, Ramona Marina Grigorescu, Gabriel Vasilievici, Anca Irina Gheboianu, Sofia Slamnoiu-Teodorescu and Elvira Alexandrescu
Appl. Sci. 2024, 14(13), 5755; https://doi.org/10.3390/app14135755 - 1 Jul 2024
Cited by 1 | Viewed by 2282
Abstract
In this paper, based on our previous expertise on ceramic artifacts, several archaeometric methods applied to some samples collected from the Dudești archaeological site (Oltenia region, Romania) are reported for the first time in the literature. The chemical composition, and microstructural and morphological [...] Read more.
In this paper, based on our previous expertise on ceramic artifacts, several archaeometric methods applied to some samples collected from the Dudești archaeological site (Oltenia region, Romania) are reported for the first time in the literature. The chemical composition, and microstructural and morphological characterization of these samples offer important conclusions about the processing conditions. Some specific techniques such as X-ray diffraction (XRD), wavelength-dispersive X-ray fluorescence (WDXRF), optical microscopy (OM), stereomicroscopy, environmental scanning electron microscopy (ESEM), Fourier-transform infrared spectroscopy (FTIR), and Raman spectroscopy provide compositional information about composition and the decay processes. Additionally, the Brunauer–Emmett–Teller (BET) method helps to estimate pore sizes and specific surface areas. A thermogravimetric analysis (TGA/TDG) was used to establish details regarding the production technology and also the raw materials source used to make the ceramics. The obtained results indicated that the ceramics are based on a paste of muscovite and feldspar, with high plasticity, together with quartz and hematite/goethite and calcite, the latter in very low concentrations. According to the obtained results, we could assume that clays from the investigated samples had a low concentration of calcium. Gypsum is present as paste in a very low concentration, identified by the presence of a sulphate group in WDXRF. In the same context, iron oxides have a significant impact on the firing atmosphere of iron-rich clay, resulting in blackening under reducing conditions and a reddish coloration under oxidative conditions. The use of hematite and gypsum as pigments further contributes to the color variations in the pottery. The consistent firing temperature range of 200–600 °C in Dudești pottery implies a standardized production process, the variation in color being dependent on the specific reducing/oxidative regime conditions (reducing atmosphere followed by rapid oxidation). This relationship between clay composition and local sources suggests a connection to Neolithic pottery production in the region and their color depending on the reducing/oxidative regime conditions. Full article
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9 pages, 6634 KiB  
Communication
Defects and Mechanical Properties of Silicon Nitride Ball Bearings for Electric Vehicle Reducers
by Jinhyeok Jang, Youngmin Lee, Hoonhee Cheong and Jeongho Yang
World Electr. Veh. J. 2024, 15(6), 272; https://doi.org/10.3390/wevj15060272 - 20 Jun 2024
Cited by 2 | Viewed by 1865
Abstract
In this study, two types of Si3N4 ball bearings for integrated-type EV reducers developed via different manufacturing processes were analyzed to study the microstructure of the balls and the defects that may occur during the manufacturing process. Three types of [...] Read more.
In this study, two types of Si3N4 ball bearings for integrated-type EV reducers developed via different manufacturing processes were analyzed to study the microstructure of the balls and the defects that may occur during the manufacturing process. Three types of defects were confirmed that can reduce the fatigue life of Si3N4 ball bearings in operating environments. The microstructure was analyzed to identify the main additive components of each bearing, and pore defects with a size of less than 1 μm, and the types (particle defects or surface defects) and sizes of defects, were analyzed using LSCM, OM, and SEM. Hardness and fracture toughness, which are representative mechanical properties of ceramic materials, were evaluated. The results, evaluated using a Vickers indentation crack-based method, were statistically analyzed to confirm differences in hardness and fracture toughness between the two samples. Full article
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20 pages, 18808 KiB  
Article
Evolution of Pore Spaces in Marine Organic-Rich Shale: Insights from Multi-Scale Analysis of a Permian–Pennsylvanian Sample
by Zilong Wang, Xiaoguang Yang and Shaobin Guo
Minerals 2024, 14(4), 392; https://doi.org/10.3390/min14040392 - 10 Apr 2024
Cited by 3 | Viewed by 1441
Abstract
The quantitative evolution pattern of pore space and genetic pore types along the maturation process in organic-rich shale reservoirs is unclear, which affects the assessment of shale storage capacity and petroleum production. A black shale outcrop sample from Kansas that is of Permian–Pennsylvanian [...] Read more.
The quantitative evolution pattern of pore space and genetic pore types along the maturation process in organic-rich shale reservoirs is unclear, which affects the assessment of shale storage capacity and petroleum production. A black shale outcrop sample from Kansas that is of Permian–Pennsylvanian age was collected and subjected to thermal simulation experiments at 10 different maturity stages to understand the pore sizes and pore types. Scanning electron microscopy (SEM) and image processing were used to characterize the full-scale pore-size distribution and volume evolution of this shale sample by combining low-temperature gas (CO2 and N2) physisorption and mercury intrusion porosimetry (MIP) in order to discuss the effects of hydrocarbon generation and diagenesis (HG&D) on pore development at different pore sizes. The study showed that the original shale sample is dominated by slit-like pores, with mainly organic matter (OM) pores distributed in 0–100 nm, intraparticle pores (Intra-P) of clays distributed in 30–100 nm, and interparticle pores (Inter-P) distributed in 100–1000 nm. With the increase in maturity or Ro, the OM pores increased gradually, and the OM pore-size distribution diverged to the two poles. In the oil generation stage, the OM pores were distributed in the range of 30–100 nm, while in the gas generation stage, the OM-hosted pores were mainly distributed in the range of 10–20 nm and 100–500 nm. Further into the over-maturity stage, the OM pores were mainly distributed in the range of 0–10 nm and >100 nm. The pore volume distribution across the whole pore sizes showed that the pore volume of low-maturity shale samples was mainly provided by 100–1000 nm (macropores), and the pore volumes of 0–2 nm, 30–100 nm and 1000+ nm pores gradually increase with increasing thermal maturity, with the final pore-size distribution having four peaks at 0–2, 30–100, 500–1000 nm, and 10–100 µm. Hydrocarbon generation mainly affects the pore volume in the 0–2 nm and 100–1000 nm intervals, with a positive correlation. The 2–30 nm and 30–100 nm pores were likely controlled by diagenesis, such as mineral transformation, illitization, and cementation during the maturation process. Full article
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14 pages, 4698 KiB  
Article
Simultaneous Pore Detection and Morphological Features Extraction in Laser Powder Bed Fusion with Image Processing
by Jiaming Li, Xiaoxun Zhang, Fang Ma, Shuxian Wang and Yuanyou Huang
Materials 2024, 17(6), 1373; https://doi.org/10.3390/ma17061373 - 17 Mar 2024
Viewed by 1555
Abstract
Internal pore defects are inevitable during laser powder bed fusion (LPBF), which have a significant impact on the mechanical properties of the parts. Therefore, detecting pores and obtaining their morphology will contribute to the quality of LPBF parts. Currently, supervised models are used [...] Read more.
Internal pore defects are inevitable during laser powder bed fusion (LPBF), which have a significant impact on the mechanical properties of the parts. Therefore, detecting pores and obtaining their morphology will contribute to the quality of LPBF parts. Currently, supervised models are used for defect image detection, which requires a large amount of LPBF sample data, image labeling, and computing power equipment during the training process, resulting in high detection costs. This study extensively collected LPBF sample data and proposed a method for pore defect classification by obtaining its morphological features while detecting pore defects in optical microscopy (OM) images under various conditions. Compared with other advanced models, the proposed method achieves better detection accuracy on pore defect datasets with limited data. In addition, quickly detecting pore defects in a large number of labeling ground truth images will also contribute to the development of deep learning. In terms of image segmentation, the average accuracy scores of this method in the test images exceed 85%. The research results indicate that the algorithm proposed in this paper is suitable for quickly and accurately identifying pore defects from optical microscopy images. Full article
(This article belongs to the Section Advanced Composites)
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10 pages, 5033 KiB  
Communication
Effect of Sintering Temperature on Microstructure Characteristics of Porous NiTi Alloy Fabricated via Elemental Powder Sintering
by Tianhu Miao, Sha Zhan, Xiaojuan Chen and Li Hu
Materials 2024, 17(3), 743; https://doi.org/10.3390/ma17030743 - 4 Feb 2024
Cited by 2 | Viewed by 1842
Abstract
To investigate the effect of the sintering temperature on the microstructure characteristics of porous NiTi alloys, two types of porous NiTi alloys with equal atomic ratios were fabricated via elemental powder sintering at 950 °C and 1000 °C. Afterwards, optical microscopy (OM), scanning [...] Read more.
To investigate the effect of the sintering temperature on the microstructure characteristics of porous NiTi alloys, two types of porous NiTi alloys with equal atomic ratios were fabricated via elemental powder sintering at 950 °C and 1000 °C. Afterwards, optical microscopy (OM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were collectively applied to investigate the pore characteristics and microstructure of the fabricated porous NiTi alloy. The results show that when the sintering temperature increases from 950 °C to 1000 °C, the average pore size increases from 36.00 μm to 181.65 μm, owing to the integration of these newly formed small pores into these pre-existing large-sized pores. The measured density increases from 2.556 g/cm3 to 3.030 g/cm3, while the porosity decreases from 60.4% to 51.8%. This is due to the occurrence of shrinkage after the sufficient diffusion of atoms. Furthermore, the characterization results confirm that a change in the sintering temperature would not change the phase types within a porous NiTi alloy; namely, the matrix consists primarily of B2 NiTi, with a significant amount of Ni4Ti3 precipitates and a small amount of Ni3Ti precipitates and Ti2Ni precipitates. However, as the sintering temperature increases, the number of Ni4Ti3 precipitates decreases significantly. The formation of a Ni4Ti3 phase in the present study is closely related to the enrichment of Ni content in the matrix owing to the diffusion rate difference between Ni atoms and Ti atoms and the absence of a transient liquid phase (TLP) during the sintering process owing to the relatively low sintering temperature (lower than the eutectic temperature). Moreover, the increasing sintering temperature speeds up the atom diffusion, which contributes to a reduction in the enrichment of Ni as well as the number of formed Ni4Ti3 precipitates. Full article
(This article belongs to the Section Metals and Alloys)
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