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20 pages, 54914 KiB  
Article
Treatment and Valorization of Waste Wind Turbines: Component Identification and Analysis
by Xiaohan Zhao, Daria Pakuła, Miłosz Frydrych, Roksana Konieczna, Bogna Sztorch, Rafał Kozera, Hongzhi Liu, Hui Zhou and Robert E. Przekop
Materials 2025, 18(2), 468; https://doi.org/10.3390/ma18020468 - 20 Jan 2025
Abstract
Recycling end-of-life wind turbines poses a significant challenge due to the increasing number of turbines going out of use. After many years of operation, turbines lose their functional properties, generating a substantial amount of composite waste that requires efficient and environmentally friendly processing [...] Read more.
Recycling end-of-life wind turbines poses a significant challenge due to the increasing number of turbines going out of use. After many years of operation, turbines lose their functional properties, generating a substantial amount of composite waste that requires efficient and environmentally friendly processing methods. Wind turbine blades, in particular, are a problematic component in the recycling process due to their complex material composition. They are primarily made of composites containing glass and carbon fibers embedded in polymer matrices such as epoxies and polyester resins. This study presents an innovative approach to analyzing and valorizing these composite wastes. The research methodology incorporates integrated processing and analysis techniques, including mechanical waste treatment using a novel compression milling process, instead of traditional knife mills, which reduces wear on the milling tools. Based on the differences in the structure and colors of the materials, 15 different kinds of samples named WT1-WT15 were distinguished from crushed wind turbines, enabling a detailed analysis of their physicochemical properties and the identification of the constituent components. Fourier transform infrared spectroscopy (FTIR) identified key functional groups, confirming the presence of thermoplastic polymers (PET, PE, and PP), epoxy and polyester resins, wood, and fillers such as glass fibers. Thermogravimetric analysis (TGA) provided insights into thermal stability, degradation behavior, and the heterogeneity of the samples, indicating a mix of organic and inorganic constituents. Differential scanning calorimetry (DSC) further characterized phase transitions in polymers, revealing variations in thermal properties among samples. The fractionation process was carried out using both wet and dry methods, allowing for a more effective separation of components. Based on the wet separation process, three fractions—GF1, GF2, and GF3—along with other components were obtained. For instance, in the case of the GF1 < 40 µm fraction, thermogravimetric analysis (TGA) revealed that the residual mass is as high as 89.7%, indicating a predominance of glass fibers. This result highlights the effectiveness of the proposed methods in facilitating the efficient recovery of high-value materials. Full article
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<p>Separation method.</p>
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<p>FTIR spectra of: (<b>A</b>) WT1, WT3; (<b>B</b>) WT2, WT5, WT8; (<b>C</b>) WT4, WT6; (<b>D</b>) WT10-12.</p>
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<p>TGA curves of (<b>A1</b>) WT1, WT3; (<b>B1</b>) WT6, WT7; (<b>C1</b>) WT2, WT5, WT8, WT10-12; (<b>D1</b>) WT13-WT15; (<b>E1</b>) WT4 and DTG curves of (<b>A2</b>) WT1, WT3; (<b>B2</b>) WT6, WT7; (<b>C2</b>) WT2, WT5, WT8, WT10-12; (<b>D2</b>) WT13-WT15; (<b>E2</b>) WT4 in nitrogen atmosphere.</p>
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<p>DSC curves of (<b>A</b>) WT1; (<b>B</b>) WT3; (<b>C</b>) WT2, WT6; (<b>D</b>) WT4-5, WT8, WT10; (<b>E</b>) WT11-12; (<b>F</b>) WT13-15.</p>
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<p>Mass sample of different fractions: (<b>a</b>) summed up for GF1-3 and others; (<b>b</b>) based on the size.</p>
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<p>TGA (<b>A1</b>–<b>C1</b>) and DTG (<b>A2</b>–<b>C2</b>) curves of glass fibers in nitrogen atmosphere.</p>
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16 pages, 490 KiB  
Article
COVID-19-Related Discontinuation Impact on Patient-Reported Outcomes in Long-Term Thermal Therapy: A Single-Center Observational Study at Saturnia Thermal Springs
by Elisabetta Ferrara, Manela Scaramuzzino, Giovanna Murmura, Gianmaria D’Addazio and Bruna Sinjari
Healthcare 2025, 13(2), 202; https://doi.org/10.3390/healthcare13020202 - 20 Jan 2025
Abstract
Background: Thermal therapy represents a well-established therapeutic approach for chronic musculoskeletal and respiratory conditions. To date, no studies have investigated the clinical effects of treatment interruption in thermal medicine. We aimed to evaluate the clinical impact of COVID-19 lockdown-induced thermal therapy discontinuation through [...] Read more.
Background: Thermal therapy represents a well-established therapeutic approach for chronic musculoskeletal and respiratory conditions. To date, no studies have investigated the clinical effects of treatment interruption in thermal medicine. We aimed to evaluate the clinical impact of COVID-19 lockdown-induced thermal therapy discontinuation through validated patient-reported outcomes. Methods: This single-center observational, retrospective study (March 2020–June 2024) evaluated 97 patients receiving standardized thermal therapy at Saturnia Thermal Springs. Treatment protocols included balneotherapy, mud therapy, and inhalation treatments in cycles of 12–15 sessions, with maintenance protocols every 4–6 months. Primary outcomes were assessed through VAS and SF-36 PCS, with EQ-5D and PSQI as secondary outcomes. Results: Significant clinical deterioration occurred during treatment interruption (p < 0.001) in 77.7% of patients. Recovery patterns were duration-dependent, with the 6–7-year cohort showing faster recovery (mean time to baseline: 2.8 months) compared to the 3–5-year cohort (4.6 months). Effect sizes were substantial across all outcomes (Cohen’s d > 1.0), with EQ-5D scores showing duration-dependent improvement (mean improvement in 6–7-year cohort: 0.27). Conclusions: Thermal therapy interruption precipitates quantifiable clinical deterioration, with recovery patterns significantly influenced by pre-existing treatment duration. These findings support the essential nature of treatment continuity in thermal therapy protocols. Full article
(This article belongs to the Special Issue Human Health Before, During, and After COVID-19)
19 pages, 2787 KiB  
Article
Effect of High-Pressure Processing on Color, Texture and Volatile Profile During Sardine Refrigeration
by Lama Ismaiel, Ancuta Nartea, Benedetta Fanesi, Paolo Lucci, Deborah Pacetti, Henry Jaeger and Felix Schottroff
Foods 2025, 14(2), 329; https://doi.org/10.3390/foods14020329 - 20 Jan 2025
Abstract
Extending sardine shelf life while maintaining their quality is challenging even with non-thermal technologies like high-pressure processing (HPP). This study examines the effects of HPP at 400 and 600 MPa for holding times of 1, 2.5, 5, and 10 min on fresh sardines [...] Read more.
Extending sardine shelf life while maintaining their quality is challenging even with non-thermal technologies like high-pressure processing (HPP). This study examines the effects of HPP at 400 and 600 MPa for holding times of 1, 2.5, 5, and 10 min on fresh sardines during 14 days of cold storage. Physicochemical attributes, including texture, color, and volatile organic profiles, were assessed. Increasing both pressure and holding times resulted in increased levels of hardness, chewiness, and L* during storage. HPP-treated samples maintained lower a* values compared to the control ones by the end of the experiment. The volatile profile of HPP samples was significantly affected compared to control samples, which developed exclusively volatile oxidation compounds (hexanal and 2,4-hexadienal) by the end of the storage. Volatile groups such as aldehyde and ketone were slightly impacted by both storage and HPP treatments (i.e., pressure and holding time). Ketone levels were consistently lower in all treated samples, ranging from 25.3% to 33.6% at 400 MPa and 600 MPa, respectively, compared to the control samples, which had a ketone level of 40.5% on day 14. These findings indicate the potential of HPP in prolonging shelf life and preserving quality in the sardine market. Full article
(This article belongs to the Section Food Engineering and Technology)
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<p>Schematic illustration. (<b>a</b>) The measured points on the surface of the sardine filet for color and texture analysis. (<b>b</b>) The experimental design. Three replicates for each sample were considered.</p>
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<p>(<b>a</b>) Important features selected by ANOVA plots with <span class="html-italic">p</span>-value threshold 0.05. (<b>b</b>) Changes in TPA profile (hardness, chewiness, springiness, cohesiveness and adhesiveness) in sardine filets after HPP treatment and during cold storage (0, 7, 14 days), in comparison to the control. Samples are named as follows: pressure level in MPa; holding time in minutes. Three replicates for each sample were considered. Different letters indicate significant differences (<span class="html-italic">p</span> &lt; 0.05) between control and HPP-treated samples independently from the storage day. * indicates no significant differences.</p>
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<p>Important features for color changes selected by ANOVA plots with <span class="html-italic">p</span>-value threshold 0.05. (<b>a</b>) Statistical differences between control and treated samples (pressure-holding time) independently from the storage period. (<b>b</b>) Statistical differences between control and treated samples during storage.</p>
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<p>Changes in volatile classes of sardine oil in treated and untreated control samples. Samples are named as follows: pressure level in MPa; storage period in days, independently from the pressure-holding time (i.e., data for holding times were considered as one variable for each treatment). Control values are indicated by C. (<b>a</b>) The scoring radar chart displays the changes in volatile classes expressed as a relative percentage of the total peak area. (<b>b</b>) Box plots exhibiting the variation in significant differences (<span class="html-italic">p</span> &lt; 0.05) in ketones and aldehydes.</p>
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<p>Changes in volatile compounds between HPP-treated and control samples at the end of tested cold storage (14 days). (<b>a</b>) Log2 fold change with a threshold of 3; positive values indicate predominant volatile compounds in control samples and negative ones indicate volatile compounds accumulated in HPP-treated samples. (<b>b</b>) Box plots of some discriminant compounds accumulated in control samples. Significance levels are indicated by * &lt;0.05 and ** &lt;0.01.</p>
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<p>Changes in volatile compounds at the end of the tested storage period, i.e., day 14. PCA score plot (<b>a</b>) and biplot (<b>b</b>) for the volatile compound profile of sardine oil samples treated with HPP and control ones. Samples are named as follows: pressure levels in MPa; holding time in minutes; storage time in days.</p>
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14 pages, 1815 KiB  
Article
Influence of Oil-Soluble Catalyst on Composition and Structure of Heavy Oil from Samara Region Field
by Mohammed O. N. Ali, Irek I. Mukhamatdinov, Boudkhil Affane, Rezeda E. Mukhamatdinova, Vladimir E. Katnov and Alexey V. Vakhin
ChemEngineering 2025, 9(1), 11; https://doi.org/10.3390/chemengineering9010011 - 20 Jan 2025
Abstract
In this study, an examination was conducted of the influence of iron tallate on the composition and properties of highly viscous oil from the Strelovskoye deposit in the Samara region under thermal–catalytic treatment (TCT). The research revealed that the dynamic viscosity of the [...] Read more.
In this study, an examination was conducted of the influence of iron tallate on the composition and properties of highly viscous oil from the Strelovskoye deposit in the Samara region under thermal–catalytic treatment (TCT). The research revealed that the dynamic viscosity of the oil following TCT at 300 °C, with a measurement temperature of 20 °C, decreased by a factor of 8 in comparison to the initial sample and nearly 4.5 times compared to the control sample at the 96-h mark. The most promising results in reducing the pour point temperature to 7 °C were identified following a 96-h TCT at 300 °C. This reduction was attributed to the decrease in paraffin content facilitated by the presence of the catalyst. According to the ICP-MS results, the extraction of the catalyst with the oil amounted to only 1%. This indicates that during the implementation of TCT within the reservoir, the catalyst is likely to adsorb onto the rock surfaces. Full article
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<p>Viscosity–temperature characteristics of the initial oil and oil samples after thermocatalytic treatment (TCT) with and without iron catalyst at a temperature of 250 °C and varying treatment durations.</p>
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<p>Viscosity–temperature characteristics of the initial oil and oil samples after thermocatalytic treatment (TCT) with and without iron catalyst at a temperature of 300 °C and varying treatment durations.</p>
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<p>MALDI mass spectra of resins: (<b>a</b>) initial oil; (<b>b</b>) Str-K-300-96; (<b>c</b>) Str-Fe+RASPO-1+W-S-300-96; (<b>d</b>) Str-Ni+RASPO-1+W-S-300-96.</p>
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<p>MALDI mass spectra of asphaltenes: (<b>a</b>) initial oil; (<b>b</b>) Str-K-300-96; (<b>c</b>) Str-Fe+RASPO-1+W-S-300-96; (<b>d</b>) Str-Ni+RASPO-1+W-S-300-96.</p>
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21 pages, 8422 KiB  
Article
Impact of Thermal Treatment and Accelerated Aging on the Chemical Composition, Morphology, and Properties of Spruce Wood
by František Kačík, Jozef Kúdela, Eva Výbohová, Tereza Jurczyková, Iveta Čabalová, Lukáš Adamčík, Elena Kmeťová and Danica Kačíková
Forests 2025, 16(1), 180; https://doi.org/10.3390/f16010180 - 19 Jan 2025
Viewed by 408
Abstract
Thermal modification improves the properties of wood, especially its stability and durability. We thermally treated spruce wood with the Thermowood process at three temperatures (160 °C, 180 °C, and 210 °C) and subjected it to accelerated aging in wet mode. We evaluated the [...] Read more.
Thermal modification improves the properties of wood, especially its stability and durability. We thermally treated spruce wood with the Thermowood process at three temperatures (160 °C, 180 °C, and 210 °C) and subjected it to accelerated aging in wet mode. We evaluated the chemical composition (wet chemistry, infrared spectroscopy), color, surface morphology, and wetting of the wood surface with water. Thermal treatment caused a significant decrease in hemicelluloses (up to 72.39% at a temperature of 210 °C), which initiated an increase in the content of more resistant wood components—cellulose and lignin. With accelerated aging, the hemicellulose content decreased by another 5%. The most significant differences between the infrared spectra of thermally modified wood before and after exposure to accelerated aging were in the absorption bands of lignin (1509 and 1596 cm−1) and in the region of carbonyl groups between 1800 and 1630 cm−1. Thermal treatment also caused a change in the color of the wood to dark brown; the overall color difference ΔE increased several times. The thermal-induced shortening of polysaccharide fibers and reduction in their width were even more manifested during accelerated aging. This work contains new knowledge about the properties critical for the reuse of thermally modified wood after accelerated aging, simulating the end of its life cycle. Full article
(This article belongs to the Special Issue Transformation of Wood after Processing and Modification)
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<p>Thermal modification process of spruce wood [<a href="#B3-forests-16-00180" class="html-bibr">3</a>].</p>
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<p>The test specimen of spruce wood.</p>
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<p>Color variation in spruce wood specimens during thermal treatment and accelerated aging.</p>
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<p>Differences in color coordinates and the total color difference after thermal treatment of spruce wood.</p>
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<p>Differences in color coordinates and the total color difference thermal treatment spruce wood after accelerated aging.</p>
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<p>Topographic elevation map of spruce wood surface after different thermal modifications.</p>
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<p>Topographic elevation map of thermally modified spruce wood after 600 h of accelerated aging.</p>
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<p>(<b>a</b>). FTIR spectra of spruce wood thermally treated at 160 °C (160-TW) and after accelerated aging (160-TW-XE). (<b>b</b>). FTIR spectra of spruce wood thermally treated at 180 °C (180-TW) and after accelerated aging (180-TW-XE). (<b>c</b>). FTIR spectra of spruce wood thermally treated at 210 °C (210-TW) and after accelerated aging (210-TW-XE).</p>
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<p>(<b>a</b>). FTIR spectra of spruce wood thermally treated at 160 °C (160-TW) and after accelerated aging (160-TW-XE). (<b>b</b>). FTIR spectra of spruce wood thermally treated at 180 °C (180-TW) and after accelerated aging (180-TW-XE). (<b>c</b>). FTIR spectra of spruce wood thermally treated at 210 °C (210-TW) and after accelerated aging (210-TW-XE).</p>
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<p>Fiber length distribution of spruce wood samples depends on its treatment.</p>
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<p>Fiber width distribution of spruce wood samples depends on its treatment.</p>
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18 pages, 7230 KiB  
Article
An Extensive Study of an Eco-Friendly Fireproofing Process of Lignocellulosic Miscanthus × giganteus Particles and Their Application in Flame-Retardant Panels
by Yasmina Khalaf, Rodolphe Sonnier, Nicolas Brosse and Roland El Hage
Polymers 2025, 17(2), 241; https://doi.org/10.3390/polym17020241 - 19 Jan 2025
Viewed by 461
Abstract
Increasing the flame retardancy of lignocellulosic materials such as Miscanthus × giganteus can effectively enable their wide use. This study examines the fireproofing process of Miscanthus particles using an eco-friendly process by grafting phytic acid and urea in aqueous solution. Miscanthus particles underwent [...] Read more.
Increasing the flame retardancy of lignocellulosic materials such as Miscanthus × giganteus can effectively enable their wide use. This study examines the fireproofing process of Miscanthus particles using an eco-friendly process by grafting phytic acid and urea in aqueous solution. Miscanthus particles underwent a steam explosion step before being grafted. Fireproof binderless particle panels were manufactured from miscanthus particles with or without adding olive pomace by hot-pressing. The effect of the steam explosion and/or the flame-retardant treatment on the morphology, chemical composition and thermal stability of the particles, as well as the thermal stability of the panels, was investigated. The results showed that water impregnation followed by a steam explosion at 210 °C for 8 min resulted in particles that were rich in lignin and more homogeneous in size (length and width). Fireproof particles were produced with relatively low P and N contents. The flame retardancy of the binderless particle panels was significantly improved when using miscanthus particles treated with phytic acid and urea, as shown by a reduced heat release (HRR) and an increased time-to-ignition. However, the presence of olive pomace significantly decreased the flame retardancy of the panels. Binderless particle panels prepared from grafted miscanthus particles showed the best fire properties and are considered fireproof. Full article
(This article belongs to the Section Polymer Applications)
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<p>The different steam exploded miscanthus particles obtained.</p>
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<p>The different panels produced.</p>
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<p>Box plots representing the sizes of raw M and the different M exploded particles: (<b>A</b>) length of particles (mm); (<b>B</b>) width of particles (mm).</p>
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<p>Evolution of the heat release rate (HRR) as a function of temperature for exploded miscanthus particles with and without grafting.</p>
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<p>Binderless particle panels (<b>A</b>) before the flammability test and (<b>B</b>) after the flammability test.</p>
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<p>HRR curves obtained by cone calorimeter at an irradiance of 35 kW/m<sup>2</sup> for all panels.</p>
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<p>Rate of smoke released (RSR) curves obtained by cone calorimeter at an irradiance of 35 kW/m<sup>2</sup> for all panels.</p>
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<p>Photographs of the binderless particle panels after the cone calorimeter test ((<b>A</b>): Mse; (<b>B</b>): MseOP; (<b>C</b>): Mseg; and (<b>D</b>): MsegOP).</p>
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18 pages, 15689 KiB  
Article
Using a Combined FE-CA Approach to Investigate Abnormally Large Grains Formed by the Limited Recrystallization Mechanism in a Powder Metallurgy Nickel-Based Superalloy
by Yanhui Yang, Boyan Zhang, Xiuquan Chen, Xiaoxuan Wang, Yankai Feng, Lidong Su, Zhengfei Liang and Yifan Liu
Crystals 2025, 15(1), 91; https://doi.org/10.3390/cryst15010091 (registering DOI) - 19 Jan 2025
Viewed by 158
Abstract
Powder nickel-based superalloy is the key material for hot-end components such as turbine disks and gas engine disks in aeroengines, and its microstructure uniformity has an important influence on the disks’ service performance. However, thermomechanical treatments make it easy to produce abnormally large [...] Read more.
Powder nickel-based superalloy is the key material for hot-end components such as turbine disks and gas engine disks in aeroengines, and its microstructure uniformity has an important influence on the disks’ service performance. However, thermomechanical treatments make it easy to produce abnormally large grains (ALGs) in powder superalloy disks. In order to investigate the relationship between the hot deformation conditions and ALGs of powder superalloys, isothermal compression experiments under various deformation conditions were carried out and a FE-CA method was constructed to investigate the ALGs formed by the limited recrystallization mechanism. The results indicate a close relationship between the ALGs formed after the supersolvus treatment of this alloy and the equivalent stress after thermal deformation, and the local dissolution of the γ′ phase in supersolvus heat treatment does not produce ALGs. Full article
(This article belongs to the Section Crystalline Metals and Alloys)
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Figure 1
<p>The microstructure of the P/M nickel-based superalloy bar at the edge position. (<b>a</b>) The SEM images of the primary and secondary γ′; (<b>b</b>) the IPF map of the alloy grain.</p>
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<p>The schematic diagram of the sampling location for hot compression specimens and the subsequent experimental processes.</p>
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<p>The microstructure at <span class="html-italic">P</span><sub>1</sub> after holding the alloy at 1150 °C for 2 h following separate hot deformation at 1020 °C. The reduction amounts of (<b>a<sub>i</sub></b>–<b>c<sub>i</sub></b>) (i = 1, 2, 3) are 10%, 30%, and 60%, respectively; the reduction rates corresponding to (<b>a<sub>1</sub></b>–<b>a<sub>4</sub></b>) are 0.001 s<sup>−1</sup>, 0.01 s<sup>−1</sup>, 0.1 s<sup>−1</sup>, and 1 s<sup>−1</sup>, respectively; and the meanings of (<b>b<sub>1</sub></b>–<b>b<sub>4</sub></b>,<b>c<sub>1</sub></b>–<b>c<sub>4</sub></b>) are the same as those of (<b>a<sub>1</sub></b>–<b>a<sub>4</sub></b>).</p>
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<p>The microstructure at <span class="html-italic">P</span><sub>1</sub> after holding the alloy at 1150 °C for 2 h following separate hot deformation at 1090 °C. The reduction amounts of (<b>a<sub>i</sub></b>–<b>c<sub>i</sub></b>) (i = 1, 2, 3) are 10%, 30%, and 60%, respectively; the reduction rates corresponding to (<b>a<sub>1</sub></b>–<b>a<sub>4</sub></b>) are 0.001 s<sup>−1</sup>, 0.01 s<sup>−1</sup>, 0.1 s<sup>−1</sup>, and 1 s<sup>−1</sup>, respectively; and the meanings of (<b>b<sub>1</sub></b>–<b>b<sub>4</sub></b>) and (<b>c<sub>1</sub></b>–<b>c<sub>4</sub></b>) are the same as those of (<b>a<sub>1</sub></b>–<b>a<sub>4</sub></b>).</p>
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<p>The microstructure photos and corresponding grain size distributions of the alloy after hot deformation and over-solution treatment. Hot deformation conditions: (<b>a</b>) 1020 °C, reduction 30%, reduction rate 0.005 s<sup>−1</sup>; (<b>b</b>) 1070 °C, reduction 10%, reduction rate 0.1 s<sup>−1</sup>; (<b>c</b>) 1090 °C, reduction 30%, reduction rate 0.005 s<sup>−1</sup>; (<b>d</b>) 1070 °C, reduction 30%, reduction rate 0.3 s<sup>−1</sup>. The grain size distributions of (<b>a</b>–<b>d</b>) correspond to (<b>e</b>–<b>h</b>).</p>
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<p>The displacement–load curve and final dimensions of the specimen obtained by simulation and test under thermal deformation conditions of 1020 °C, a reduction rate of 0.1 s<sup>−1</sup>, and a reduction 60%.</p>
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<p>The distribution nephograms of strain, strain rate, and stress after a deformation temperature of 1020 °C, reduction rate of 1 s<sup>−1</sup> and reduction of 10%, and microstructure photographs after over-solution treatment. (<b>a</b>–<b>c</b>) Nephograms of equivalent stress, equivalent strain, and equivalent strain rate distribution in the shaded area in (<b>d</b>) after thermal deformation, respectively; (<b>e</b>) is the microstructure of the shaded area in (<b>d</b>) after solution treatment; and (<b>f</b>) is the enlarged area of abnormally large grain microstructure in (<b>e</b>).</p>
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<p>The distribution nephograms of strain, strain rate, and stress after a deformation temperature of 1070 °C, reduction rate of 0.3 s<sup>−1</sup> and reduction of 30%, and microstructure photographs after over-solution treatment. (<b>a</b>–<b>c</b>) Nephograms of equivalent stress, equivalent strain, and equivalent strain rate distribution in the shaded area in (<b>d</b>) after thermal deformation, respectively; (<b>e</b>) is the microstructure of the shaded area in (<b>d</b>) after solution treatment; and (<b>f</b>) is the enlarged area of abnormally large grain microstructure in (<b>e</b>).</p>
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<p>Microstructure of ALGs after over-solution treatment under different heat deformation conditions. (<b>a</b>) #1020-0.5-30; (<b>b</b>) #1020-1-10.</p>
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<p>The CA simulation results of grain growth accompanied by the dissolution of the γ′ phase in supersolvus heat treatment. (<b>a<sub>1</sub></b>–<b>a<sub>4</sub></b>) The CA simulation results of the grain growth accompanied by the local dissolution of the γ′ phase. (<b>b<sub>1</sub></b>–<b>b<sub>4</sub></b>) The CA simulation results of the grain growth accompanied by the complete dissolution of the γ′ phase.</p>
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<p>LM and twin boundary maps for hot-deformed microstructures (#1020-0.5-30) corresponding to ALGs zone before and after over-solution treatment. (<b>a</b>) LM maps before over-solution treatment; (<b>b</b>) LM maps after over-solution treatment; (<b>c</b>) inverse pole figure after over-solution treatment; (<b>d</b>) twin boundary maps after over-solution treatment.</p>
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<p>LM and twin boundary maps for hot-deformed microstructures (#1020-1-10) corresponding to ALGs zone before and after over-solution treatment. (<b>a</b>) LM maps before over-solution treatment; (<b>b</b>) LM maps after over-solution treatment; (<b>c</b>) inverse pole figure after over-solution treatment.</p>
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<p>Stress–strain curve, cross section microstructure, and von Mises equivalent stress distribution diagram of specimen under thermal deformation conditions #1020-1-10. (<b>a</b>) The stress–strain curve. (<b>b</b>) Cross section microstructure and von Mises equivalent stress distribution diagram.</p>
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<p>The CA simulation and experimental results of the formation process of ALGs in the over-solution treatment process of zone A. (<b>a</b>–<b>c</b>) The CA simulation results from the initial, middle, and end of the over-solution treatment, respectively. (<b>d</b>) The microstructure of region A after over-solution treatment.</p>
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<p>The CA simulation and experimental results of the formation process of ALGs in the over-solution treatment process of zone B. (<b>a</b>–<b>c</b>) The CA simulation results from the initial, middle, and end of the over-solution treatment, respectively. (<b>d</b>) The microstructure of region B after over-solution treatment.</p>
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<p>TEM images of region A before and after over-solution treatment under thermal deformation conditions #1020-1-10. (<b>a</b>) Before over-solution treatment; (<b>b</b>) after over-solution treatment.</p>
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13 pages, 898 KiB  
Article
Changes in Microbial Safety and Quality of High-Pressure Processed Camel Milk
by Tareq M. Osaili, Dinesh Kumar Dhanasekaran, Fayeza Hasan, Reyad S. Obaid, Anas A. Al-Nabulsi, Amin N. Olaimat, Leila Cheikh Ismail, Nadia Alkalbani, Mutamed Ayyash, Gafar Babatunde Bamigbade, Richard Holley, Adan Shahzadi Cheema, Wael Ahmad Bani Odeh, Khalid Abdulla Mohd and Ayesha Khalid Haji Kamal
Foods 2025, 14(2), 320; https://doi.org/10.3390/foods14020320 - 19 Jan 2025
Viewed by 350
Abstract
High-pressure processing (HPP) is used as a non-thermal approach for controlling microbial viability. The purposes of this study were to (i) establish the decimal reduction times (D-values) for pathogenic bacteria during 350 MPa HPP treatment,; (ii) evaluate the impact of 350 MPa HPP [...] Read more.
High-pressure processing (HPP) is used as a non-thermal approach for controlling microbial viability. The purposes of this study were to (i) establish the decimal reduction times (D-values) for pathogenic bacteria during 350 MPa HPP treatment,; (ii) evaluate the impact of 350 MPa HPP on total plate count (TPC), yeasts and molds (YM), and lactic acid bacteria (LAB) in camel milk; (iii) investigate the behavior of several spoilage-causing bacteria during storage at 4 °C and 10 °C for up to 10 d post-HPP treatment; and (iv) assess the effect of HPP on the protein degradation of camel milk. The D-values for L. monocytogenes, E. coli O157:H7, and Salmonella spp. were 3.77 ± 0.36 min, 1.48 ± 0.08 min, and 2.10 ± 0.13 min, respectively. The HPP treatment decreased pathogenic microorganisms by up to 2 to 3 log cfu/mL (depending on treatment conditions). However, HPP reduced TPC, YM, and LAB by <1 log cfu/mL, regardless of the length of pressure exposure. HPP treatment, even at extended holding times, did not significantly alter either the proteolytic activity or casein micelle structure in camel milk. This study highlights HPP as a promising non-thermal technique for enhancing the microbiological safety of camel milk. Full article
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<p>Survival curve of (<b>a</b>) <span class="html-italic">Salmonella</span> spp. (R<sup>2</sup> = 0.960, correlation coefficient = −0.586), (<b>b</b>) <span class="html-italic">L. monocytogenes</span> (R<sup>2</sup> = 0.928, correlation coefficient = −0.402) with confidence and predication bands (dotted lines in camel milk samples) at 350 MPa, and (<b>c</b>) <span class="html-italic">E. coli</span> O157:H7 spp. (R<sup>2</sup> = 0.938, correlation coefficient = −0.433) at 300 MPa.</p>
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<p>SDS-PAGE gel with the lanes representing the (1) marker, 350 MPa HPP treatment of camel milk, at (2) 0 min, (3) 1 min, (4) 2 min, (5) 3 min, (6) 4 min, and (7) 5 min, respectively.</p>
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17 pages, 6785 KiB  
Article
Herbicidal Formulations with Plant-Based Compounds to Control Amaranthus hybridus, Lolium multiflorum, and Brassica rapa Weeds
by Juan J. Romero, Juliana Soler-Arango, Marcos E. Coustet, Daniela B. Moracci, Sebastián Reinoso, Marcos E. Yanniccari, Aline Schneider-Teixeira and Jimena M. Herrera
Plants 2025, 14(2), 276; https://doi.org/10.3390/plants14020276 - 18 Jan 2025
Viewed by 502
Abstract
Numerous studies have shown the potential effect of bioactive agents against weeds. In this study, we developed two binary formulations with nonanoic acid, citral, or thymoquinone as herbicides and evaluated their physicochemical properties. The presence of the bioactive compounds in the formulations was [...] Read more.
Numerous studies have shown the potential effect of bioactive agents against weeds. In this study, we developed two binary formulations with nonanoic acid, citral, or thymoquinone as herbicides and evaluated their physicochemical properties. The presence of the bioactive compounds in the formulations was confirmed through FTIR spectroscopy. A dynamic light scattering study was conducted to characterize the emulsified formulations and the size and distribution of the aggregates. In addition, thermogravimetric analysis was performed to ensure the thermal stability of the formulations. The herbicidal activity against Amaranthus hybridus, Lolium multiflorum, and Brassica rapa weeds was evaluated, and each species showed different levels of sensitivity with half maximal inhibitory concentration doses from 0.07 to 5 mM. The binary formulations negatively affected the photosynthetic system reducing Fv/Fm values at 5 days after treatment. Lastly, the phytotoxic effect of the formulations was tested on wheat germination, and they did not inhibit plant germination and seedling growth at ≤5 mM after 14 days of application. The development of new formulations with natural compounds as bioactive ingredients would allow control of a wide spectrum of weeds through a multitarget-site effect. Full article
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<p>Multiple herbicide-resistant weed populations harvested to obtain seeds employed in the experiments: (<b>A</b>) <span class="html-italic">Amaranthus hybridus</span> in soybean crop and (<b>B</b>) <span class="html-italic">Brassica rapa</span> in oat crop.</p>
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<p>FTIR spectra of components (nonanoic acid, citral, and emulsifier) corresponding to formulation F1. The colored areas represent the bands of the oxygenated organic compound functional groups of interest: grey, OH; grey, =C-H; orange, C-H; red, C=O; and green, C-O.</p>
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<p>FTIR spectra of components (nonanoic acid, thymoquinone, and emulsifier) corresponding to formulation F2. The colored areas represent the bands of the oxygenated organic compound functional groups of interest: grey, OH; grey, =C-H; orange, C-H: red, C=O; and green, C-O.</p>
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<p>(<b>A</b>) DLS size distribution for emulsifier (E, blue), formulation 1 (F1, orange), and formulation 2 (F2, grey) at 25 (line), 35 (slashed), and 45 °C (dotted). (<b>B</b>) Temperature effect on averaged diameter (d) for emulsifier (E, blue), F1 (orange), and F2 (grey).</p>
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<p>TGA thermograms: (<b>A</b>) pure active compounds (nonanoic acid, citral, thymoquinone, and emulsifier) and (<b>B</b>) formulations (F1 and F2).</p>
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<p>Effect of binary formulation F1 and F2 on PSII on seedling of <span class="html-italic">A. hybridus</span>.</p>
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<p>Percentage of germination of wheat seeds in response to different treatments (F1, orange; F2, grey and H<sub>2</sub>O, blue) at 2 mM (<b>A</b>) and 5 mM (<b>B</b>) at 1, 7, and 14 days after application. Different letters indicate significant differences (<span class="html-italic">p</span> &lt; 0.05).</p>
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<p>Leaf growth of wheat seedlings in response to different treatments (F1, orange; F2, grey and H<sub>2</sub>O, blue) at 2 mM (<b>A</b>) and 5 mM (<b>B</b>) at 1, 7, and 14 days after application. Different letters indicate significant differences (<span class="html-italic">p</span> &lt; 0.05).</p>
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19 pages, 3206 KiB  
Article
Impact of Thermal Treatment and Aging on Lignin Properties in Spruce Wood: Pathways to Value-Added Applications
by František Kačík, Eva Výbohová, Tereza Jurczyková, Adriana Eštoková, Elena Kmeťová and Danica Kačíková
Polymers 2025, 17(2), 238; https://doi.org/10.3390/polym17020238 - 18 Jan 2025
Viewed by 300
Abstract
Thermal modification is an environmentally friendly process that does not utilize chemical agents to enhance the stability and durability of wood. The use of thermally modified wood results in a significantly extended lifespan compared with untreated wood, with minimal maintenance requirements, thereby reducing [...] Read more.
Thermal modification is an environmentally friendly process that does not utilize chemical agents to enhance the stability and durability of wood. The use of thermally modified wood results in a significantly extended lifespan compared with untreated wood, with minimal maintenance requirements, thereby reducing the carbon footprint. This study examines the impact of varying modification temperatures (160, 180, and 210 °C) on the lignin of spruce wood using the ThermoWood process and following the accelerated aging of thermally modified wood. Wet chemistry methods, including nitrobenzene oxidation (NBO), size exclusion chromatography (SEC), thermogravimetry (TG), differential thermogravimetry (DTG), and Fourier transform infrared spectroscopy (FTIR), were employed to investigate the alterations in lignin. At lower modification temperatures, the predominant reaction is the degradation of lignin, which results in a reduction in the molecular weight and an enhanced yield of NBO (vanillin and vanillic acid) products. At elevated temperatures, condensation and repolymerization reactions become the dominant processes, increasing these traits. The lignin content of aged wood is higher than that of thermally modified wood, which has a lower molecular weight and a lower decomposition temperature. The results demonstrate that lignin isolated from thermally modified wood at the end of its life cycle is a promising feedstock for carbon-based materials and the production of a variety of aromatic monomers, including phenols, aromatic aldehydes and acids, and benzene derivatives. Full article
(This article belongs to the Special Issue Advances in Applied Lignin Research)
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<p>Vanillin formation from a β-<span class="html-italic">O</span>-4 middle unit of a lignin polymer [<a href="#B12-polymers-17-00238" class="html-bibr">12</a>].</p>
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<p>Reaction scheme of the lignin β-<span class="html-italic">O</span>-4 structure during acidic pretreatment, denoting the competition between depolymerization and condensation [<a href="#B29-polymers-17-00238" class="html-bibr">29</a>].</p>
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<p>FTIR spectra of lignin isolated from untreated and thermally treated spruce wood.</p>
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<p>FTIR spectra of lignin isolated from untreated and thermally treated and aged spruce wood.</p>
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<p>Linear dependence of the vanillin content (VAN) in wood lignin on its weight average molecular weight (<span class="html-italic">M</span><sub>w</sub>).</p>
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<p>Linear dependence of the vanillin acid content (VANac) in wood lignin on its Z-average molecular weight (<span class="html-italic">M</span><sub>z</sub>).</p>
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<p>Results from GLZ (ANOVA models) for the different measures of dependence on sample and modification (models with interactions are used).</p>
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35 pages, 14202 KiB  
Article
Phase Transitions and Structural Evolution of Manganese Ores During High-Temperature Treatment
by Ruslan Z. Safarov, Yerlan A. Baikenov, Assemgul K. Zhandildenova, Eldar E. Kopishev, Ruslan M. Kamatov, Jumat B. Kargin, Henry Sanchez Cornejo, Crispin H. W. Barnes and Luis De Los Santos Valladares
Metals 2025, 15(1), 89; https://doi.org/10.3390/met15010089 (registering DOI) - 18 Jan 2025
Viewed by 169
Abstract
The aim of this research is to investigate the phase composition and structural peculiarities of complex metamorphic manganese ores from Central Kazakhstan before and after sintering in the temperature range of 600–1200 °C in an air atmosphere. X-ray diffraction, X-ray fluorescence, scanning electron [...] Read more.
The aim of this research is to investigate the phase composition and structural peculiarities of complex metamorphic manganese ores from Central Kazakhstan before and after sintering in the temperature range of 600–1200 °C in an air atmosphere. X-ray diffraction, X-ray fluorescence, scanning electron microscopy, and optical microscopy were used to analyze changes in elemental and phase composition. In their initial state, according to XRF analysis, the Bogach ore was manganese-rich, with a manganese content of 60.77 wt.%, while the Zhaksy ore contained manganese (44.88 wt.%), silicon (20.85 wt.%), and iron (6.14 wt.%) as its main components. In the Bogach ore samples, manganese content increased from 60.77% to 65.7% as the sintering temperature rose to 1100 °C, while the hausmannite phase (Mn3O4) emerged as the dominant phase, comprising 95.77% of the crystalline component at 1200 °C. Conversely, the Zhaksy ore samples displayed a sharp increase in braunite-phase (Mn7O12Si) content, reaching 83.81% at 1100 °C, alongside significant quartz amorphization. The degree of crystallinity in Bogach ore peaked at 56.2% at 900 °C but declined at higher temperatures due to amorphous phase formation. A surface morphology analysis revealed the transformation of dense, non-uniform particles into porous, granular structures with pronounced recrystallization as the temperature increased. In the Bogach samples, sintering at 900 °C resulted in elongated, needle-like crystalline formations, while at 1200 °C, tetragonal crystals of hausmannite dominated, indicating significant grain growth and recrystallization. For Zhaksy samples, sintering at 1100 °C led to a porous morphology with interconnected grains and microvoids, reflecting enhanced braunite crystallization and quartz amorphization. These findings provide quantitative insights into optimizing manganese oxide phases for industrial applications, such as catalysts and pigments, and emphasize the impact of thermal treatment on phase stability and structural properties. This research contributes to the development of efficient processing technologies for medium-grade manganese ores, aligning with Kazakhstan’s strategic goals in sustainable resource utilization. Full article
(This article belongs to the Special Issue Recent Progress in Metal Extraction and Recycling)
9 pages, 9026 KiB  
Article
Innovative Powder Pre-Treatment Strategies for Enhancing Maraging Steel Performance
by Drahomír Dvorský, David Nečas, Esther de Prado, Jan Duchoň, Petr Svora, Ondřej Ekrt, Angelina Strakošová, Jiří Kubásek and Dalibor Vojtěch
Materials 2025, 18(2), 437; https://doi.org/10.3390/ma18020437 - 18 Jan 2025
Viewed by 215
Abstract
Maraging steel is a high-performance material valued for its exceptional properties, making it ideal for demanding applications such as aerospace, tooling, and automotive industries, where high strength, toughness, and precision are required. These steels can be prepared by powder metallurgy techniques, which offer [...] Read more.
Maraging steel is a high-performance material valued for its exceptional properties, making it ideal for demanding applications such as aerospace, tooling, and automotive industries, where high strength, toughness, and precision are required. These steels can be prepared by powder metallurgy techniques, which offer new processing possibilities. This paper introduces novel thermal powder pre-treatment and its impact on the final mechanical properties. Solid solution pre-treatment results in a modest improvement in strength (from 972 MPa to 1000 MPa), while the use of pre-aged powder achieves the highest strength (1316 MPa) and lowest ductility (2.6%). A self-composite material is created by mixing pre-treated powders with the same chemical composition but different properties. Such material was characterized by intermediate strength (1174 MPa) and ductility (3.1%). Although challenges such a porosity and oxidation were present, this approach allows for tuning of mechanical properties by mixing pre-treated powders, offering significant potential for advanced engineering applications. Full article
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<p>SEM micrographs of (<b>A</b>) atomized powder (AP), (<b>B</b>) solid solution-treated powder (T4), (<b>C</b>) aged powder (T6), (<b>D</b>) XRD patterns in logarithmic scale. The patterns have been vertically shifted for better visualization and converted to Cu radiation to facilitate comparison with the bibliography.</p>
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<p>(<b>A</b>) Surface of sample after SPS showing layer of C penetration (optical microscopy), (<b>B</b>) SEM image and corresponding EDS analysis of T4 sample.</p>
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<p>OM micrographs of compact samples from (<b>A</b>) atomized powder (AP), (<b>B</b>) solid solution-treated powder (T4), (<b>C</b>) aged powder (T6), (<b>D</b>) mix of T4 and T6 powder.</p>
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<p>STEM images of (<b>A</b>) AP sample, (<b>B</b>) T4 sample, (<b>C</b>) T6 sample, and EDS analysis of oxides.</p>
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<p>(<b>A</b>) Tensile (dashed line) and (<b>B</b>) compressive (solid line) curves of prepared materials.</p>
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17 pages, 18811 KiB  
Article
Safe Treatment of Surface Coalfield Fires Above Shallow-Buried Goaf in Steeply Dipping Coal Seams
by Pihong Zhang, Ruchang Chen, Guoqing Zhu, Dezhi Yang, Xin Li, Wei Jiang, Hao Liu and Zhiyi Zhang
Fire 2025, 8(1), 33; https://doi.org/10.3390/fire8010033 - 18 Jan 2025
Viewed by 279
Abstract
Xinjiang is a region of China that suffers severe energy resource loss and air pollution resulting from long-term coalfield fires in near-surface inclined coal seams. Beneath these fire areas, abandoned mined-out goaf is common. Accidents easily occur during the treatment of such fire [...] Read more.
Xinjiang is a region of China that suffers severe energy resource loss and air pollution resulting from long-term coalfield fires in near-surface inclined coal seams. Beneath these fire areas, abandoned mined-out goaf is common. Accidents easily occur during the treatment of such fire areas owing to the instability of strata overlying the goaf. Here, we carried out non-destructive exploration of the goaf below a fire area using the airborne transient electromagnetic method, accurately identifying the locations and sizes of 21 goaf areas. We then established a stratigraphic model using the thermal-solid coupling function in UDEC software. Our simulations showed that under the combined action of high temperature generated by coal combustion and high pressure generated by fire-fighting machinery, the maximum displacement and vertical stress in strata overlying the goaf were 1.42 m and 36 MPa, respectively. Such large displacement and stress values inevitably lead to the destabilization of overlying strata via turning, sliding, and tipping, seriously threatening the safety of mining personnel and machinery. In the field, the rock layer above the goaf was first accurately blasted, and then fire extinguishing was carried out after the overlying rock had collapsed and compacted. Full article
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<p>Distribution of coalfield fires in Xinjiang region of China (<b>a</b>); structural profile shallow-buried goaf (<b>b</b>).</p>
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<p>Topography of the prospecting area. (<b>a</b>) Topography; (<b>b</b>) Construction situation.</p>
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<p>Schematic diagram of the airborne transient electromagnetic measurement. (<b>a</b>) Principle for goaf exploration; (<b>b</b>) Field work drawing.</p>
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<p>Airborne transient electromagnetic measurement line layout.</p>
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<p>Rock mechanics experimental process of overlying strata.</p>
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<p>Schematic numerical model diagrams. (<b>a</b>) Basic numerical model; (<b>b</b>) Pressure and temperature loading.</p>
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<p>Abnormal area apparent resistivity contour maps.</p>
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<p>Experimental results of thermal properties: (<b>a</b>) Specific heat capacity; (<b>b</b>) Thermal conductivity; (<b>c</b>) Tensile strength; (<b>d</b>) Elastic modulus.</p>
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<p>Rock strata movement in a fire area. (<b>a</b>) Without the effect of the temperature field; (<b>b</b>) With the effect of the temperature field; (<b>c</b>) With the effect of stress and temperature field.</p>
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<p>Subsidence curves of overlying strata.</p>
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<p>Vertical stress distribution cloud maps. (<b>a</b>) Without the effect of the temperature field; (<b>b</b>) With the effect of the temperature field; (<b>c</b>) Temperature field-load interaction.</p>
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<p>Vertical stress distribution of goaf roof. (<b>a</b>) Left goaf roof; (<b>b</b>) Right goaf roof.</p>
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<p>Diagram of stability evaluation of the rock overlying a goaf (A, B, C, D are the four inflection points of the shape of goaf roof strata).</p>
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<p>Borehole layout. (<b>a</b>) Planar profile; (<b>b</b>) Dip profile.</p>
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<p>Site construction management flow chart. (<b>a</b>) Injecting water into the surface of the fire area; (<b>b</b>) Stripping and leveling; (<b>c</b>) Water injection in fish-scale-like pits; (<b>d</b>) Transporting soil for compaction.</p>
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21 pages, 7804 KiB  
Article
In Situ X-Ray Study During Thermal Cycle Treatment Combined with Complementary Ex Situ Investigation of InGaN Quantum Wells
by Ewa Grzanka, Sondes Bauer, Artur Lachowski, Szymon Grzanka, Robert Czernecki, Byeongchan So, Tilo Baumbach and Mike Leszczyński
Nanomaterials 2025, 15(2), 140; https://doi.org/10.3390/nano15020140 - 17 Jan 2025
Viewed by 344
Abstract
In situ X-ray reciprocal space mapping was performed during the interval heating and cooling of InGaN/GaN quantum wells (QWs) grown via metal–organic vapor phase epitaxy (MOVPE). Our detailed in situ X-ray analysis enabled us to track changes in the peak intensities and radial [...] Read more.
In situ X-ray reciprocal space mapping was performed during the interval heating and cooling of InGaN/GaN quantum wells (QWs) grown via metal–organic vapor phase epitaxy (MOVPE). Our detailed in situ X-ray analysis enabled us to track changes in the peak intensities and radial and angular broadenings of the reflection. By simulating the radial diffraction profiles recorded during the thermal cycle treatment, we demonstrate the presence of indium concentration distributions (ICDs) in the different QWs of the heterostructure (1. QW, bottom, 2. QW, middle, and 3. QW, upper). During the heating process, we found that the homogenization of the QWs occurred in the temperature range of 850 °C to 920 °C, manifesting in a reduction in ICDs in the QWs. Furthermore, there is a critical temperature (T = 940 °C) at which the mean value of the indium concentration starts to decrease below 15% in 1. QW, indicating the initiation of decomposition in 1. QW. Moreover, further heating up to 1000 °C results in extended diffuse scattering along the angular direction of the diffraction spot, confirming the propagation of the decomposition and the formation of trapezoidal objects, which contain voids and amorphous materials (In-Ga). Heating InGaN QWs up to T = 1000 °C led to a simultaneous decrease in the indium content and ICDs. During the cooling phase, there was no significant variation in the indium concentrations in the different QWs but rather an increase in the defect area, which contributes to the amplification of diffuse scattering. A comparison of ex situ complementary high-resolution transmission microscopy (Ex-HRTEM) measurements performed at room temperature before and after the thermal cycle treatment provides proof of the formation of four different types of defects in the QWs, which result from the decomposition of 1. QW during the heating phase. This, in turn, has strongly influenced the intensity of the photoluminescence emission spectra without any detectable shift in the emission wavelength λMQWs. Full article
(This article belongs to the Section Synthesis, Interfaces and Nanostructures)
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<p>(<b>a</b>) Layout of the InGaN QW sample. (<b>b</b>) Example of the reciprocal space map for the (0004) reflection showing the GaN(0004) reflection and the InGaN satellite peaks, where the full angular broadening (<span class="html-italic">FW<sub>ang</sub></span>) and radial full-width half-maximum (<span class="html-italic">FWHM<sub>rad</sub></span>) are illustrated by a horizontal black dashed line and vertical magenta line, respectively. (<b>c</b>) RSMs recorded during the heating and cooling phases with the indication of annealing time <span class="html-italic">t<sub>A</sub></span> and the acquisition time <span class="html-italic">t<sub>M</sub></span>. (<b>d</b>) Schematic presentation of the in situ X-ray diffraction set-up including the hexapod for mounting and aligning the sample and the one-dimensional Mythen detector.</p>
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<p>(<b>a</b>) Comparison of the radial diffraction profiles as a function measured during the heating phase at <span class="html-italic">T<sub>RT</sub></span>, <span class="html-italic">T</span><sub>700</sub>, <span class="html-italic">T</span><sub>800</sub>, <span class="html-italic">T</span><sub>900</sub>, <span class="html-italic">T</span><sub>920</sub>, <span class="html-italic">T</span><sub>940</sub>, <span class="html-italic">T</span><sub>960</sub>, <span class="html-italic">T</span><sub>980</sub>, and <span class="html-italic">T</span><sub>1000</sub>. The XRD profile of <span class="html-italic">T<sub>RT</sub></span> was rescaled along the X-axis. The inset corresponds to the radial profile of satellite peak SL3, indicated by a dashed square. (<b>b</b>) Variation in the full-width half-maximum <span class="html-italic">FWHM<sub>rad</sub>_SL3</span> (left axis) and the area of satellite peak SL3 <span class="html-italic">Area<sub>rad</sub>_SL3</span> (right axis) with the temperature.</p>
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<p>(<b>a</b>) Variation in the area of the radial profiles <span class="html-italic">Area<sub>rad</sub></span> corresponding to all satellites recorded during the heating phase. (<b>b</b>) The area ratio <span class="html-italic">A<sub>T</sub>/A<sub>RT</sub></span> at different temperatures <span class="html-italic">A<sub>T</sub></span> with respect to room temperature <span class="html-italic">A<sub>RT</sub></span> as a function of the satellite peak order.</p>
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<p>(<b>a</b>,<b>b</b>) Variation in radial <span class="html-italic">FWHM<sub>rad</sub></span> and angular broadening <span class="html-italic">FW<sub>ang</sub></span> with the temperature, respectively, during the heating phase for all satellite peaks.</p>
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<p>(<b>a</b>) Comparison of the radial diffraction profiles as a function measured during the cooling phase from <span class="html-italic">T<sub>c</sub></span><sub>1000</sub> to <span class="html-italic">T<sub>cRT</sub></span>. The XRD profile of <span class="html-italic">T<sub>cRT</sub></span> was rescaled along the X-axis. The inset corresponds to the radial profile of SL3, as indicated by a dashed square. (<b>b</b>) Variation in peak area <span class="html-italic">Area<sub>rad</sub>_SL</span> of the radial profiles of all satellites with the temperature recorded during the cooling phase.</p>
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<p>(<b>a</b>,<b>b</b>) Variation in the radial <span class="html-italic">FWHM<sub>rad</sub></span> and the angular broadening <span class="html-italic">FW<sub>ang</sub></span> with the temperature, respectively, during the cooling phase for the different satellite peaks.</p>
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<p>Plots (<b>a</b>–<b>e</b>) compare the radial diffraction profiles recorded during the heating and the cooling phases of the thermal cycle treatment at specific temperatures, such as <span class="html-italic">T</span> = 980 °C, 960 °C, 920 °C, 700 °C, and <span class="html-italic">RT</span>, respectively. (<b>f</b>) Variation in the radial peak area <span class="html-italic">Area<sub>rad</sub>_SL</span> with the temperature T during the complete thermal cycle treatment for higher-order satellite peaks SL3, SL4, and SL5.</p>
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<p>(<b>a</b>) The variation in the percentage loss <span class="html-italic">(A<sub>T</sub>-A<sub>Tc</sub>)*</span>100<span class="html-italic">/A<sub>T</sub></span> of diffracted peak intensities of all satellites with the temperature; (<b>b</b>) variation in the angular broadening <span class="html-italic">FW<sub>ang</sub></span> with temperature T during the complete thermal cycle treatment for all satellite peaks; (<b>c</b>) variation in the radial broadening <span class="html-italic">FWHM<sub>rad</sub></span> as a function of the temperature for SL3; (<b>d</b>) variation in the indium concentration <span class="html-italic">χ<sub>In</sub></span> [%] of 1. QW, 2. QW, and 3. QW with temperature during the heating (<b>e</b>) and cooling phases of the thermal cycle treatment. (<b>f</b>) Dependence of indium mean value concentration &lt;χ<sub>In</sub>&gt; on the temperature of 1. QW, 2. QW, and 3. QW during the thermal cycle treatment. Ranges: <span class="html-italic">R</span>1 = 30%&lt; <span class="html-italic">χ<sub>In</sub></span> &lt; 40%; <span class="html-italic">R</span>2 = 20%&lt; <span class="html-italic">χ<sub>In</sub></span> &lt; 30%; <span class="html-italic">R</span>3 = 14%&lt; <span class="html-italic">χ<sub>In</sub></span> &lt; 20%; <span class="html-italic">R</span>4 = 0%&lt; <span class="html-italic">χ<sub>In</sub></span> &lt; 14%. The vertical discontinuous blue lines refer to <span class="html-italic">T<sub>RT</sub></span>, <span class="html-italic">T</span><sub>940</sub>, <span class="html-italic">T</span><sub>1000</sub>, <span class="html-italic">T<sub>c</sub></span><sub>940</sub>, and <span class="html-italic">T<sub>cRT</sub></span>.</p>
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<p>Reciprocal space maps of (0004) reflection of the InGaN heterostructure at (<b>a1</b>) <span class="html-italic">T<sub>RT</sub></span>, (<b>b2</b>) <span class="html-italic">T</span><sub>940</sub>, (<b>c2</b>) <span class="html-italic">T</span><sub>980</sub>, (<b>d2</b>) <span class="html-italic">T</span><sub>1000</sub>, (<b>e2</b>) <span class="html-italic">T<sub>c</sub></span><sub>940</sub>, and (<b>f1</b>) <span class="html-italic">T<sub>cRT</sub></span>. (<b>a2</b>) STEM image (left) together with indium concentration map (right) for InGaN QWs at <span class="html-italic">T<sub>RT</sub></span>; (<b>f2</b>) STEM image for InGaN QWs at <span class="html-italic">T<sub>cRT</sub></span>, schematic presentation of the indium concentration distribution (ICD) given by ranges <span class="html-italic">R</span>1 = 30% &lt; <span class="html-italic">χ<sub>in</sub></span> &lt; 40%, <span class="html-italic">R</span>2 = 20% &lt; <span class="html-italic">χ<sub>in</sub></span> &lt; 30%, <span class="html-italic">R</span>3 = 14% &lt; <span class="html-italic">χ<sub>in</sub></span> &lt; 20%, and <span class="html-italic">R</span>4 = <span class="html-italic">χ<sub>in</sub></span> &lt; 14% for 1. QW, 2. QW, and 3. QW at (<b>a3</b>) <span class="html-italic">T<sub>RT</sub></span>, (<b>b1</b>) <span class="html-italic">T</span><sub>940</sub>, (<b>c1</b>) <span class="html-italic">T</span><sub>980</sub>, (<b>d1</b>) <span class="html-italic">T</span><sub>1000</sub>, (<b>e1</b>) <span class="html-italic">T<sub>c</sub></span><sub>940</sub>, and (<b>f3</b>) <span class="html-italic">T<sub>cRT</sub></span>, together with illustrations of the defect indicated by trapezoid-shaped objects.</p>
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<p>STEM images of QW heterostructures corresponding to (<b>a</b>) T<sub>RT</sub> after the MOVPE growth and (<b>b</b>) at T<sub>cRT</sub> after thermal cycle treatment; the scale bar is 50 nm. (<b>c1</b>) Indium concentration map with a size of 100 × 100 nm in InGaN QW heterostructures derived from STEM at T<sub>RT</sub> prior to the thermal cycle treatment, (<b>c2</b>) the indium concentration &lt;χ<sub>In-STEM</sub>&gt; profiles derived from the map of (<b>c1</b>), and (<b>c3</b>) &lt;χ<sub>In-STEM</sub>&gt; profiles of 1. QW corresponding to the dashed box in (<b>c2</b>) and showing the presence of an indium concentration distribution (ICD) in the individual QWs.</p>
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<p>TEM images of different types of defects in 1. QW at T<sub>cRT</sub> corresponding to different locations of the QW. (<b>a</b>) Types I and II are highlighted by green and orange boxes, respectively. (<b>b</b>) Defect type III is indicated by a red box and (<b>c</b>) defect type IV is indicated by a blue box. The corresponding HRTEMs of different defect types: (<b>d</b>) type I of the green box, (<b>e</b>) type II of the orange box, (<b>f</b>) type III of the red box, and (<b>g</b>) type IV of the blue box.</p>
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<p>Comparison of the emission spectra of the InGaN QW heterostructures recorded before and after the thermal cycle treatment T<sub>RT</sub> and T<sub>cRT</sub>, respectively.</p>
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14 pages, 2012 KiB  
Article
Changes in the Flavor of Cold-Pressed Tiger Nut Oil (Cyperus esculentus L.) During Refining Processes and Evaluation of Its Thermal Properties
by Yue Zhao, Yang Sun, Heyi Sun, Tianying Sun, Jian Ren and Chunli Song
Foods 2025, 14(2), 301; https://doi.org/10.3390/foods14020301 - 17 Jan 2025
Viewed by 374
Abstract
Oil extracted from tiger nut is a good, edible source owing to its richness in unsaturated fatty acids. This study investigated the effects of the refining processes on the flavor components of crude tiger nut oil by GC-MS and focused on the thermal [...] Read more.
Oil extracted from tiger nut is a good, edible source owing to its richness in unsaturated fatty acids. This study investigated the effects of the refining processes on the flavor components of crude tiger nut oil by GC-MS and focused on the thermal stability of the refined oil under high-temperature conditions. Three different refining processes were evaluated: citric acid-assisted hydration degumming, alkali deacidification and bleaching. In the present study, the neutralization refining resulted in 11.67% losses. The refined oil had higher brightness and transparency. Moreover, 109 volatiles were identified, mainly including aldehydes, alcohols, pyrazines and furans, the characteristic flavor compounds of which present a fatty, fresh and nutty flavor. Hence, the refining processes have a significant effect on the flavor components of tiger nut oil, and the accumulated information can be helpful in increasing the tiger nut oil quality to meet the market value. The results of the thermal properties indicated the significant degradation of oleic acid and linoleic acid with prolonged heating, leading to increases in the acid value by 17 times and the peroxide value by 31 times after prolonged heating at 210 °C for 10 h compared with those without heating. When the refined tiger nut oil was heated at 210 °C for 4 h, the carbonyl value (62.6 meq/kg) exceeded the recommended value, and after heating for 8 h, the total polar compound percentages (50%, the instrument limit value) also exceeded the national standard. In order to extend the cooking heating time, it is necessary to appropriately decrease the heating temperature. This study provides a scientific reference for the frying of tiger nut oil in food and the high-temperature treatment of food containing tiger nut oil. Full article
(This article belongs to the Section Food Engineering and Technology)
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Figure 1

Figure 1
<p>The oil yield and oil loss rate of the tiger nut oil in different refining processes.</p>
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<p>The sensory color of the tiger nut oil in refining processes. A: crude tiger nut oil, B: degummed tiger nut oil, C: neutralized tiger nut oil, D: bleached tiger nut oil.</p>
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<p>Total number and numbers of common and differential volatile compounds of different refined oils.</p>
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<p>Variety and content changes of volatile compounds in the tiger nut oil during refining processes. (<b>a</b>) Component number, (<b>b</b>) volatile compounds.</p>
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<p>Clustering heat map of volatile compounds in refined tiger nut oils.</p>
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<p>The thermal characteristics of the refined tiger nut oil. (<b>a</b>): carbonyl value, (<b>b</b>): polar compound content. Different letters (a–f) in the same column are significantly different (<span class="html-italic">p</span> &lt; 0.05).</p>
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