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22 pages, 6314 KiB  
Article
Design and Optimization of W-Mo-V High-Speed Steel Roll Material and Its Heat-Treatment-Process Parameters Based on Numerical Simulation
by Zhiting Zhu, Mingyu Duan, Hao Pi, Zhuo Li, Jibing Chen and Yiping Wu
Materials 2025, 18(1), 34; https://doi.org/10.3390/ma18010034 (registering DOI) - 25 Dec 2024
Abstract
W-Mo-V high-speed steel (HSS) is a high-alloy high-carbon steel with a high content of carbon, tungsten, chromium, molybdenum, and vanadium components. This type of high-speed steel has excellent red hardness, wear resistance, and corrosion resistance. In this study, the alloying element ratios were [...] Read more.
W-Mo-V high-speed steel (HSS) is a high-alloy high-carbon steel with a high content of carbon, tungsten, chromium, molybdenum, and vanadium components. This type of high-speed steel has excellent red hardness, wear resistance, and corrosion resistance. In this study, the alloying element ratios were adjusted based on commercial HSS powders. The resulting chemical composition (wt.%) is C 1.9%, W 5.5%, Mo 5.0%, V 5.5%, Cr 4.5%, Si 0.7%, Mn 0.55%, Nb 0.5%, B 0.2%, N 0.06%, and the rest is Fe. This design is distinguished by the inclusion of a high content of molybdenum, vanadium, and trace boron in high-speed steel. When compared to traditional tungsten-based high-speed steel rolls, the addition of these three types of elements effectively improves the wear resistance and red hardness of high-speed steel, thereby increasing the service life of high-speed steel mill-roll covers. JMatPro (version 7.0) simulation software was used to create the composition of W-Mo-V HSS. The phase composition diagrams at various temperatures were examined, as well as the contents of distinct phases within the organization at various temperatures. The influence of austenite content on the martensitic transformation temperature at different temperatures was estimated. The heat treatment parameters for W-Mo-V HSS were optimized. By studying the phase equilibrium of W-Mo-V high-speed steel at different temperatures and drawing CCT diagrams, the starting temperature for the transformation of pearlite to austenite (Ac1 = 796.91 °C) and the ending temperature for the complete dissolution of secondary carbides into austenite (Accm = 819.49 °C) during heating was determined. The changes in carbide content and grain size of W-Mo-V high-speed steel at different tempering temperatures were calculated using JMatPro software. Combined with analysis of Ac1 and Accm temperature points, it was found that the optimal annealing temperatures were 817–827 °C, quenching temperatures were 1150–1160 °C, and tempering temperatures were 550–610 °C. The scanning electron microscopy (SEM) examination of the samples obtained with the aforementioned heat treatment parameters revealed that the martensitic substrate and vanadium carbide grains were finely and evenly scattered, consistent with the simulation results. This suggests that the simulation is a useful reference for guiding actual production. Full article
(This article belongs to the Special Issue Advanced Materials: Process, Properties, and Applications)
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Figure 1

Figure 1
<p>(<b>a</b>) Effect of carbon content in austenite on the amount of residual austenite; (<b>b</b>) effect of carbon content in austenite on martensitic transformation temperature [<a href="#B37-materials-18-00034" class="html-bibr">37</a>].</p>
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<p>Equilibrium-phase diagrams of Fe-5.5W-5.0Mo-5.5V-4.5Cr-0.7Si-0.55Mn-0.5Nb-0.2B-0.06N-1.9C high-speed steels at different temperatures (the numbers indicate weight percent).</p>
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<p>Analysis of elemental content in HSS Fe-5.5W-5.0Mo-5.5V-4.5Cr-0.7Si-0.55Mn-0.5Nb-0.2B-0.06N-1.9C: (<b>a</b>) elemental content in ferrite; (<b>b</b>) elemental content in austenite.</p>
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<p>Analysis of the content of different carbides in Fe-5.5W-5.0Mo-5.5V-4.5Cr-0.7Si-0.55Mn-0.5Nb-0.2B-0.06N-1.9C high-speed steel. (<b>a</b>) Elemental content in MN; (<b>b</b>) elemental content in M (C, N); (<b>c</b>) elemental content in M<sub>6</sub>C; (<b>d</b>) elemental content in M<sub>23</sub>C<sub>6</sub>.</p>
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<p>Analysis of elemental content in M<sub>3</sub>B<sub>2</sub> borides in Fe-5.5, W-5.0Mo-5.5V-4.5Cr-0.7Si-0.55Mn-0.5Nb-0.2B-0.06N-1.9C high-speed steel.</p>
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<p>Schematic diagram of several spheroidal annealing processes for alloy steels.</p>
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<p>Carbon content of austenite at different temperatures.</p>
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<p>Fe-5.5W-5.0Mo-5.5V-4.5Cr-0.7Si-0.55Mn-0.5Nb-0.2B-0.06N-1.9C. Variation of carbide content of each carbide with the tempering time at different tempering temperatures of high-speed steels: (<b>a</b>) 550 °C; (<b>b</b>) 580 °C; (<b>c</b>) 610 °C; (<b>d</b>) 640 °C; (<b>e</b>) 670 °C; (<b>f</b>) 700 °C; (<b>g</b>) 730 °C; (<b>h</b>) 760 °C.</p>
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<p>Fe-5.5W-5.0Mo-5.5V-4.5Cr-0.7Si-0.55Mn-0.5Nb-0.2B-0.06N-1.9C. Variation of carbide grain size with tempering time in high-speed steels at different tempering temperatures: (<b>a</b>) 550 °C; (<b>b</b>) 580 °C; (<b>c</b>) 610 °C; (<b>d</b>) 640 °C; (<b>e</b>) 670 °C; (<b>f</b>) 700 °C; (<b>g</b>) 730 °C; (<b>h</b>) 760 °C.</p>
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<p>SEM photos after quenching at different temperatures. (<b>a</b>) 1180 °C × 100; (<b>b</b>) 1160 °C × 100.</p>
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<p>Strength of W-Mo-V high-speed steels at different temperatures.</p>
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13 pages, 1580 KiB  
Article
Effect of Process Pressure on the Properties of Cu2O Thin Films Deposited by RF Magnetron Sputtering
by Junghwan Park, Chang-Sik Son, Young-Guk Son and Donghyun Hwang
Crystals 2025, 15(1), 2; https://doi.org/10.3390/cryst15010002 - 24 Dec 2024
Abstract
Cu2O thin films were deposited on soda-lime glass substrates using RF magnetron sputtering under various process pressures, and their structural, morphological, compositional, and optical properties were investigated. X-ray diffraction (XRD) revealed that the films crystallized in the cubic Cu2O [...] Read more.
Cu2O thin films were deposited on soda-lime glass substrates using RF magnetron sputtering under various process pressures, and their structural, morphological, compositional, and optical properties were investigated. X-ray diffraction (XRD) revealed that the films crystallized in the cubic Cu2O phase, with the highest crystallinity observed at 5 mTorr, as evidenced by the sharp and intense (111) peak. Raman spectroscopy confirmed the predominance of Cu2O vibrational modes across all samples, with improved phase purity and crystallinity at 5 mTorr and 10 mTorr. Field-emission scanning electron microscopy (FE-SEM) showed that the films deposited at 5 mTorr and 10 mTorr exhibited densely packed, well-defined grains, while those at 1 mTorr and 15 mTorr displayed irregular or poorly defined morphologies. X-ray photoelectron spectroscopy (XPS) confirmed the presence of Cu(I) without significant secondary phases, with slight surface oxidation observed at higher pressures. Optical characterization revealed that transmittance increased with pressure, reaching ~90% in the NIR range at 15 mTorr. The optical band gap (Eg) values increased from 2.34 eV at 1 mTorr to 2.43 eV at 15 mTorr with higher process pressure. Cu2O films deposited at 5 mTorr and 10 mTorr exhibited an optimal balance between high transparency and band gap values. These findings highlight the critical role of process pressure in determining the properties of Cu2O thin films and identify 5 mTorr as the optimal deposition condition for achieving high-quality films with superior structural and optical performance. Full article
(This article belongs to the Section Materials for Energy Applications)
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Figure 1
<p>XRD patterns of the Cu<sub>2</sub>O thin films deposited under various process pressures.</p>
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<p>Raman spectra of the Cu<sub>2</sub>O thin films deposited under different process pressures.</p>
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<p>FE-SEM images of the Cu<sub>2</sub>O thin films deposited under different process pressures.</p>
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<p>XPS analysis of the Cu<sub>2</sub>O thin films deposited at different process pressures: (<b>a</b>) survey spectra showing Cu 2p, O 1s, and C 1s peaks, (<b>b</b>) high-resolution Cu 2p spectra confirming the presence of Cu(I) in the Cu<sub>2</sub>O phase, and (<b>c</b>) O 1s spectra illustrating the oxygen bonding states in the Cu<sub>2</sub>O structure.</p>
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<p>Optical properties of the Cu<sub>2</sub>O thin films deposited under various process pressures: (<b>a</b>) transmittance spectra showing transparency variations and (<b>b</b>) Tauc plots estimating the optical band gaps.</p>
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14 pages, 3394 KiB  
Article
Enhanced Diclofenac Removal from Constructed Wetland Effluent Using a Photoelectrocatalytic System with N-TiO2 Nanocrystal-Modified TiO2 Nanotube Anode and Graphene Oxide/Activated Carbon Photocathode
by Xiongwei Liang, Shaopeng Yu, Bo Meng, Xiaodi Wang, Chunxue Yang, Chuanqi Shi and Junnan Ding
Catalysts 2024, 14(12), 954; https://doi.org/10.3390/catal14120954 - 23 Dec 2024
Abstract
This investigation reports on the efficacy of a photoelectrocatalysis (PEC) system enhanced by a nitrogen-doped TiO2 nanocrystal-modified TiO2 nanotube array (N-TiO2 NCs/TNTAs) anode paired with a graphene oxide/activated carbon (GO/AC) photocathode for diclofenac removal from effluent. The FE-SEM and EDX [...] Read more.
This investigation reports on the efficacy of a photoelectrocatalysis (PEC) system enhanced by a nitrogen-doped TiO2 nanocrystal-modified TiO2 nanotube array (N-TiO2 NCs/TNTAs) anode paired with a graphene oxide/activated carbon (GO/AC) photocathode for diclofenac removal from effluent. The FE-SEM and EDX analyses validated the elemental composition of the anode—27.56% C, 30.81% N, 6.03% O, and 26.49% Ti. The XRD results confirmed the anatase phase and nitrogen integration, essential for photocatalytic activity enhancement. Quantum chemical simulations provided a comprehensive understanding of the red-shifted absorption bands in N-TiO2, and UV-vis DRS demonstrated a red-shift in absorption to the visible spectrum, indicating improved light utilization. The PEC configuration achieved a photocurrent density of 9.8 mA/dm2, significantly higher than the unmodified and solely nitrogen-doped counterparts at 4.8 mA/dm2 and 6.1 mA/dm2, respectively. Notably, this system reduced diclofenac concentrations by 58% within 75 min, outperforming standard photocatalytic setups. These findings underscore the potential of N-TiO2 NCs/TNTAs-AC-GO/PTFE composite material for advanced environmental photoelectrocatalytic applications. Full article
(This article belongs to the Special Issue Nanomaterials in Environmental Catalysis)
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Figure 1

Figure 1
<p>FE-SEM images of graphene oxide (<b>a</b>), active carbon (<b>b</b>), N-TiO<sub>2</sub> NCs/TNTAs (<b>c</b>), N-TiO<sub>2</sub> NCs (<b>d</b>) N-TiO<sub>2</sub> NCs/TNTAs—AC-GO/PTFE composite material (<b>e</b>), and EDX analysis of N-TiO<sub>2</sub> NCs/TNTAs—AC-GO/PTFE (<b>f</b>).</p>
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<p>XRD patterns of TiO<sub>2</sub> NTs and N-TiO<sub>2</sub> NCs/TNTAs.</p>
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<p>Absorption spectrum curves of TiO<sub>2</sub> and N-TiO<sub>2</sub>.</p>
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<p>Absorption spectrum curves of TiO<sub>2</sub> and GO.</p>
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<p>DRS of TiO<sub>2</sub> NCs/TiO<sub>2</sub> NTs, N-TiO<sub>2</sub> NCs/TiO<sub>2</sub> NTs, and N-TiO<sub>2</sub> NCs/TiO<sub>2</sub> NTs-AC-GO/PTFE.</p>
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<p>The results of photoelectron catalytic system and photocatalytic system on the fluorescence intensity.</p>
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<p>Transient photocurrent responses of TiO<sub>2</sub> NCs/TiO<sub>2</sub> NTs, N-TiO<sub>2</sub> NCs/TiO<sub>2</sub> NTs, and N-TiO<sub>2</sub> NCs/TiO<sub>2</sub> NTs-AC-GO/PTFE.</p>
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<p>Degradation results of diclofenac under photocatalysis and photoelectrocatalysis.</p>
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<p>The proposed photocatalytic mechanism of the N-TiO<sub>2</sub> NCs/TiO<sub>2</sub> NTs-AC-GO photoelectrode.</p>
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39 pages, 28889 KiB  
Article
Pyrochlore-Supergroup Minerals and Their Relation to Columbite-Group Minerals in Peralkaline to Subaluminous A-Type Rare-Metal Granites with Special Emphasis on the Madeira Pluton, Amazonas, Brazil
by Karel Breiter, Hilton Tulio Costi and Zuzana Korbelová
Minerals 2024, 14(12), 1302; https://doi.org/10.3390/min14121302 (registering DOI) - 23 Dec 2024
Abstract
Niobium (Nb) and tantalum (Ta) are quoted as “strategic” or “critical” elements for contemporaneous society. The main sources of Nb and Ta are minerals of the pyrochlore supergroup (PSGM) and the columbite group (CGM) mined from different magmatic lithologies. Textures and chemical compositions [...] Read more.
Niobium (Nb) and tantalum (Ta) are quoted as “strategic” or “critical” elements for contemporaneous society. The main sources of Nb and Ta are minerals of the pyrochlore supergroup (PSGM) and the columbite group (CGM) mined from different magmatic lithologies. Textures and chemical compositions of PSGM and CGM often provide key information about the origin of NbTa mineralization. Therefore, we decided to carry out a detailed study of the relations between the PSGM and CGM and their post-magmatic transformations, and the Madeira peralkaline pluton (Brazil) is an ideal object for such a study. Textures of the PSGM and CGM were studied using BSE imaging and SEM mapping, and their chemical compositions were determined using 325 electron microprobe analyses. Pyrochlore from the Madeira granite can be chemically characterized as Na, Ca-poor, U- and Pb-dominant, and Sn- and Zn-enriched; REE are enriched only during alteration. Two stages of alteration are present: (i) introduction of Fe + Mn, with the majority of them consumed by columbitization; (ii) introduction of Si and Fe, and in lesser amounts also Pb and U: Si, Pb, and U incorporated into pyrochlore, iron forming Fe-oxide halos around pyrochlore. During both stages, F and Na decreased. In the case of a (nearly) complete pyrochlore columbitization, U and Th were exsolved to form inclusions of a thorite/coffinite-like phase. In contrast to altered pyrochlores from other localities, pyrochlore from Madeira shows a relatively high occupancy of the A-site. Although Madeira melt was Na-, F-rich, contemporaneous crystallization of cryolite consumed both elements and pyrochlore was, from the beginning, relatively Na-, F-poor. Full article
(This article belongs to the Special Issue Rare-Metal Granites)
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Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>Textures of the studied types of Madeira granites by automated mineralogy (TIMA): (<b>a</b>) hypersolvus granite; (<b>b</b>) core albite granite; (<b>c</b>) border albite granite. Explanation: dark blue—quartz, red—K-feldspar, light blue—albite, orange—fluorite, yellow—Li-mica, green—cryolite.</p>
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<p>Whole-rock geochemical characteristic of the studied rare-metal granites: (<b>a</b>) aluminum saturation index (ASI = Al/(Na + K + 0.5Ca) mol) vs. Nb/Ta (by weight); (<b>b</b>), Nb vs. Ta by weight; (<b>c</b>), U vs. Th by weight; (<b>d</b>), Pb vs. Zn by weight. Data from Raimbault et al. [<a href="#B48-minerals-14-01302" class="html-bibr">48</a>] (Beauvoir), Badanina et al. [<a href="#B36-minerals-14-01302" class="html-bibr">36</a>] (Orlovka), and authors’ data (Madeira, Cínovec and Podlesí). Values for deeper crust from Rudnick and Gao [<a href="#B59-minerals-14-01302" class="html-bibr">59</a>].</p>
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<p>Back-scattered electron images (BSE) of pyrochlore crystals from the Madeira pluton. Fresh or only very slightly altered examples (type 1 pyrochlore): (<b>a</b>) an almost fresh homogeneous pyrochlore crystal associated with crystals of hematite (dark gray) in the cryolite-albite matrix (black), Madeira albite granite core facies (#PHR247, crystal 4); (<b>b</b>) a distinctly zoned pyrochlore crystal in darker zones starting to transform into columbite-Fe, Madeira albite granite core facies (#PHR 159, crystal 1); (<b>c</b>) a zoned pyrochlore crystal associated with zircon (dark gray) with overgrowths of columbite, Madeira albite granite core facies (#PHR 160, crystal 3); (<b>d</b>) a zoned pyrochlore crystal with overgrowths of columbite, Madeira albite granite core facies (#PHR 163, crystal 3). Type 2 pyrochlore: (<b>e</b>) an inhomogeneously zoned pyrochlore crystal with Pb-enriched (bright) domains and a thin veinlet of secondary columbite (dark), Madeira albite granite core facies (#PHR 242, crystal 7); (<b>f</b>) a distinctly zoned pyrochlore crystal starting to transform into columbite –Fe along cracks, Madeira albite granite core facies (#PHR 82A, crystal 7). Red numbers refer to EPMA analyses of pyrochlore (compare <a href="#minerals-14-01302-t001" class="html-table">Table 1</a>), and yellow numbers to analyses of columbite (compare <a href="#minerals-14-01302-t002" class="html-table">Table 2</a>). Scale bars in all cases 200 μm.</p>
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<p>Back-scattered electron images (BSE) of pyrochlore crystals from the Madeira pluton. Medium-grade altered examples (type 2 pyrochlore): (<b>a</b>) a zoned pyrochlore crystal with its core irregularly replaced with columbite along a network of thin cracks, Madeira albite granite core facies, (#PHR128, crystal 1); (<b>b</b>) zoned pyrochlore with the intermediate zone replaced with columbite, Madeira albite granite core facies, (#PHR160, crystal 1); (<b>c</b>) a zoned pyrochlore crystal with its core partly replaced with columbite and a thick columbite overgrowth. Bright domains are enriched in U. Madeira albite granite core facies (#PHR 163, crystal 2); (<b>d</b>) a zoned pyrochlore crystal with its core partly replaced with columbite and an altered rim enriched in Pb, associated with cassiterite. Madeira albite granite core facies (#PHR 245, crystal 6); (<b>e</b>) patchy-colored pyrochlore with the outer zone partly replaced with columbite, Madeira albite granite core facies (#PHR 128, crystal 3); (<b>f</b>) zoned pyrochlore replaced with columbite from the core and the rim, bright domains enriched in U or Pb, Madeira albite granite core facies (#PHR 245, crystal 1). Scale bars in all cases 200 μm.</p>
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<p>Back-scattered electron images (BSE) of pyrochlore crystals from the Madeira pluton. Strongly altered examples from the core albite granite (type 3 pyrochlore): (<b>a</b>) patchy-zoned pyrochlore replaced with columbite from the rim, Madeira albite granite core facies (#PHR128, crystal 2); (<b>b</b>) patchy-zoned pyrochlore irregularly replaced with columbite and rimmed by hematite, Madeira hypersolvus granite (#PHR191, crystal 1); (<b>c</b>) patchy-zoned pyrochlore irregularly replaced with columbite, Madeira albite granite core facies (#PHR171, crystal 4); (<b>d</b>) remnants of patchy-zoned pyrochlore replaced with hematite from the rims, Madeira albite granite core facies, (#PHR246, crystal 4); (<b>e</b>) remnants of strongly altered pyrochlore replaced with hematite, bright domains enriched in Pb, Madeira hypersolvus granite, (#PHR191, crystal 1); (<b>f</b>) a remnant of a euhedral pyrochlore crystal (bright area) replaced with columbite (dark) and uraninite (small bright inclusions), Madeira albite granite core facies (#PHR247, crystal 2). Scale bars in all cases 200 μm.</p>
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<p>Back-scattered electron images (BSE) of columbite from the Madeira border albite granite (sample PHR-174): (<b>a</b>) an aggregate of primary-looking tabular columbite crystals (gray) with small inclusions of cassiterite (bright); (<b>b</b>) an aggregate of tabular columbite crystals (gray) associated with pyrite (dark gray). Columbite is transformed to type 4 pyrochlore in two ways: (i) thin bright coatings of U-rich pyrochlore on the columbite surface and in the interstices, and (ii) pervasive replacement forming inhomogeneous colander-like domains of Si, U-rich pyrochlore with small bright spots of a U-rich phase. Scale bars 100 μm.</p>
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<p>Chemical characteristics of PSGM from the Madeira granite and some other rare-metal granites: (<b>a</b>) Nb vs. Ta; (<b>b</b>) Nb + Ta vs. Si; (<b>c</b>) F vs. Si; (<b>d</b>) Sn vs. W; (<b>e</b>) Ca vs. Na; (<b>f</b>) Th vs. U; (<b>g</b>) Pb vs. Na; (<b>h</b>) F vs. Na. All in atoms per formula unit (apfu).</p>
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<p>The distribution of REE in pyrochlore/microlite (chondrite-normalized according to [<a href="#B67-minerals-14-01302" class="html-bibr">67</a>]): (<b>a</b>) type 1 pyrochlore from the Madeira core albite granite: sample PHR160 in black, PHR161 in red; (<b>b</b>) type 2 pyrochlore from the Madeira core albite granite: sample PHR242 in black, PHR243 in red; (<b>c</b>) type 3 pyrochlore from the Madeira hypersolvus granite: sample PHR191, crystal 1 in black, crystal 2 in green; (<b>d</b>) type 3 pyrochlore from the Madeira core albite granite (sample PHR247 in black) and type 4 pyrochlore from the Madeira border albite granite (sample PHR174 in red); (<b>e</b>) microlite (in red) and pyrochlore (in black) from Cínovec.</p>
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<p>Chemical characteristics of CGM: (<b>a</b>) Mn/(Fe + Mn) vs. Ta/(Nb + Ta); (<b>b</b>) SnO<sub>2</sub> vs. WO<sub>3</sub>; (<b>c</b>) TiO<sub>2</sub> vs. UO<sub>2</sub>.</p>
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<p>The distribution of elements in a relatively fresh pyrochlore crystal from Madeira, sample PHR160, crystal 3. Relative contents of Si and Na perfectly show a thin cryolite halo immediately around pyrochlore, dividing it from albite, while the enrichment in Fe along crystal rims indicates columbite overgrowth/replacement. Scale bar equals 100 μm.</p>
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<p>The distribution of elements in a zoned pyrochlore crystal, sample PHR 82A, crystal 7: the distribution of Si and Na shows a cryolite halo separating pyrochlore from the feldspar matrix. A slight enrichment in Si indicates two zones of incipient alteration. The crystal is penetrated by a network of fissures along which it is replaced with columbite, as indicated by Fe enrichment. The behavior of U is similar to that of Pb but different from that of Th. Scale bar equals 250 μm.</p>
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<p>The distribution of elements in a strongly altered pyrochlore crystal, sample 247, crystal 2: the major part of the crystal is replaced with columbite-Fe. U, Pb-rich pyrochlore forms only small remnants at present, with lower Nb and Fe contents than in columbite. The major part of U and Th, primarily bound in pyrochlore and non-compatible in columbite, forms inclusions of thorite-coffinite s.s., while Pb was mostly dispersed. Scale bar equals 100 μm.</p>
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<p>Back-scattered electron images (BSE) of microlite and CGM from Orlovka deposit: (<b>a</b>) a fresh, zoned microlite crystal, a flat, banded pegmatite-aplite body (#O 353, crystal 10); (<b>b</b>) a zoned microlite crystal with a Nb-rich, slightly altered core and fresh, Ta-rich rims. The core is slightly altered along cracks and locally has a porous structure. Amazonite-topaz-lepidolite granite (#O-369, crystal 2); (<b>c</b>) an anhedral microlite grain altered from the rims inwards, amazonite-lepidolite granite (#O-253, grain 3); (<b>d</b>) a fresh, subhedral, zoned columbite-Mn crystal, fine-grained lepidolite granite (#4703, crystal 3); (<b>e</b>), a zoned crystal with an euhedral columbite-Mn core and anhedral tantalite-Fe rims, albite-muscovite granite (#O-222, crystal 1); (<b>f</b>) an anhedral grain of tantalite-Fe in association with wolframite, a flat, banded pegmatite-aplite body (#O-353, grain 7).</p>
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<p>Back-scattered electron images (BSE) of pyrochlore, microlite, and columbite from Cínovec: (<b>a</b>) microlite associated with pyrite, greisenized granite, Cínovec-South deposit (#5423, grain 1); (<b>b</b>) microlite replaced with cassiterite, greisenized granite, Cínovec-South deposit (#5436, grain 1); (<b>c</b>) an anhedral pyrochlore aggregate embedded in fluorite, Cínovec biotite granite, borehole CS-1, depth 741 m (#4690B, grain 1); (<b>d</b>) remnants of Si, U-rich pyrochlore and columbite, both replaced with scheelite, greisenized granite, Cínovec-South deposit (#5427, grain 2); (<b>e</b>) a zoned columbite crystal with two zones in the euhedral core and the patchy anhedral rim, quartz-zinnwaldite greisen, Cínovec-South deposit (#13, grain 2); (<b>f</b>) an aggregate of fine, tabular crystals of columbite, albite granite, Cínovec, borehole Cs-1, depth 24 m (#4972, grain 1).</p>
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<p>Occupancy of A and B sites in PSGM: (<b>a</b>), Na vs. Ca vs. other elements and vacancies at the A site; (<b>b</b>), Na + Ca vs. other elements vs. vacancies at the A site; (<b>c</b>), Nb vs. Ta vs. other elements at the B site. Data from Beauvoir, according to [<a href="#B10-minerals-14-01302" class="html-bibr">10</a>,<a href="#B49-minerals-14-01302" class="html-bibr">49</a>].</p>
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<p>Chemical characteristics of PSGM from different lithologies: (<b>a</b>) Nb vs. Ta; (<b>b</b>) Nb + Ta vs. Si; (<b>c</b>) F vs. Si; (<b>d</b>) Sn vs. W; (<b>e</b>) Ca vs. Na; (<b>f</b>) Th vs. U; (<b>g</b>) Pb vs. Na; (<b>h</b>) F vs. Na; all in atoms per formula unit (apfu). For data sources, see the Geology section.</p>
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16 pages, 5584 KiB  
Article
Analyses of the Properties of the NiO-Doped Ga2O3 Wide-Bandgap Semiconductor Thin Films
by Cheng-Fu Yang, En-Chi Tsao, Yi-Wen Wang, Hsin-Pei Lin, Teen-Hang Meen and Shu-Han Liao
Coatings 2024, 14(12), 1615; https://doi.org/10.3390/coatings14121615 - 23 Dec 2024
Abstract
The study began by pre-sintering Ga2O3 powder at 950 °C for 1 h, followed by the preparation of a mixture of Ga2O3 and 12 at% NiO powders to fabricate a source target material. An electron beam (e-beam) [...] Read more.
The study began by pre-sintering Ga2O3 powder at 950 °C for 1 h, followed by the preparation of a mixture of Ga2O3 and 12 at% NiO powders to fabricate a source target material. An electron beam (e-beam) system was then used to deposit NiO-doped Ga2O3 thin films on Si substrates. X-ray diffraction (XRD) analyses revealed that the pre-sintered Ga2O3 at 950 °C exhibited β-phase characteristics, and the deposited NiO-doped Ga2O3 thin films exhibited an amorphous phase. After the deposition of the NiO-doped Ga2O3 thin films, they were divided into two portions. One portion underwent various analyses directly, while the other was annealed at 500 °C in air before being analyzed. Field-emission scanning electron microscopy (FESEM) was utilized to process the surface observation, and the cross-sectional observation was primarily used to measure the thickness of the NiO-doped Ga2O3 thin films. UV-Vis spectroscopy was used to calculate the bandgap by analyzing the transmission spectra, while the Agilent B1500A was employed to measure the I-V characteristics. Hall measurements were also performed to assess the mobility, carrier concentration, and resistivity of both NiO-doped Ga2O3 thin films. The first innovation is that the 500 °C-annealed NiO-doped Ga2O3 thin films exhibited a larger bandgap and better electrical conductivity. The manuscript provides an explanation for the observed increase in the bandgap. Another important innovation is that the 500 °C-annealed NiO-doped Ga2O3 thin films revealed a high-energy bandgap of 4.402 eV. The third innovation is that X-ray photoelectron spectroscopy (XPS) analyses of the Ga2p3/2, Ga2p1/2, Ga3d, Ni2p3/2, and O1s peaks were conducted to further investigate the reasons behind the enhanced electrical conductivity of the 500 °C-annealed NiO-doped Ga2O3 thin films. Full article
(This article belongs to the Special Issue Coatings for Advanced Devices)
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<p>Schematic diagram for the NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films.</p>
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<p>Schematic diagram to obtain the various NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films and the different analyses for the various NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films.</p>
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<p>Surface morphologies of (<b>a</b>) un-annealed and (<b>b</b>) 500 °C-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films and (<b>c</b>) the cross-sectional image of the deposited NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films.</p>
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<p>EDS analysis of the 500 °C-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films: (<b>a</b>) analysis area and (<b>b</b>) analysis result.</p>
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<p>Tauc plots of (<b>a</b>) un-annealed, (<b>b</b>) 500 °C-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films, and (<b>c</b>) un-annealed and undoped Ga<sub>2</sub>O<sub>3</sub> thin films.</p>
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<p>SIMS analysis results of Ga, Ni, Si, and O elements of (<b>a</b>) un-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films and (<b>b</b>) 500 °C-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films.</p>
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<p>Current–voltage properties of the un-annealed and 500 °C-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films.</p>
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<p>XPS spectra of the Ga<sub>2p3/2</sub> peaks and the Gaussian-resolved components (<b>a</b>) un-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films and (<b>b</b>) 500 °C-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films.</p>
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<p>XPS spectra of the Ga<sub>2p1/2</sub> peaks and the Gaussian-resolved components (<b>a</b>) un-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films and (<b>b</b>) 500 °C-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films.</p>
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<p>XPS spectra of the Ga<sub>3d</sub> peaks and the Gaussian-resolved components in (<b>a</b>) un-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films and (<b>b</b>) 500 °C-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films.</p>
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<p>XPS spectra of the Ni<sub>2p3/2</sub> and Ni <sub>2p1/2</sub> peaks and the Gaussian-resolved components of (<b>a</b>) un-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films and (<b>b</b>) 500 °C-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films.</p>
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<p>XPS spectra of the O<sub>1s</sub> peaks and the Gaussian-resolved components in (<b>a</b>) un-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films and (<b>b</b>) 500 °C-annealed NiO-doped Ga<sub>2</sub>O<sub>3</sub> thin films.</p>
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14 pages, 4991 KiB  
Article
Study on Reduction Mechanism of Iron Oxide by Industrial Lignin
by Dongwen Xiang, Qiang Zhang, Guoqing Wu, Yajie Wang, Dong Li, Qinghua Zhang and Huaxin Hu
Metals 2024, 14(12), 1467; https://doi.org/10.3390/met14121467 - 23 Dec 2024
Abstract
To effectively utilize industrial lignin, a large amount of waste produced by the pulp and paper industry, this paper primarily explores its potential as a substitute for coal-based reducing agents in the reduction of iron oxides. The weight change, phase change, and activation [...] Read more.
To effectively utilize industrial lignin, a large amount of waste produced by the pulp and paper industry, this paper primarily explores its potential as a substitute for coal-based reducing agents in the reduction of iron oxides. The weight change, phase change, and activation energy change during the reduction of iron oxide by industrial lignin were characterized using detection methods such as TG-DTG-DSC, XRD, and SEM. The results show that the maximum weight loss rate of industrial lignin reducing iron oxide is (4.52%·min−1) > Lu’an anthracite (2.01%·min−1) > Shenmu bituminous coal (1.57%·min−1). The activation energy variation range during the reduction of Fe2O3 by industrial lignin, calculated using the Flynn–Wall–Ozawa (FWO) method, is 241.91~463.51 kJ·mol−1, and the activation energy first decreased, then increased, then decreased slightly with the increase of conversion fraction. There is a coupling effect in the reduction of Fe2O3 by industrial lignin. Full article
(This article belongs to the Special Issue Advanced Metal Smelting Technology and Prospects)
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<p>Thermogravimetric curve of reducing agent pyrolysis and its reduction of Fe<sub>2</sub>O<sub>3</sub> at heating rate of 10 °C·min<sup>−1</sup>.</p>
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<p>Phase composition of mixed samples of different reductants and Fe<sub>2</sub>O<sub>3</sub> under conditions of <span class="html-italic">n</span><sub>c</sub>/<span class="html-italic">n</span><sub>o</sub> = 1 and heating rate of 10 °C·min<sup>−1</sup>.</p>
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<p>SEM-EDS diagram of IL + Fe<sub>2</sub>O<sub>3</sub> mixed sample after reduction at heating rate of 10 °C·min<sup>−1</sup>.</p>
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<p>TG-DTG curve of Fe<sub>2</sub>O<sub>3</sub> reduction process under different heating rates. (<b>a</b>) LA + Fe<sub>2</sub>O<sub>3</sub>; (<b>b</b>) SM + Fe<sub>2</sub>O<sub>3</sub>; (<b>c</b>) IL + Fe<sub>2</sub>O<sub>3</sub>.</p>
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<p>TG-DTG-DSC curve of reduction of iron oxide by IL at heating rate of 10 °C·min<sup>−1</sup>.</p>
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<p>Linear fitting relationship between ln<span class="html-italic">β</span> and 1/<span class="html-italic">T</span> under different conversion rates calculated by FWO method.</p>
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<p>Linear fitting relationship between ln(<span class="html-italic">β</span>/<span class="html-italic">T</span><sup>2</sup>) and 1/<span class="html-italic">T</span> under different conversion rates calculated by KAS method.</p>
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<p>The activation energy change of Fe<sub>2</sub>O<sub>3</sub> reduction by IL obtained by FWO and KAS method.</p>
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16 pages, 17228 KiB  
Article
Microstructure and Corrosion Resistance of Laser-Cladded FeCo1.5CrNi1.5Ti0.5 High-Entropy Alloy Coatings
by Sui Wang, Siqi Tian, Renjie Liu, Dengya Chen, Chao Wang, Jing Li and Sen Yang
Coatings 2024, 14(12), 1608; https://doi.org/10.3390/coatings14121608 - 23 Dec 2024
Abstract
Due to their excellent mechanical properties and corrosion resistance, high-entropy alloys (HEAs) have the potential to be used as new engineering structures and functional materials. In this study, an FeCo1.5CrNi1.5Ti0.5HEA coating was prepared on the surface of [...] Read more.
Due to their excellent mechanical properties and corrosion resistance, high-entropy alloys (HEAs) have the potential to be used as new engineering structures and functional materials. In this study, an FeCo1.5CrNi1.5Ti0.5HEA coating was prepared on the surface of a 1Cr18Ni9Ti alloy by laser cladding technology. Phase structure and microstructure were characterized by XRD and using an SEM. The corrosion resistance was evaluated by an electrochemical workstation, and the polarization curves were obtained in simulated seawater and 3.5 wt.% NaCl and 5% HCl solutions. The corrosion morphology of the Fe-based HEA coating was further characterized using the SEM, super depth of field observation, and 3D topological images. The results showed that the Fe-based HEA coating had a single-phase FCC structure with a grain size of about 10.7 ± 0.25 μM. Electrochemical analysis results showed that the corrosion resistance of the current Fe-based HEA coating was poor in HCl solutions. However, it exhibited good corrosion properties in simulated seawater and 3.5 wt.% NaCl solutions. Further analysis of the corrosion morphology revealed that in simulated seawater and the 3.5 wt.% NaCl solution, the surface of the current Fe-based HEA coating exhibited a preferential corrosion tendency between dendrites, while in the 5% HCl solution, it exhibited more obvious pitting characteristics. The results indicate that the current Fe-based HEA coating exhibits good comprehensive performance, especially in an acidic Cl corrosion environment. These findings provide a reference for the application of laser cladding prepared Fe HEA coatings. Full article
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<p>The coating sample and the XRD pattern. (<b>a</b>) The macroscopic sample prepared by laser cladding; the inset shows the OM of the lateral surface of the coating; (<b>b</b>) the XRD pattern of FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA powder and coating.</p>
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<p>Microstructure of FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA coating at different multiples: (<b>a</b>) 2000×; (<b>b</b>) 5000×.</p>
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<p>SEM image and the corresponding elemental distribution maps of the FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA coating.</p>
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<p>OCP and polarization curves of the FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA coating and the metal substrate at normal temperature under different working conditions: (<b>a</b>) OCP curves; (<b>b</b>) simulated seawater; (<b>c</b>) 3.5 wt.% NaCl solution; (<b>d</b>) 5% HCl solution.</p>
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<p>EIS results and equivalent circuits of the FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA coating in simulated seawater, a 3.5 wt.% NaCl solution, and a 5% HCl solution. (<b>a</b>) Nyquist plots; (<b>b</b>) Bode plots; (<b>c</b>) the equivalent circuit used for simulated seawater and the 3.5 wt.% NaCl solution; (<b>d</b>) the equivalent circuit used for the 5% HCl solution.</p>
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<p>Micrographs and the corresponding 3D topological images of FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA coating and the metal substrate after electrochemical testing in simulated seawater. (<b>a</b>) Super-depth morphology of the HEA coating; (<b>b</b>) 3D topological image of the HEA coating; (<b>c</b>) super-depth morphology of the metal substrate; (<b>d</b>) 3D topological image of the metal substrate.</p>
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<p>Micrographs and the corresponding 3D topological images of the FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA coating and the metal substrate after electrochemical testing in a 3.5 wt.% NaCl solution. (<b>a</b>) Super-depth morphology of the HEA coating; (<b>b</b>) 3D topological image of the HEA coating; (<b>c</b>) super-depth morphology of the metal substrate; (<b>d</b>) 3D topological image of the metal substrate.</p>
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<p>Micrographs and the corresponding 3D topological images of the FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA coating and the metal substrate after electrochemical testing in a 3.5 wt.% NaCl solution. (<b>a</b>) Super-depth morphology of the HEA coating; (<b>b</b>) 3D topological image of the HEA coating; (<b>c</b>) super-depth morphology of the metal substrate; (<b>d</b>) 3D topological image of the metal substrate.</p>
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<p>Micrographs and the corresponding 3D topological images of the FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA coating and the metal substrate after electrochemical testing in a 5% HCl solution. (<b>a</b>) Super-depth morphology of the HEA coating; (<b>b</b>) 3D topological image of the HEA coating; (<b>c</b>) super-depth morphology of the metal substrate; (<b>d</b>) 3D topological image of the metal substrate.</p>
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<p>SEM images of the FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA coating and the metal substrate after electrochemical testing in simulated seawater. (<b>a</b>) HEA coating, 500×; (<b>b</b>) HEA coating, 2000×; (<b>c</b>) the metal substrate, 500×; (<b>d</b>) the metal substrate, 2000×.</p>
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<p>SEM images of the FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA coating and the metal substrate after electrochemical testing in a 3.5 wt.% NaCl solution. (<b>a</b>) HEA coating, 500×; (<b>b</b>) HEA coating, 2000×; (<b>c</b>) the metal substrate, 500×; (<b>d</b>) the metal substrate, 2000×.</p>
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<p>SEM images of the FeCo<sub>1.5</sub>CrNi<sub>1.5</sub>Ti<sub>0.5</sub> HEA coating and the metal substrate after electrochemical testing in a 5% HCl solution. (<b>a</b>) HEA coating, 500×; (<b>b</b>) HEA coating, 2000×; (<b>c</b>) the metal substrate, 500×; (<b>d</b>) the metal substrate, 2000×.</p>
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15 pages, 10134 KiB  
Article
Investigation of Calcium Phosphate-Based Biopolymer Composite Scaffolds for Bone Tissue Engineering
by Monika Furko, Zsolt E. Horváth, Istvan Tolnai, Katalin Balázsi and Csaba Balázsi
Int. J. Mol. Sci. 2024, 25(24), 13716; https://doi.org/10.3390/ijms252413716 - 22 Dec 2024
Viewed by 400
Abstract
We present a novel method for preparing bioactive and biomineralized calcium phosphate (mCP)-loaded biopolymer composite scaffolds with a porous structure. Two types of polymers were investigated as matrices: one natural, cellulose acetate (CA), and one synthetic, polycaprolactone (PCL). Biomineralized calcium phosphate particles were [...] Read more.
We present a novel method for preparing bioactive and biomineralized calcium phosphate (mCP)-loaded biopolymer composite scaffolds with a porous structure. Two types of polymers were investigated as matrices: one natural, cellulose acetate (CA), and one synthetic, polycaprolactone (PCL). Biomineralized calcium phosphate particles were synthesized via wet chemical precipitation, followed by the addition of organic biominerals, such as magnesium gluconate and zinc gluconate, to enhance the bioactivity of the pure CP phase. We compared the morphological and chemical characteristics of the two types of composites and assessed the effect of biomineralization on the particle structure of pure CP. The precipitated CP primarily consisted of nanocrystalline apatite, and the addition of organic trace elements significantly influenced the morphology by reducing particle size. FE-SEM elemental mapping confirmed the successful incorporation of mCP particles into both CA and PCL polymer matrices. Short-term immersion tests revealed that the decomposition rate of both composites is slow, with moderate and gradual ionic dissolution observed via ICP-OES measurements. The weight loss of the PCL-based composite during immersion was minimal, decreasing by only 0.5%, while the CA-based composite initially exhibited a slight weight increase before gradually decreasing over time. Full article
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<p>FE-SEM images of amorphous apatite (CP) (<b>a</b>) biomineralized (Mg, Zn added apatite (mCP) (<b>b</b>), pure cellulose acetate (<b>c</b>), pure PCL polymer (<b>d</b>), as well as their composites CA-mCP (<b>e</b>) and PCL-mCP (<b>f</b>). The parameters used in the preparation were kept consistent to ensure their comparability.</p>
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<p>FE-SEM images of amorphous apatite (CP) (<b>a</b>) biomineralized (Mg, Zn added apatite (mCP) (<b>b</b>), pure cellulose acetate (<b>c</b>), pure PCL polymer (<b>d</b>), as well as their composites CA-mCP (<b>e</b>) and PCL-mCP (<b>f</b>). The parameters used in the preparation were kept consistent to ensure their comparability.</p>
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<p>Scanning electron microscope image and the corresponding elemental mapping of biomineralized (Mg, Zn) calcium apatite.</p>
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<p>Scanning electron microscope image and the corresponding elemental mapping of PCL-mCP composite (<b>a</b>) and CA-mCP composite (<b>b</b>).</p>
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<p>XRD patterns of CP and mCP powders (<b>a</b>) prepared by wet chemical method and the PCL-mCP, CA.mCP composites (<b>b</b>).</p>
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<p>FE-SEM images on CA-mCP (<b>a</b>) and PCL-mCP (<b>c</b>) composites as prepared as well as CA-mCP (<b>b</b>) and PCL-mCP (<b>d</b>) composites after two weeks of immersion in saline solution.</p>
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<p>Sample weight changes during the two-week immersion period in saline solution at room temperature. Values are graphed as the mean ± standard deviation (<span class="html-italic">n</span> = 3). * indicates <span class="html-italic">p</span>  &lt;  0.05; ** indicates <span class="html-italic">p</span> &lt;  0.01.</p>
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<p>Cumulative concentrations of the dissolved bioactive ions from CA-mCP (<b>a</b>) and PCL-mCP (<b>b</b>) composites soaked in saline solution at room temperature. The values are normalized to the unit area of samples. All data points are presented as the mean ± standard deviation (<span class="html-italic">n</span> = 3).</p>
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12 pages, 4216 KiB  
Article
A Novel Bifunctional Surface Coating Method to Effectively Eliminate Residual Li on NCM811 by Using Uniformly Dispersed Metal Oxide Solution
by Seung Hyun Kim, Nanasaheb M. Shinde, Young-Eun Yun and Jeom-Soo Kim
Batteries 2024, 10(12), 453; https://doi.org/10.3390/batteries10120453 - 22 Dec 2024
Viewed by 171
Abstract
A uniformly coating transition metal oxide solution (TS-M) was developed to simultaneously remove residual Li compounds (RLCs) and stabilize the surface of NCM811 material. XRD analysis revealed that the synthesized cathode samples (TS-M, where M = Ti, Ge, Sn) exhibited hexagonal α-NaFeO2 [...] Read more.
A uniformly coating transition metal oxide solution (TS-M) was developed to simultaneously remove residual Li compounds (RLCs) and stabilize the surface of NCM811 material. XRD analysis revealed that the synthesized cathode samples (TS-M, where M = Ti, Ge, Sn) exhibited hexagonal α-NaFeO2 structures without impurity phases. FE-SEM and EDX results confirmed the formation of a uniform metal oxide coating (TS-Ti, TS-Ge: and TS-Sn) on the surface of NCM811, demonstrating its potential as a high-performance cathode material for lithium-ion batteries (LIBs). Among the treated samples, the TS-Sn sample delivered an excellent discharge capacity of 172.4 mAh g−1 with a retention of 90.4% after 50 cycles at a 1.0 C rate, outperforming the TS-Ge and TS-Ti samples. Electrochemical impedance spectroscopy (EIS) further validated the improved impedance of NCM samples after Ti, Ge, and Sn coatings. Based on these findings, the application of Ti, Ge, and Sn metal oxide coatings to NCM811 is considered a reliable surface modification strategy for enhancing electrochemical performance by eliminating RLCs and stabilizing the surface. Full article
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<p>Schematic illustration for bifunctional coating process.</p>
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<p>(<b>a</b>) XRD patterns, (<b>b</b>) lattice parameters a and c, (<b>c</b>) I(003)/I(104) ratio, and (<b>d</b>) c/3a ratio of pristine NCM811, W50, TS-Ti, TS-Ge, and TS-Sn cathode materials.</p>
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<p>SEM images of pristine NCM811 (<b>a</b>,<b>b</b>), TS-Ti (<b>c</b>,<b>d</b>), TS-Ge (<b>e</b>,<b>f</b>), and TS-Sn (<b>g</b>,<b>h</b>). Corresponding EDS mapping analysis images (<b>i</b>): TS-Ti (<b>i-1</b>), TS-Ge (<b>i-2</b>), and TS-Sn (<b>i-3</b>), respectively.</p>
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<p>Residual Li concentrations of pristine, W50, TS-Ti, TS-Ge, and TS-Sn samples.</p>
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<p>Survey XPS spectrum of pristine NCM811, TS-Ti, TS-Ge, and TS-Sn (<b>a</b>); and high-resolution XPS spectra of Ti 2p (<b>b</b>), Ge 2p (<b>c</b>), and Sn 3d (<b>d</b>) levels.</p>
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<p>(<b>a</b>) Galvanostatic charge and discharge profiles of pristine, W50, and TSM (Ti, Ge, and Sn) at constant current of 0.1C. (<b>b</b>) Rate characteristics of all samples at 0.5C, 1.0C, and 2.0C. Cycling performance combined with coulombic efficiencies with current density of 1.0C(charge)/1C(discharge) at (<b>c</b>) 25 °C and (<b>d</b>) 45 °C.</p>
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<p>Nyquist plots of pristine and TS-M samples (<b>a</b>) before and (<b>b</b>) after 50 cycles; (<b>c</b>) equivalent circuit model used for fitting EIS spectra.</p>
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15 pages, 5908 KiB  
Article
Fabrication and Coating of Porous Ti6Al4V Structures for Application in PEM Fuel Cell and Electrolyzer Technologies
by Juan Villemur, Carlos Romero, Jose Manuel Crego and Elena Gordo
Materials 2024, 17(24), 6253; https://doi.org/10.3390/ma17246253 - 21 Dec 2024
Viewed by 304
Abstract
The production of green hydrogen through proton exchange membrane water electrolysis (PEMWE) is a promising technology for industry decarbonization, outperforming alkaline water electrolysis (AWE). However, PEMWE requires significant investment, which can be mitigated through material and design advancements. Components like bipolar porous plates [...] Read more.
The production of green hydrogen through proton exchange membrane water electrolysis (PEMWE) is a promising technology for industry decarbonization, outperforming alkaline water electrolysis (AWE). However, PEMWE requires significant investment, which can be mitigated through material and design advancements. Components like bipolar porous plates (BPPs) and porous transport films (PTFs) contribute substantially to costs and performance. BPPs necessitate properties like corrosion resistance, electrical conductivity, and mechanical integrity. Titanium, commonly used for BPPs, forms a passivating oxide layer, reducing efficiency. Effective coatings are crucial to address this issue, requiring conductivity and improved corrosion resistance. In this study, porous Ti64 structures were fabricated via powder technology, treating them with thermochemical nitriding. The resulting structures with controlled porosity exhibited enhanced corrosion resistance and electrical conductivity. Analysis through scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), grazing incidence XRD and X-ray photoelectron spectroscopy (XPS) confirmed the effectiveness of the coating, meeting performance requirements for BPPs. Full article
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<p>Characteristics of Ti-6Al-4V powder: (<b>a</b>) SEM micrograph and (<b>b</b>) particle size distribution.</p>
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<p>Scanning electron microscopy (SEM) images of porous Ti-6Al-4V specimens: (<b>a</b>) cross-section of a Ti-6Al-4V porous sample, (<b>b</b>) pore size distribution, (<b>c</b>) inner pore in a Ti-6Al-4V porous sample, (<b>d</b>) surface of an inner pore.</p>
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<p>Scanning electron microscopy (SEM) images of dense Ti-6Al-4V specimens: (<b>a</b>) cross-section of a Ti-6Al-4V dense specimen, (<b>b</b>) EDS analysis of the surface of the specimen.</p>
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<p>XRD patterns of as-sintered and nitride Ti64 samples.</p>
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<p>GIXRD patterns of nitride Ti64 samples.</p>
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<p>XPS spectra of Ti-6Al-4V: (<b>a</b>) Ti 2p of untreated Ti-6Al-4V, (<b>b</b>) Ti 2p of nitrided Ti-6Al-4V, and (<b>c</b>) N 1 s of nitrided Ti-6Al-4V.</p>
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<p>Potentiodynamic polarization curves of Ti-6Al-4V simulating the PEMFC anode conditions.</p>
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<p>Chronoamperometric test of the Ti64 samples at 0.6 V vs. Ag/AgCl simulating the PEMFC cathode conditions.</p>
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<p>Interfacial contact resistance (ICR) of untreated and treated Ti-6Al-4V: (<b>a</b>) evolution with compaction force, (<b>b</b>) insert of (<b>a</b>) centered on the low ICR values, (<b>c</b>) comparison of pre- and post-corrosion measured at 135 N/cm<sup>2</sup>.</p>
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18 pages, 9422 KiB  
Article
Activating Peroxymonosulfate by a NovelFe-MOF-C/N Catalyst to Effectively Degrade Sulfamethoxazole: Catalyst Performance and Its Mechanism
by Zhaowei Wu, Meiyi Hu, Pengfan Zhuo, Jie Wang and Shaoping Tong
Separations 2024, 11(12), 356; https://doi.org/10.3390/separations11120356 - 21 Dec 2024
Viewed by 437
Abstract
A composite Fe-MOF-C/N was prepared with Fe-MOF and g-C3N4 precursors, and its activation property of peroxymonosulfate (PMS) in the degradation of Sulfamethoxazole (SMX) was studied. XRD, SEM, and TEM analyses showed that Fe-MOF-C/N was porous and mainly composed of phases [...] Read more.
A composite Fe-MOF-C/N was prepared with Fe-MOF and g-C3N4 precursors, and its activation property of peroxymonosulfate (PMS) in the degradation of Sulfamethoxazole (SMX) was studied. XRD, SEM, and TEM analyses showed that Fe-MOF-C/N was porous and mainly composed of phases of Fe3N, C0.08Fe1.92, and graphite. XPS indicated that Fe-MOF-C/N mainly had Fe, C, N, and O elements, among which Fe existed in the form of Fe2+ and Fe3+. Fe-MOF-C/N was used to activate PMS to degrade SMX, and the result showed that Fe-MOF-C/N had excellent catalytic performance and 84.17% of SMX could be removed in 8 min. Free radical quenching experiments showed that 1O2 was the main active species in Fe-MOF-C/N/PMS. The stability experiment showed that Fe-MOF-C/N had good stability, and the degradation rate of SMX only decreased by 5.8% after five times of use. Full article
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<p>XRD spectra of Fe-MOF-C/N-1:0.5.</p>
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<p>SEM of Fe-MOF-C/N-1:0.5 before (<b>a</b>) and after calcination (<b>b</b>).</p>
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<p>Mapping of Fe-MOF-C/N-1:0.5 after calcination (<b>a</b>); distribution of each element (<b>b</b>); distribution of C (<b>c</b>); distribution of N (<b>d</b>) and distribution of Fe (<b>e</b>).</p>
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<p>TEM image at 100 nm (<b>a,b</b>); TEM image with lattice spacing at 5 nm (<b>c</b>); TEM image with lattice spacing at 10 nm (<b>d</b>) of Fe-MOF-C/N-1:0.5.</p>
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<p>N<sub>2</sub> Absorption/desorption isotherms (<b>a</b>) and pore size distribution (<b>b</b>) of Fe-MOF-C/N-1:0.5.</p>
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<p>XPS spectra of Fe-MOF-C/N-1:0.5 (full spectrum (<b>a</b>) and high-resolution spectra of elements ((<b>b</b>) C, (<b>c</b>) Fe, and (<b>d</b>) N)).</p>
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<p>Efficiencies of Fe-MOF-C/N-1:0.5/PMS in degradation of SMX. Reaction conditions: SMX solution (200 mL 50 mg/L); PMS and Fe-MOF-C/N (0.20 g/L); pH = 7.</p>
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<p>Effect of mass ratio of precursors on degradation efficiency of SMX. Reaction conditions: SMX solution (200 mL 50 mg/L); PMS and Fe-MOF-C/N (0.20 g/L); pH = 7.</p>
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<p>Effect of calcination temperature on degradation of SMX. Reaction conditions: SMX solution (200 mL 50 mg/L); PMS and Fe-MOF-C/N (0.20 g/L); pH = 7.</p>
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<p>XRD spectra of Fe-MOF-C/N-1:0.5 prepared at different calcination temperatures.</p>
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<p>Effect of ethanol, TBA, and FFA on degradation of SMX. Reaction conditions: SMX solution (200 mL 50 mg/L); PMS and Fe-MOF-C/N (0.20 g/L); pH = 7.</p>
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<p>Effect of different initial pH values on degradation efficiency of SMX. Reaction conditions: SMX solution (200 mL 50 mg/L); PMS and Fe-MOF-C/N (0.20 g/L); pH = 7.</p>
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<p>Effect of different dosage of PMS on degradation efficiency of SMX. Reaction conditions: SMX solution (200 mL 50 mg/L) and Fe-MOF-C/N (0.20 g/L); pH = 7.</p>
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<p>Effect of different dosage of Fe-MOF-C/N-1:0.5 on degradation of SMX. Reaction conditions: SMX solution (200 mL 50 mg/L) and PMS (0.20 g/L).</p>
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<p>The adsorption effect of different Fe-MOF-C/N-1:0.5 dosages on SMX. Reaction conditions: SMX solution (200 mL 50 mg/L) and PMS (0.20 g/L).</p>
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<p>Recycling test of Fe-MOF-C/N-1:0.5 for activating PMS. Reaction conditions: SMX solution (200 mL 50 mg/L); PMS and Fe-MOF-C/N (0.20 g/L).</p>
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<p>XRD of fresh and used catalysts.</p>
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<p>Possible degradation pathway of SMX.</p>
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<p>Toxicity analysis of intermediate products of SMX, Lethal concentrations of intermediates products to large dophnia (<b>a</b>); Lethal concentrations of intermediates to fat-heat fish (<b>b</b>); Developmental toxicity (<b>c</b>); Mutagenicity (<b>d</b>).</p>
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18 pages, 3212 KiB  
Article
Facile Hydrothermal Assisted Basic Catalyzed Sol Gel Synthesis for Mesoporous Silica Nanoparticle from Alkali Silicate Solutions Using Dual Structural Templates
by Khaled M. AlMohaimadi, Hassan M. Albishri, Khaled A. Thumayri, Awadh O. AlSuhaimi, Yassin T. H. Mehdar and Belal H. M. Hussein
Gels 2024, 10(12), 839; https://doi.org/10.3390/gels10120839 - 19 Dec 2024
Viewed by 298
Abstract
This work presents a novel hydrothermally aided sol-gel method for preparation of mesoporous silica nanoparticles (MSNs) with a narrow particle size distribution and varied pore sizes. The method was carried out in alkaline media in presence of polyethylene glycol (PEG) and cetyltrimethylammonium chloride [...] Read more.
This work presents a novel hydrothermally aided sol-gel method for preparation of mesoporous silica nanoparticles (MSNs) with a narrow particle size distribution and varied pore sizes. The method was carried out in alkaline media in presence of polyethylene glycol (PEG) and cetyltrimethylammonium chloride (CTAC) as dual templates and permitted the synthesis of spherical mesoporous silica with a high surface area (1011.42 m2/g). The MSN materials were characterized by FTIR, Thermogravimetric (TG), Nitrogen adsorption and desorption and Field emission scanning electron microscopic analysis (FESEM). The materials feasibility as solid phase adsorbent has been demonstrated using cationic dyes; Rhodamine B (RB) and methylene blue (MB) as models. Due to the large surface area and variable pore width, the adsorption behaviors toward cationic dyes showed outstanding removal efficiency and a rapid sorption rate. The adsorption isotherms of RB and MB were well-fitted to the Langmuir and Freundlich models, while the kinetic behaviours adhered closely to the pseudo-second-order pattern. The maximum adsorption capacities were determined to be 256 mg/g for MB and 110.3 mg/g for RB. The findings suggest that MSNs hold significant potential as solid-phase nanosorbents for the extraction and purification of dye pollutants, particularly in the analysis and treatment of effluents containing cationic dyes. Full article
(This article belongs to the Special Issue Advanced Aerogels: From Design to Application)
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<p>A comparison of EDS data (<b>a</b>) before and (<b>b</b>) after ion exchange.</p>
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<p>The infrared spectrum of mesoporous silica nanoparticles with CTAC/PEG composites (<b>a</b>) and after removal of CTAC and PEG molecules (<b>b</b>).</p>
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<p>Thermal analysis profiles of mesoporous silica nanoparticles after removal CTAC and PEG molecules.</p>
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<p>N<sub>2</sub> adsorption-desorption isotherm curves of MSNs. Inset show the linear ship of relative pressure. (<b>a</b>) MSN-1 (black), MSN-2 (red), MSN-3 (blue); (<b>b</b>) MSN-4 (black), MSN-5 (red).</p>
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<p>BJH pore size distribution plots of MSNs. (<b>a</b>) MSN-1 (black), MSN-2 (red), MSN-3 (blue); (<b>b</b>) MSN-4 (black), MSN-5 (red).</p>
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<p>SEM micrographs and size distributions of MSNs prepared from sodium silicate obtained with different PEG concentration (<b>a</b>,<b>b</b>) 0.55, (<b>c</b>,<b>d</b>) 1.1 (<b>e</b>,<b>f</b>) 1.38 (<b>g</b>,<b>h</b>), 1.65 (<b>i</b>,<b>j</b>), and 2.2 mM.</p>
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<p>SEM micrographs and size distributions of MSNs prepared from sodium silicate obtained with different PEG concentration (<b>a</b>,<b>b</b>) 0.55, (<b>c</b>,<b>d</b>) 1.1 (<b>e</b>,<b>f</b>) 1.38 (<b>g</b>,<b>h</b>), 1.65 (<b>i</b>,<b>j</b>), and 2.2 mM.</p>
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<p>The effect of pH vale on the adsorption efficiency of dye on MSNs.</p>
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<p>Experimental data and fitting models for MB: (<b>a</b>) UV-Vis spectra for initial concentration-dependent MB adsorption in the presence of mesoporous silica. (<b>b</b>) The residual concentration of MB in the solution at various times. (<b>c</b>) Experimental dynamic data for MB adsorption on MSNs, as well as typical nonlinear fitting data for the Elovich, pseudo-first order, and pseudo-second order models. (<b>d</b>) Experimental data for MSNs isothermal adsorption at various MB starting concentrations, as well as a nonlinear fitted curve based on Langmiur, Freundilich, and Redlich-Peterson isotherms (m = 100 mg, T = 25 °C, V<sub>0</sub> = 100 mL, t = 60 min).</p>
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<p>Experimental data and fitting models for RB: (<b>a</b>) Depicts UV-Vis spectra for initial concentration-dependent RB adsorption in the presence of mesoporous silica. (<b>b</b>) The residual concentration of MB in the solution at various times. (<b>c</b>) Experimental dynamic data for RB adsorption on MSNs, as well as typical nonlinear fitting data for the Elovich, pseudo-first order, and pseudo-second order models. (<b>d</b>) Experimental data for MSNs isothermal adsorption at various RB starting concentrations, as well as a nonlinear fitted curve based on Langmiur, Freundilich, and Redlich-Peterson isotherms (m = 100 mg, T = 25 °C, V<sub>0</sub> = 100 mL, t = 60 min).</p>
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14 pages, 5585 KiB  
Article
Improved Surface Properties of Low-Carbon Steel by Chromizing–Titanizing Coating Using Pack Cementation Process
by Ayman Yousef, A. M. Bastaweesy, Ibrahim M. Maafa and Ahmed Abutaleb
Metals 2024, 14(12), 1456; https://doi.org/10.3390/met14121456 - 19 Dec 2024
Viewed by 370
Abstract
This study investigates the application of chromizing and titanizing coatings on low-carbon steel (LCS) via the pack cementation process, utilizing various compositions, temperatures, and durations. The coating was analyzed using standard techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive [...] Read more.
This study investigates the application of chromizing and titanizing coatings on low-carbon steel (LCS) via the pack cementation process, utilizing various compositions, temperatures, and durations. The coating was analyzed using standard techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and Vickers hardness testing, to determine their characteristics. The kinetics of the pack chromizing, titanizing, and chromotitanizing of low-carbon steel exhibited parabolic behavior, with the rate constant with increasing temperature. The formed diffusion layers primarily consisted of Cr, Ti, Cr1.9Ti, FeTi, Al2O3, Cr2O3, TiO2, and Cr1.36Fe0.52, in addition to Fe. The microhardness reached its highest value of 900 HV0.01 Kgf with 48% FeTi, followed by 790 HV0.01 Kgf with 12% FeCr–36% FeTi, 730 HV0.01 Kgf with 24% FeCr–24% FeTi, 680 HV0.01 Kgf with 36% FeCr–12% FeTi, and 560 HV0.01 Kgf with 48% FeCr. The results indicate a significant enhancement in the mechanical properties of low-carbon steel through the coating process. This study confirms that the pack cementation coatings of chromizing, titanizing, and chromotitanizing significantly enhance the surface hardness and mechanical integrity of low-carbon steel. The controlled diffusion process leads to the formation of robust intermetallic layers, and the variation in FeCr and FeTi composition allows for tailored mechanical properties. Additionally, the results suggest that the interplay between Cr and Ti promotes the development of a complex, multilayered microstructure that balances hardness with potential toughness, providing a broad spectrum of industrial applications. This research underscores the versatility of pack cementation as an effective method to engineer advanced coatings, offering a cost-efficient pathway to enhance the performance of low-carbon steel in demanding environments. Full article
(This article belongs to the Topic Alloys and Composites Corrosion and Mechanical Properties)
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<p>Effect of process time on average coating thickness of coated specimens at different temperatures used: (<b>a</b>) 48% FeCr; (<b>b</b>) 36% FeCr–12% FeTi; (<b>c</b>) 24% FeCr–24% FeTi; (<b>d</b>) 12% FeCr–36% FeTi; and (<b>e</b>) 48% FeTi.</p>
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<p>Relationship between the square root of process time and average coating thickness of coated specimens at different temperatures used: (<b>a</b>) 48% FeCr; (<b>b</b>) 36% FeCr–12% FeTi; (<b>c</b>) 24% FeCr–24% FeTi; (<b>d</b>) 12% FeCr–36% FeTi; and (<b>e</b>) 48% FeTi.</p>
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<p>Arrhenius plot of parabolic rate constant versus inverse absolute temperature for average coating thickness of chromized, titanized, and chromotitanized LCS.</p>
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<p>Optical images of pack chromizing specimens at 900 °C for (<b>a</b>) 3 h, (<b>b</b>) 5 h, and (<b>c</b>) 7 h; at 1000 °C for (<b>d</b>) 3 h, (<b>e</b>) 5 h, and (<b>f</b>) 7 h; and at 1100 °C for (<b>g</b>) 3 h, (<b>h</b>) 5 h, and (<b>i</b>) 7 h.</p>
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<p>SEM images of coated samples consisting of (<b>a</b>) 24% FeTi–24% FeCr at 900 °C for 5 h, Reprinted from ref. [<a href="#B29-metals-14-01456" class="html-bibr">29</a>]; (<b>b</b>) 48% FeTi at 1000 °C for 5 h, Reprinted from ref. [<a href="#B29-metals-14-01456" class="html-bibr">29</a>]; (<b>c</b>) 48% FeCr at 900 °C for 3 h, Reprinted from ref. [<a href="#B29-metals-14-01456" class="html-bibr">29</a>]; (<b>d</b>) 48% FeTi at 1100 °C for 5 h; and (<b>e</b>) 24% FeTi–24% FeCr at 1100 °C for 7 h. (Pack composed of 48 wt% (Cr or Ti or CrTi), 50 wt% Al<sub>2</sub>O<sub>3</sub> powder, and 2 wt% NH<sub>4</sub>Cl).</p>
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<p>EDX distribution for the corresponding SEM images (<b>a</b>) 24% FeTi–24% FeCr at 900 °C for 5 h; (<b>b</b>) 48% FeTi at 1000 °C for 5 h; (<b>c</b>) 48% FeCr at 900 °C for 3 h; (<b>d</b>) 48% FeTi at 1100 °C for 5 h; and (<b>e</b>) 24% FeTi–24% FeCr at 1100 °C for 7 h. (Pack composed of 48 wt% (Cr or Ti or CrTi), 50 wt% Al<sub>2</sub>O<sub>3</sub> powder, and 2 wt% NH<sub>4</sub>Cl).</p>
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<p>XRD pattern of the coated specimen for (<b>a</b>) 48% FeCr, (<b>b</b>) 36% FeCr–12% FeTi, and (<b>c</b>) 48% FeTi at 1000 °C for 5 h.</p>
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<p>Cross-sectional micro-Vickers hardness profiles.</p>
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10 pages, 3832 KiB  
Communication
Resuspended Nano-Minerals in Coal Ash: A Potential Factor in Elevated Lung Cancer Rates in Xuanwei and Fuyuan, Yunnan, China
by Wenhua Wang, Mengyang Wang, Longyi Shao, Jiajia Shao and Pengju Liu
Toxics 2024, 12(12), 919; https://doi.org/10.3390/toxics12120919 - 19 Dec 2024
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Abstract
Xuanwei and the neighboring Fuyuan (XF) counties in Yunnan Province have the highest lung cancer incidence rates in China. Previous studies suggest that the nano-minerals released during the combustion of locally sourced “smoky” (bituminous) coal are the primary contributors to these elevated cancer [...] Read more.
Xuanwei and the neighboring Fuyuan (XF) counties in Yunnan Province have the highest lung cancer incidence rates in China. Previous studies suggest that the nano-minerals released during the combustion of locally sourced “smoky” (bituminous) coal are the primary contributors to these elevated cancer rates. The coal ash generated during combustion predominantly consists of nano-minerals, which can be resuspended into the atmosphere during routine ash-handling activities. In this study, coal ash samples from XF counties and four additional provinces with lower lung cancer incidence rates were resuspended to simulate ash-handling activities and subsequently collected using a cascade PM2.5 sampler. Individual particles were analyzed using a high-resolution scanning electron microscope coupled with energy-dispersive X-ray spectroscopy (SEM-EDX). Based on their morphology and elemental composition, the particles were categorized into five major types: quartz, Si- and Al-rich (SiAl-rich), Ca-rich, Ca- and Mg-rich (CaMg-rich), and Fe-rich particles. The relative abundance of crystalline quartz particles was significantly higher in Xuanwei (22.2%) and Fuyuan (13.7%) compared to the other provinces, where quartz was also detected in lower concentrations. Similarly, the proportion of Fe-rich particles was notably higher in Xuanwei (10.9%) and Fuyuan (5.1%) than in other regions. These findings highlight the potential role of quartz and Fe-rich particles in contributing to the high lung cancer rates observed in XF counties. Further research is warranted to elucidate the toxicological mechanisms underlying the health effects of these particle types. Full article
(This article belongs to the Section Air Pollution and Health)
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<p>Diagram showing coal burning and ash collection system.</p>
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<p>Morphology and elemental composition of quartz and SiAl-rich particles.</p>
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<p>Morphology and elemental composition of Ca-rich and CaMg-rich particles.</p>
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<p>Morphology and elemental composition of Fe-rich particles.</p>
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19 pages, 3322 KiB  
Article
Magnetic Composite Carbon from Microcrystalline Cellulose to Tackle Paracetamol Contamination: Kinetics, Mass Transfer, Equilibrium, and Thermodynamic Studies
by Pascal S. Thue, Alfred G. N. Wamba, Beatris L. Mello, Fernando M. Machado, Karoline F. Petroman, Willian Cézar Nadaleti, Robson Andreazza, Glaydson S. dos Reis, Mohamed Abatal and Eder C. Lima
Polymers 2024, 16(24), 3538; https://doi.org/10.3390/polym16243538 - 19 Dec 2024
Viewed by 339
Abstract
This study reported a one-spot preparation of magnetic composite carbon (MCC@Fe) from microcrystalline cellulose (MC). The pure cellulose was impregnated in iron (III) chloride solution and carbonized at 650 °C. The MCC@Fe composite adsorbent underwent various characterization techniques. XRD identified nanostructured Fe3 [...] Read more.
This study reported a one-spot preparation of magnetic composite carbon (MCC@Fe) from microcrystalline cellulose (MC). The pure cellulose was impregnated in iron (III) chloride solution and carbonized at 650 °C. The MCC@Fe composite adsorbent underwent various characterization techniques. XRD identified nanostructured Fe3O4 particles with an average crystallite size of 34.3 nm embedded in the core subunits of the material. FESEM images indicated a rough and irregular surface, with some cavities along its surface, incorporating Fe3O4 nanoparticles, while EDS analysis confirmed the presence of elements like Fe, C, and O. Notably, combining thermal and chemical treatments produces a composite with more pores and a high specific surface area (500.0 m2 g−1) compared to MC (1.5 m2/g). VSM analysis confirmed the magnetic properties (0.76 emu/g), while the Hydrophobic Index (HI) showed that MCC@Fe was hydrophobic (HI 1.395). The adsorption studies consisted of kinetic, mass transfer, equilibrium, and thermodynamics studies. Kinetic study of the adsorption of paracetamol on MCC@Fe composite proved to be rapid, and the time necessary for covering 95% of the surface (t0.95) was lower than 27 min following the fractal-like pseudo-first-order model (FPFO). Liu’s isotherm proved to be the most appropriate for understanding the adsorption equilibrium. Remarkably, the maximum sorption capacity (Qmax) of paracetamol was 34.78 mg g−1 at 45 °C. The ΔH° value (+27.00 kJ/mol) and the negative ΔG° values were consistent with the physisorption mechanism and favorable process. Furthermore, the mass transfer mechanism showed that the transfer is governed by the intraparticle diffusion model, with surface diffusion being the rate-limiting step when considering the Biot number greater than 100. This research displayed a single-route production of inexpensive magnetic nano adsorbents capable of efficiently eliminating paracetamol from aqueous environments. Full article
(This article belongs to the Section Polymer Applications)
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<p>(<b>a</b>) Diffractograms of raw CP (<span style="color:red">red line</span>) and MCC@Fe adsorbent (<span style="color:blue">blue line</span>). (<b>b</b>) VSM hysteresis loops of MCC@Fe at room temperature.</p>
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<p>SEM images of MCC@Fe adsorbent at different magnifications: (<b>a</b>) ×500 (<b>b</b>) ×700 and (<b>c</b>) ×2000.</p>
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<p>(<b>a</b>) FTIR spectra and (<b>b</b>) TGA/DTG curves of MCC@Fe magnetic composite.</p>
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<p>Kinetics curves at (<b>a</b>) 125.0 mg/L and (<b>b</b>) 250.0 mg/L, using MCC@Fe composite adsorbent (pH 7.0, 1.5 g L<sup>−1</sup> of adsorbent dosage, and 25 °C).</p>
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<p>(<b>a</b>,<b>b</b>) Film diffusion model. (<b>c</b>,<b>d</b>) Intraparticle diffusion model of adsorption of paracetamol on MCC@Fe composite. Initial pH at 7, temperature at 25 °C, initial concentrations at 125 mg/L (<b>a</b>,<b>c</b>) and 250 mg/L (<b>b</b>,<b>d</b>), and dose (<b>d</b>) adsorbent at 1.5 g/L.</p>
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<p>(<b>a</b>) Adsorption isotherm of uptake PCT onto MCC@Fe adsorbent at 45 °C. (<b>b</b>) Van’t Hoff graph for uptake of PCT onto MCC@Fe adsorbent. Conditions: 1.5 g L<sup>−1</sup> of adsorbent dosage; contact time, 60 min; and pH 7.</p>
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<p>Possible mechanism of interaction of PCT onto MCC@Fe.</p>
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<p>Desorption experiments of MCC@Fe composite for PCT.</p>
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