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Keywords = ultrafine-grain microstructure

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18 pages, 10785 KB  
Article
Microstructure, Texture, and Mechanical Properties of 6N Ultra-High-Purity Copper Processed by Cryorolling for Advanced Sputtering Targets
by Wenpeng Yuan, Shifeng Liu, Hang Zhao, Linyu Lu, Qiuyan Xie and Xinggui Lei
Metals 2025, 15(12), 1369; https://doi.org/10.3390/met15121369 - 12 Dec 2025
Viewed by 194
Abstract
The performance of ultra-high-purity copper sputtering targets is critical for nanoscale integrated circuit fabrication, yet challenges such as dynamic recovery and recrystallization hinder grain refinement and texture control. In the present work, cryogenic deformation was introduced to address these issues. Through electron backscatter [...] Read more.
The performance of ultra-high-purity copper sputtering targets is critical for nanoscale integrated circuit fabrication, yet challenges such as dynamic recovery and recrystallization hinder grain refinement and texture control. In the present work, cryogenic deformation was introduced to address these issues. Through electron backscatter diffraction (EBSD), X-ray diffraction (XRD), and mechanical testing, the microstructure, texture, and mechanical properties of 6N ultra-high-purity copper processed by room-temperature rolling (RTR) and cryorolling (CR) were comparatively investigated. Results reveal that RTR deformation is dominated by slip mechanisms; the RTR sample with 90% reduction exhibits obvious dynamic recrystallization (DRX) and forms a bimodal structure dominated by Copper ({112}⟨111⟩) and S ({123}⟨634⟩) textures. In contrast, CR suppresses thermal activation processes, enabling deformation mechanisms suggestive of twinning activity, leading to ultrafine fibrous structures, while shifting texture components toward Brass ({110}⟨112⟩) and S. Compared to RTR-processed samples, CR-processed samples possess superior mechanical performance. The CR sample with 90% reduction exhibits: a microhardness of 164.60 HV, a yield strength of 385.61 MPa, and a tensile strength of 648.02 MPa, which are, respectively, 33.2%, 91.7%, and 84.6% higher than those of RTR counterparts. Williamson–Hall analysis confirms that the CR sample with 90% reduction achieves finer substructure sizes (~133 nm) and higher stored energy (~22 J·mol−1) by suppressing dynamic recovery, providing a robust driving force for subsequent annealing. This work demonstrates that cryorolling optimizes microstructure and texture through twin-dislocation synergy, providing a fundamental basis for the development of advanced sputtering targets. Full article
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13 pages, 4315 KB  
Article
Formation of the Structure, Properties, and Corrosion Resistance of Zirconium Alloy Under Three-Roll Skew Rolling Conditions
by Anna Kawałek, Alexandr Arbuz, Kirill Ozhmegov, Irina Volokitina, Andrey Volokitin, Nikita Lutchenko and Fedor Popov
Materials 2025, 18(24), 5578; https://doi.org/10.3390/ma18245578 - 11 Dec 2025
Viewed by 237
Abstract
Zirconium and its alloys are widely used in nuclear power engineering due to their favorable physical and mechanical properties and their low thermal-neutron absorption cross-section. Their high corrosion resistance in aqueous and steam environments at elevated temperatures is essential for the reliable operation [...] Read more.
Zirconium and its alloys are widely used in nuclear power engineering due to their favorable physical and mechanical properties and their low thermal-neutron absorption cross-section. Their high corrosion resistance in aqueous and steam environments at elevated temperatures is essential for the reliable operation of fuel assemblies and is associated with the formation of a stable, compact ZrO2 oxide layer. However, under reactor conditions, the presence of hydrogen, iodine and other fission products can reduce corrosion resistance, making detailed corrosion assessment necessary. Manufacturing technology, alongside alloy composition, also plays a decisive role in determining corrosion behavior. This study presents corrosion test results for a Zr-1%Nb alloy processed under thermomechanical conditions corresponding to rolling in a special type of three-roll skew rolling–Radial-Shear Rolling (RSR). The applied rolling technology ensured the formation of a pronounced ultrafine-grained (UFG) structure in the near-surface layers, with an average grain size below 0.6 µm. EBSD and TEM observations revealed a largely equiaxed microstructure with refined grains and increased grain boundary density. The corrosion testing was performed in high-temperature steam vessels at 400 °C and 10.3 MPa for 72, 336, 720 and 1440 h. The results demonstrate that RSR processing is an efficient alternative to conventional multi-pass normal bar rolling with vacuum heat treatments, allowing a significant reduction in processing steps and eliminating the need for expensive tooling and intermediate thermal or chemical treatments. Bars manufactured using this method meet the ASTM B351 requirements. The specific weight gain did not exceed 22 mg/dm2 after 72 h and 34.5 mg/dm2 after 336 h. After 1440 h, the samples exhibited a continuous, uniform dark-grey oxide layer with an average thickness below 5.3 µm. Full article
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14 pages, 2965 KB  
Article
Study on Microstructure Evolution and Influencing Factors of Pure Copper Wire After Directional Heat Treatment
by Hao Xu, Xin Dong, Feixiang Chen, Yang Chen and Guang Chen
Crystals 2025, 15(11), 984; https://doi.org/10.3390/cryst15110984 - 14 Nov 2025
Cited by 1 | Viewed by 386
Abstract
The Ohon Continuous Casting is the main method for preparing single crystal copper wire, and it is also the research hotspot at present, but it is difficult to directly cast ultrafine single crystal copper wire (diameter < 0.05 mm). The copper wire obtained [...] Read more.
The Ohon Continuous Casting is the main method for preparing single crystal copper wire, and it is also the research hotspot at present, but it is difficult to directly cast ultrafine single crystal copper wire (diameter < 0.05 mm). The copper wire obtained by continuous casting must be drawn and deformed before it can be used in practice, but this will bring a series of problems such as single crystal structure destruction and conductivity deterioration. Directional heat treatment technology can control the direction of heat flow at a low temperature, realize the directional migration of grain boundaries in the recrystallization process, and form columnar crystals or single crystals, which is of great significance for improving electrical conductivity. In this paper, the directional heat treatment method was used to investigate the microstructure evolution and influencing factors of pure copper wire, the process parameters were optimized, and the conductivity of pure copper wire was measured. It was found that the conductivity of pure copper wire increased by 5% when the heating temperature was 750 °C and the withdrawing velocity was 15 μm/s, which laid a foundation for the improvement of conductivity of pure copper wire. Full article
(This article belongs to the Section Crystalline Metals and Alloys)
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25 pages, 6510 KB  
Article
Enhancing Dry-Sliding Wear Performance of a Powder-Metallurgy-Processed “Metal Matrix–Carbide” Composite via Laser Surface Modification
by Yuliia Chabak, Vasily Efremenko, Yevhen Barma, Ivan Petrišinec, Bohdan Efremenko, František Kromka, Ivan Sili and Taras Kovbasiuk
Eng 2025, 6(11), 313; https://doi.org/10.3390/eng6110313 - 5 Nov 2025
Cited by 1 | Viewed by 504
Abstract
The increasing demand for enhanced wear resistance and mechanical integrity in tooling applications has driven the development of advanced surface engineering strategies for high-alloy steels. Böhler K390 MICROCLEAN, a powder-metallurgical V–Cr–Mo–W cold work tool steel with high vanadium content, features a composite metal [...] Read more.
The increasing demand for enhanced wear resistance and mechanical integrity in tooling applications has driven the development of advanced surface engineering strategies for high-alloy steels. Böhler K390 MICROCLEAN, a powder-metallurgical V–Cr–Mo–W cold work tool steel with high vanadium content, features a composite metal matrix–carbide microstructure, consisting of uniformly distributed coarse vanadium carbides and finer carbides (M7C3, M6C/MC) embedded in a ferritic matrix. This study investigated the effects of non-melting laser surface treatment (LST) applied to both as-received and bulk heat-treated K390 specimens. Microstructural characterization using SEM, EBSD, XRD, and EDX revealed the formation of a hardened surface layer comprising a structureless mixture of ultrafine-grained martensite and retained austenite, localized around vanadium carbides. Lattice parameter analysis and Williamson–Hall evaluation demonstrated increased carbon content, lattice distortion, and crystallite size reduction, contributing to high dislocation density (6.4 × 1014 to 2.6 × 1015 m−2) and enhanced hardness. Microhardness was increased by up to 160% compared to the initial state (reaching 835–887 HV20), and dry-sliding testing showed up to 3.94 times reduced volume loss and decreased friction coefficients. Wear occurred via the formation and delamination of thin oxide tribo-layers, which enhanced the wear behavior. The combined approach of bulk heat treatment followed by LST produced a graded microstructure with superior mechanical stability, offering clear advantages for extending tool life under severe contact loads in stamping and forming operations. Full article
(This article belongs to the Special Issue Advances in Precision Machining and Surface Engineering of Materials)
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17 pages, 15551 KB  
Article
Composition Optimization and Microstructure-Property Investigation of Al-3.0Ce-xCa-yMn Alloy Exhibiting High Hot Tearing Resistance
by Xiaoxiao Wei, Suhui Zhang, Xiaofei Wang, Yulin Teng, Wanwen Zhang and Mengmeng Wang
Metals 2025, 15(11), 1195; https://doi.org/10.3390/met15111195 - 27 Oct 2025
Viewed by 480
Abstract
This study employs a combined approach of theoretical calculations and experimental validation to systematically optimize the alloy composition, aiming to mitigate the hot cracking susceptibility of an Al-3.0Ce-xCa-yMn alloy in laser powder bed fusion (LPBF) processing. Through advanced characterization techniques such as electron [...] Read more.
This study employs a combined approach of theoretical calculations and experimental validation to systematically optimize the alloy composition, aiming to mitigate the hot cracking susceptibility of an Al-3.0Ce-xCa-yMn alloy in laser powder bed fusion (LPBF) processing. Through advanced characterization techniques such as electron backscatter diffraction (EBSD), transmission electron microscopy (TEM), and mechanical property testing, the intrinsic relationship between microstructure and mechanical performance was thoroughly elucidated. Computational results revealed that the addition of Ca significantly lowered the eutectic precipitation temperature, thereby effectively reducing the hot cracking tendency while maintaining a stable volume fraction of the Al11(Ce, Ca)3 phase. The optimal mass fractions of calcium (Ca) and manganese (Mn) were determined to be 0.8% and 1.9%, respectively. Microstructural characterization indicates that the alloy consisted of an α-Al matrix embedded with Al-Ce-Ca ternary eutectic compounds, and nanoscale Al6Mn spherical precipitates were uniformly distributed within the matrix. Mechanical property evaluations demonstrated that the Al-3Ce-0.8Ca-1.9Mn alloy exhibited an outstanding balance of strength and ductility at both room and elevated temperatures, with room temperature yield strength, tensile strength, and elongation values of 321 ± 15 MPa, 429 ± 8 MPa, and 10.9 ± 2.3%, respectively. This exceptional performance was attributed to a synergistic combination of multiple strengthening mechanisms including eutectic structure-induced strengthening, grain boundary strengthening due to ultrafine grains, and dislocation pinning strengthening caused by nano-sized Al6Mn precipitates. Full article
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19 pages, 4904 KB  
Article
Room-Temperature Superplasticity in a Biodegradable Zn-0.1Mg Alloy
by Karel Saksl, Róbert Kočiško, Patrik Petroušek, Miloš Matvija, Martin Fujda, Dávid Csík, Zuzana Molčanová, Beáta Ballóková, Iryna Cuperová, Katarína Gáborová, Maksym Lisnichuk, Miloslav Lupták and Adam Lupták
Metals 2025, 15(10), 1161; https://doi.org/10.3390/met15101161 - 21 Oct 2025
Viewed by 406
Abstract
Biodegradable zinc-based alloys have recently emerged as promising candidates for temporary biomedical implants due to their favorable biocompatibility, appropriate degradation rate, and relatively simple processing. In this study, the Zn-0.1Mg alloy was investigated after being processed by means of a two-step equal-channel angular [...] Read more.
Biodegradable zinc-based alloys have recently emerged as promising candidates for temporary biomedical implants due to their favorable biocompatibility, appropriate degradation rate, and relatively simple processing. In this study, the Zn-0.1Mg alloy was investigated after being processed by means of a two-step equal-channel angular pressing (ECAP) route, consisting of the first pass at 150 °C followed by a second pass at room temperature. The mechanical properties were evaluated using uniaxial tensile tests at different strain rates, while the microstructure and phase composition were analyzed using synchrotron hard X-ray diffraction and transmission electron microscopy (TEM). The processed alloy exhibited a remarkable enhancement in both strength and ductility compared to the annealed state. At the lowest applied strain rate, a fracture elongation of up to 240% was achieved at room temperature, representing a unique manifestation of superplasticity under ambient conditions. Diffraction analysis confirmed the stability of the supersaturated Zn matrix with minor Mg2Zn11 intermetallic phase. TEM observations revealed an ultrafine-grained microstructure and activation of non-basal slip systems, which enabled efficient plastic flow. These findings demonstrate that controlled severe plastic deformation provides an effective pathway for tailoring Zn-Mg alloys, opening opportunities for their use in the next generation of bioresorbable low-to-moderate load orthopedic fixation devices, e.g., plates, screws, suture anchors and craniofacial miniplates. Full article
(This article belongs to the Special Issue The Forming Behaviour and Plasticity of Metallic Alloys)
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15 pages, 4007 KB  
Article
Investigation on the Mechanical Properties of White Layers by Cutting and Burnishing Coupling Effect in BTA Deep Hole Drilling
by Huang Zhang, Pengxiang Yan, Haoran Guo, Ze Chen, Zihao Hou and Yaoming Li
J. Manuf. Mater. Process. 2025, 9(9), 319; https://doi.org/10.3390/jmmp9090319 - 20 Sep 2025
Viewed by 830
Abstract
The unique cutting–burnishing coupling effect in BTA deep hole drilling generates a high-hardness and -brittleness white layer (ultrafine martensitic layer), which will degrade component performance and accelerate tool wear. This work investigated the formation mechanism and the mechanical properties of the white layer [...] Read more.
The unique cutting–burnishing coupling effect in BTA deep hole drilling generates a high-hardness and -brittleness white layer (ultrafine martensitic layer), which will degrade component performance and accelerate tool wear. This work investigated the formation mechanism and the mechanical properties of the white layer generated in three distinct regions (the cutting edge radius zone, cutting–burnishing corner zone, and guide pad edge zone) through nanoindentation, SEM and BSE. The microstructure and thickness of the white layer under different feedrates are investigated. The correlations between the white layer, the structure of guide pads, and wear behaviors of the TiN- and TiCN/Al2O3-coated guide pads are revealed. Variations in hardness are observed across different zones. The white layer undergoes a soft-to-hard transition due to rapid quenching and the cutting–burnishing effect at the sharp corner. The highest hardness (9.758 GPa) was observed in the guide pad zone, accompanied by grain refinement. The chamfered TiN-coated guide pad exhibits superior wear resistance but suffers fatigue cracking and adhesive wear in the initial guiding zone. The TiCN/Al2O3-coated pad with rounded corners experiences brittle spalling in the mid-to-rear guiding zone. These findings enhance the understanding of the white layer formation in deep hole drilling and provide a foundation for tool optimization. Full article
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16 pages, 9544 KB  
Article
Solid-State Recycling of AA6063 Aluminum Chips via Accumulative Roll Bonding: A Green Pathway to High-Performance Materials
by Mauro Carta, Noomane Ben Khalifa, Pasquale Buonadonna, Francesco Aymerich and Mohamad El Mehtedi
Metals 2025, 15(9), 1042; https://doi.org/10.3390/met15091042 - 19 Sep 2025
Viewed by 3636
Abstract
Accumulative Roll Bonding (ARB) is a severe plastic deformation process typically used to produce ultra-fine-grained structures. This study investigates the feasibility of using the ARB process to recycle aluminum chips from an Al-Mg-Si alloy (AA6063). The chips were first compacted under a 200 [...] Read more.
Accumulative Roll Bonding (ARB) is a severe plastic deformation process typically used to produce ultra-fine-grained structures. This study investigates the feasibility of using the ARB process to recycle aluminum chips from an Al-Mg-Si alloy (AA6063). The chips were first compacted under a 200 kN hydraulic press and then directly hot-rolled at 550 °C without prior heat treatment to a final sheet thickness of 1.5 mm. Subsequent ARB cycles were then applied to achieve full consolidation. Mechanical properties were evaluated through tensile testing and microhardness measurements, while microstructure was characterized using Optical Microscopy and SEM-EBSD. These analyses revealed significant grain refinement and improved homogeneity with increasing ARB cycles. Mechanical testing showed that the ARB process substantially enhanced both tensile strength and hardness of the recycled AA6063 chips while maintaining good ductility. The best results were obtained after two ARB cycles, yielding an ultimate tensile strength (UTS) of 170 MPa and an elongation at rupture of 15.7%. The study conclusively demonstrates that the ARB process represents a viable and effective method for recycling aluminum chips. This approach not only significantly improves mechanical properties and microstructural characteristics but also offers environmental benefits by eliminating the energy-intensive melting stage. Full article
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23 pages, 6297 KB  
Article
Laser-Driven Surface Alloying of Ti6Al4V: Coupled Microstructural Evolution, Phase Behavior, and Mechanical Performance
by Hana Beyene Mamo, Klaudiusz Gołombek, Gilmar Ferreira Batalha and Marcin Adamiak
Materials 2025, 18(18), 4237; https://doi.org/10.3390/ma18184237 - 9 Sep 2025
Viewed by 846
Abstract
This study investigates the microstructural and mechanical evolution of Ti6Al4V alloy surfaces modified through laser surface alloying (LSA) with antimicrobial elements silver (Ag) and copper (Cu) to enhance surface performance for biomedical applications. The as-received Ti6Al4V exhibited a typical equiaxed α-β [...] Read more.
This study investigates the microstructural and mechanical evolution of Ti6Al4V alloy surfaces modified through laser surface alloying (LSA) with antimicrobial elements silver (Ag) and copper (Cu) to enhance surface performance for biomedical applications. The as-received Ti6Al4V exhibited a typical equiaxed α-β microstructure with baseline hardness. Following LSA treatment using a 1000 W pulsed laser, distinct transformations were observed in the melt zone (MZ) and heat-affected zone (HAZ), influenced by the specific alloying element. Ag incorporation led to the development of ultrafine acicular martensitic structures and a higher fraction of high-angle grain boundaries, resulting in moderate hardness improvement. In contrast, Cu alloying promoted the formation of Ti2Cu intermetallic phases, dendritic morphologies, and pronounced solute segregation, leading to a more significant increase in hardness. Electron Backscatter Diffraction(EBSD) and Energy Dispersive Spectroscopy (EDS) analyses revealed grain refinement, texture evolution, and elemental redistribution across the modified regions, while X-ray Diffraction XRD confirmed the presence of new phases. The comparative analysis highlights that although both Ag and Cu improve microstructural complexity and hardness, Cu-modified zones exhibited higher hardness values than Ag-modified zones, suggesting a stronger surface strengthening effect under the tested conditions. These findings contribute valuable insights into the structure–property relationships of LSA-modified Ti alloys, supporting their potential for durable and antimicrobial biomedical implants. Full article
(This article belongs to the Special Issue Microstructure Engineering of Metals and Alloys, 3rd Edition)
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12 pages, 9490 KB  
Article
Effect of Ultra-Rapid Heating/Cooling on the Microstructure and Properties of TC4-B-Si Titanium Matrix Composites
by Xiaonan Lu, Jianchao Li, Cheng Liu, Likun Wang, Sainan Ma, Bo Yuan, Bowen Gong, Wenting Ouyang, Huan Wang, Xiang Gao, Huiping Tang and Hua-Xin Peng
Materials 2025, 18(18), 4223; https://doi.org/10.3390/ma18184223 - 9 Sep 2025
Viewed by 901
Abstract
Titanium matrix composites (TMCs) possess excellent properties, which are widely applied in various high-end fields. An ultrafine multi-scale network structure may further enhance the TMCs. Then, the application potential is widened. Here, the in situ synthesized TC4-B-Si composites were prepared by selective laser [...] Read more.
Titanium matrix composites (TMCs) possess excellent properties, which are widely applied in various high-end fields. An ultrafine multi-scale network structure may further enhance the TMCs. Then, the application potential is widened. Here, the in situ synthesized TC4-B-Si composites were prepared by selective laser melting technology, to achieve ultrafine microstructure by inducing ultra-rapid heating/cooling process. The preparation process–structure–performance relationships were investigated. It was found that an appropriate laser energy density leads to high-density TMCs with stable molten pools and good interlayer bonding. With the decreasing energy density, the in situ generated TiB network structure is refined from the sub-micron scale to the nano-scale. The most Si atoms are supersaturated solid-dissolved in the titanium matrix. In addition, the TiB distribution becomes heterogeneous. Due to the co-effect of grain refinement and reinforcement distribution, the microhardness shows a rising and then falling trend, with decreasing energy density. With a good balance of these two factors, the maximum value of microhardness reaches 454 HV. Therefore, controlling process parameters is a feasible way to achieve multi-structures, and thus enhanced properties. This method is expected to be used on various lightweight and wear-resistant structural components. Full article
(This article belongs to the Section Metals and Alloys)
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22 pages, 9293 KB  
Article
Thermal Stability of the Ultra-Fine-Grained Structure and Mechanical Properties of AlSi7MgCu0.5 Alloy Processed by Equal Channel Angular Pressing at Room Temperature
by Miloš Matvija, Martin Fujda, Ondrej Milkovič, Marek Vojtko and Katarína Gáborová
Crystals 2025, 15(8), 701; https://doi.org/10.3390/cryst15080701 - 31 Jul 2025
Viewed by 735
Abstract
Understanding the limitations of cold-formed aluminum alloys in practice applications is essential, particularly due to the risk of substructural changes and a reduction in strength when exposed to elevated temperatures. In this study, the thermal stability of the ultra-fine-grained (UFG) structure formed by [...] Read more.
Understanding the limitations of cold-formed aluminum alloys in practice applications is essential, particularly due to the risk of substructural changes and a reduction in strength when exposed to elevated temperatures. In this study, the thermal stability of the ultra-fine-grained (UFG) structure formed by equal channel angular pressing (ECAP) at room temperature and the mechanical properties of the AlSi7MgCu0.5 alloy were investigated. Prior to ECAP, the plasticity of the as-cast alloy was enhanced by a heat treatment consisting of solution annealing, quenching, and artificial aging to achieve an overaged state. Four repetitive passes via ECAP route A resulted in the homogenization of eutectic Si particles within the α-solid solution, the formation of ultra-fine grains and/or subgrains with high dislocation density, and a significant improvement in alloy strength due to strain hardening. The main objective of this work was to assess the microstructural and mechanical stability of the alloy after post-ECAP annealing in the temperature range of 373–573 K. The UFG microstructure was found to be thermally stable up to 523 K, above which notable grain and/or subgrain coarsening occurred as a result of discontinuous recrystallization of the solid solution. Mechanical properties remained stable up to 423 K; above this temperature, a considerable decrease in strength and a simultaneous increase in ductility were observed. Synchrotron radiation X-ray diffraction (XRD) was employed to analyze the phase composition and crystallographic characteristics, while transmission electron microscopy (TEM) was used to investigate substructural evolution. Mechanical properties were evaluated through tensile testing, impact toughness testing, and hardness measurements. Full article
(This article belongs to the Special Issue Celebrating the 10th Anniversary of International Crystallography)
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14 pages, 4080 KB  
Article
High-Compressive-Strength Silicon Carbide Ceramics with Enhanced Mechanical Performance
by Zijun Qian, Kang Li, Yabin Zhou, Hao Xu, Haiyan Qian and Yihua Huang
Materials 2025, 18(15), 3598; https://doi.org/10.3390/ma18153598 - 31 Jul 2025
Viewed by 1032
Abstract
This study demonstrates the successful fabrication of high-performance reaction-bonded silicon carbide (RBSC) ceramics through an optimized liquid silicon infiltration (LSI) process employing multi-modal SiC particle gradation and nano-carbon black (0.6 µm) additives. By engineering porous preforms with hierarchical SiC distributions and tailored carbon [...] Read more.
This study demonstrates the successful fabrication of high-performance reaction-bonded silicon carbide (RBSC) ceramics through an optimized liquid silicon infiltration (LSI) process employing multi-modal SiC particle gradation and nano-carbon black (0.6 µm) additives. By engineering porous preforms with hierarchical SiC distributions and tailored carbon sources, the resulting ceramics achieved a compressive strength of 2393 MPa and a flexural strength of 380 MPa, surpassing conventional RBSC systems. Microstructural analyses revealed homogeneous β-SiC formation and crack deflection mechanisms as key contributors to mechanical enhancement. Ultrafine SiC particles (0.5–2 µm) refined pore architectures and mediated capillary dynamics during infiltration, enabling nanoscale dispersion of residual silicon phases and minimizing interfacial defects. Compared to coarse-grained counterparts, the ultrafine SiC system exhibited a 23% increase in compressive strength, attributed to reduced sintering defects and enhanced load transfer efficiency. This work establishes a scalable strategy for designing RBSC ceramics for extreme mechanical environments, bridging material innovation with applications in high-stress structural components. Full article
(This article belongs to the Section Advanced and Functional Ceramics and Glasses)
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15 pages, 6582 KB  
Article
Microstructure and Mechanical Properties of the TC4 Alloy Obtained by Equal-Channel Angular Pressing in Combination with Reversible Hydrogen Alloying
by Irina P. Semenova, Luiza R. Rezyapova, Alexander V. Polyakov, Yuecheng Dong, Zhonggang Sun and Igor V. Alexandrov
Metals 2025, 15(8), 839; https://doi.org/10.3390/met15080839 - 27 Jul 2025
Viewed by 690
Abstract
This paper studies the effect of reversible hydrogen alloying of the TC4 alloy on the microstructure, phase composition, and mechanical properties before and after equal-channel angular pressing. It is shown that the introduction of 0.3% hydrogen followed by quenching from a temperature of [...] Read more.
This paper studies the effect of reversible hydrogen alloying of the TC4 alloy on the microstructure, phase composition, and mechanical properties before and after equal-channel angular pressing. It is shown that the introduction of 0.3% hydrogen followed by quenching from a temperature of 850 °C leads to the formation of a thin-plate α″-martensite, which made it possible to implement 6 passes (ε ~ 4.2) of pressing at 600 °C. As a result of the deformation of the TC4-H alloy and subsequent thermal vacuum treatment to remove hydrogen, an ultrafine-grained structure with an average size of the α-phase of 0.15 μm was formed, which led to strengthening of the alloy to 1490 MPa with a relative elongation of about 5% at room temperature. The reasons for a more significant refinement of the grain/subgrain structure and an increase in the tensile strength of the hydrogenated alloy after equal-channel angular pressing in comparison with hydrogen-free TC4 alloy are discussed. Full article
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26 pages, 10667 KB  
Article
Influence of Nitrogen and Hydrogen Addition on Composition, Morphology, Adhesion, and Wear Resistance of Amorphous Carbon Coatings Produced by RFCVD Method on Surface-Hardened Ultra-Fine Grained Bainitic 30HGSNA Steel
by Karol Wunsch, Tomasz Borowski, Emilia Skołek, Agata Roguska, Rafał Chodun, Michał Urbańczyk, Krzysztof Kulikowski, Maciej Spychalski, Andrzej Wieczorek and Jerzy Robert Sobiecki
Coatings 2025, 15(8), 877; https://doi.org/10.3390/coatings15080877 - 26 Jul 2025
Cited by 1 | Viewed by 2719
Abstract
Ultra-fine-grained bainitic (UFGB) steels offer excellent mechanical properties, which can be further improved by applying diamond-like carbon (DLC) coatings. However, poor adhesion between the coating and substrate remains a key limitation. Since the steel’s microstructure degrades at high temperatures, enhancing adhesion without heating [...] Read more.
Ultra-fine-grained bainitic (UFGB) steels offer excellent mechanical properties, which can be further improved by applying diamond-like carbon (DLC) coatings. However, poor adhesion between the coating and substrate remains a key limitation. Since the steel’s microstructure degrades at high temperatures, enhancing adhesion without heating the substrate is essential. This study investigates surface hardening combined with simultaneous nitrogen and hydrogen doping during the Radio Frequency Chemical Vapor Deposition (RFCVD) process to improve coating performance. Varying gas compositions were tested to assess their effects on coating properties. Nitrogen incorporation decreased hardness from 12 GPa to 9 GPa but improved adhesion, while hydrogen limited damage after coating failure. Optimizing the gas mixture led to enhanced adhesion and wear resistance. Raman and X-ray photoelectron spectroscopy (XPS) analyses confirmed that the optimized coatings had the highest sp3 bond content and elevated nitrogen levels. While both hardness and adhesion contributed to wear resistance, no direct link to coating thickness was found. Overall, co-doping with nitrogen and hydrogen is an effective approach to improve adhesion and wear resistance without requiring high processing temperatures or complex equipment. Full article
(This article belongs to the Special Issue Recent Advances in Surface Functionalisation, 2nd Edition)
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17 pages, 4068 KB  
Article
Mechanical Properties and Tribological Behavior of Al2O3–ZrO2 Ceramic Composites Reinforced with Carbides
by Jana Andrejovská, Dávid Medveď, Marek Vojtko, Richard Sedlák, Piotr Klimczyk and Ján Dusza
Lubricants 2025, 13(7), 310; https://doi.org/10.3390/lubricants13070310 - 17 Jul 2025
Cited by 1 | Viewed by 1133
Abstract
To elucidate the key material parameters governing the tribological performance of ceramic composites under dry sliding against steel, this study presents a comprehensive comparative assessment of the microstructural characteristics, mechanical performance, and tribological behavior of two alumina–zirconia (Al2O3–ZrO2 [...] Read more.
To elucidate the key material parameters governing the tribological performance of ceramic composites under dry sliding against steel, this study presents a comprehensive comparative assessment of the microstructural characteristics, mechanical performance, and tribological behavior of two alumina–zirconia (Al2O3–ZrO2) ceramic composites, each reinforced with a 42 vol.% carbide phase: zirconium carbide (ZrC) and tungsten carbide (WC). Specifically, tungsten carbide (WC) was selected for its exceptional bulk mechanical properties, while zirconium carbide (ZrC) was chosen to contrast its potentially different interfacial reactivity against a steel counterface. ZrC and WC were selected as reinforcing phases due to their high hardness and distinct chemical and interfacial properties, which were expected to critically affect the wear and friction behavior of the composites under demanding conditions. Specimens were consolidated via spark plasma sintering (SPS). The investigation encompassed macro- and nanoscale hardness measurements (Vickers hardness HV1, HV10; nanoindentation hardness H), elastic modulus (E), fracture toughness (KIC), coefficient of friction (COF), and specific wear rate (Ws) under unlubricated reciprocating sliding against 100Cr6 steel at normal loads of 10 N and 25 N. The Al2O3–ZrO2–WC composite exhibited an ultrafine-grained microstructure and markedly enhanced mechanical properties (HV10 ≈ 20.9 GPa; H ≈ 33.6 GPa; KIC ≈ 4.7 MPa·m½) relative to the coarse-grained Al2O3–ZrO2–ZrC counterpart (HV10 ≈ 16.6 GPa; H ≈ 27.0 GPa; KIC ≈ 3.2 MPa·m½). Paradoxically, the ZrC-reinforced composite demonstrated superior tribological performance, with a low and load-independent specific wear rate (Ws ≈ 1.2 × 10−9 mm3/Nm) and a stable steady-state COF of approximately 0.46. Conversely, the WC-reinforced system exhibited significantly elevated wear volumes—particularly under the 25 N regime—and a higher, more fluctuating COF. Scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM–EDX) of the wear tracks revealed the formation of a continuous, iron-enriched tribofilm on the ZrC composite, derived from counterface material transfer, whereas the WC composite surface displayed only sparse tribofilm development. These findings underscore that, in steel-paired tribological applications of Al2O3–ZrO2–based composites, the efficacy of interfacial tribolayer generation can supersede intrinsic bulk mechanical attributes as the dominant factor governing wear resistance. Full article
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