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Microstructure, Crystallography, and Mechanical Properties of Metallic Materials

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A special issue of Metals (ISSN 2075-4701). This special issue belongs to the section "Crystallography and Applications of Metallic Materials".

Deadline for manuscript submissions: closed (28 February 2026) | Viewed by 12501

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Special Issue Editors

Dr. Aman Gupta

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Guest Editor

Department of Advanced Components and Materials Engineering, Sunchon National University, Suncheon 57922, Republic of Korea
Interests: crystallographic texture; grain boundary engineering; electron microscopy; plastic deformation; metals and alloys

Dr. Gyan Shankar

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Guest Editor

Oak Ridge National Laboratory, Oak Ridge, TN, USA
Interests: materials engineering; additive manufacturing; deformation; recrystallization; texture

Special Issue Information

Dear Colleagues,

Microstructures are the building blocks used by the metallurgist to understand the behavior of metallic materials through the examination of grain morphology, orientations, dislocations, second phase particles, precipitates/intermetallics, etc. Working with the optical microscope or electron microscope (SEM, EBSD, TEM) has its advantages in terms of its cost effectiveness and level of magnification and resolution. Thermomechanical processing (TMP) of any metals or alloys is one of the necessary preliminary steps before its application. The arrangement of grains changes during the TMP, and hence it also affects the crystallographic texture. Most of the manufacturing processes, such as cold/hot deformation, additive manufacturing, welding/joining, severe plastic deformation, etc., are involved in the fabrication of a component that changes the crystallographic texture of metals and alloys. TMP also has a significant effect on the mechanical properties of the alloys. Mechanical properties such as yield strength, ductility, and micro-hardness are the important design parameters which are used by every metallurgist and mechanical engineer during the manufacturing of an engineering component for structural application. Hence, it is very important to understand the correlation between microstructural and crystallographic texture evolution with the mechanical properties of the materials for any application.

This topics of Special Issue include, but are not limited to:

Welding behavior of BCC/FCC materials.
Plastic deformation of metals/alloys.
Electron Back-Scattered Diffraction (EBSD) study.
Crystallographic texture (micro- and macro-texture).
Refractory complex concentrated alloys (RCCA).
High-entropy alloys and textures.
Friction stirs processing and mechanical properties.
Phase transformation in stainless steels.
Recrystallization behavior of Beta-Ti alloys.
Cryogenic deformation and EBSD study.
Nucleation and grain growth phenomena in BCC/FCC.
Design of new microstructures in additive manufacturing.

The above-mentioned keywords cover the various aspects of microstructure and crystallographic texture evolution. The publications in this Special Issue will give a thorough understanding of SEM, EBSD, and XRD to the scientific community.

Dr. Aman Gupta
Dr. Gyan Shankar
Guest Editors

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Keywords

microstructure
crystallographic texture evolution
mechanical properties
metallic materials
recrystallization behavior
texture
recrystallization behavior
grain growth

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Published Papers (8 papers)

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Research

14 pages, 10237 KB

Open AccessArticle

A Correlation with the Deformation Stored Energy and Self-Annealing Behavior of ETP-Cu

by Aman Gupta and Saurabh Tiwari

Metals 2026, 16(4), 432; https://doi.org/10.3390/met16040432 (registering DOI) - 17 Apr 2026

Abstract

In the present study, room temperature (RTR) and cryogenic (CR) rolling of electrolytic tough pitch copper (ETP-Cu) was performed to elucidate how deformation temperature and reduction ratio (40% and 80% thickness reductions) control dislocation storage, local stored energy (SE), and self-annealing. Correlated SEM/EDS and EBSD analyses were used to (i) locate Cu₂O particles, (ii) quantify local misorientation, and (iii) map the SE for self-annealing. Point EDS confirms that the intermetallic particles are copper oxides (Cu₂O), with apparent O content varying with particle size and EDS interaction volume. RTR80 (80% rolled) exhibits systematically higher KAM values and a larger area fraction of high SE than RTR40 (40% rolled), explaining the greater frequency and spatial density of self-annealed grains at higher reduction. Cryogenic rolling produces more severe fragmentation and a higher fraction of subgrains than RTR at equivalent reductions. CR80 shows the high KAM structures and locally highest SE regions among all conditions, and a higher fraction of self-annealed grains. Nevertheless, the mapped average SE for CR80 (2.93 × 10⁶ J/m³) was lower than for RTR80 (3.34 × 10⁶ J/m³) due to rapid post-deformation dislocation annihilation/self-annealing upon warming at RT. In all conditions, Cu₂O particles and bulged/irregular grain boundaries concentrate dislocations and SE and act as dominant particle-stimulated nucleation (PSN) sites and RT recrystallization, respectively. These results demonstrate that deformation temperature and reduction jointly determine the spatial distribution of SE and hence the propensity for self-annealing in ETP Cu. Full article

(This article belongs to the Special Issue Microstructure, Crystallography, and Mechanical Properties of Metallic Materials)

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11 pages, 3106 KB

Open AccessCommunication

Distribution of Twin Boundaries on Three-Dimensional Grains of 316L Stainless Steel

by Tingguang Liu, Guanglei Wang and Shuang Xia

Metals 2026, 16(3), 288; https://doi.org/10.3390/met16030288 - 4 Mar 2026

Viewed by 329

Abstract

The revelation of the distribution of twin boundaries on three-dimensional (3D) grains is of critical importance for the comprehension of their influence on material properties. However, this remains a significant challenge in the field of 3D material characterization. In this study, the distribution of twin boundaries on the surfaces of 3D grains in solution-annealed 316L stainless steel was systematically and quantitatively characterized using 3D electron backscatter diffraction. The results show that the average size of twin boundaries is significantly larger than that of random boundaries (approximately 52% larger). Although the size distributions of grains, random boundaries, and twin boundaries, as well as the distributions of the total number of grain boundaries and the number of twin boundaries per grain, all conform to a lognormal distribution, the area fraction of twin boundaries on grain surfaces exhibits a typical Lorentz distribution, while their number fraction shows no clear pattern. On average, each grain possesses 9.6 boundaries, of which 1.7 are twin boundaries, and the average area coverage of twin boundaries on grain surfaces reaches 38.4%. The findings offer a 3D statistical foundation for optimizing grain boundary engineering strategies in austenitic alloys. Full article

(This article belongs to the Special Issue Microstructure, Crystallography, and Mechanical Properties of Metallic Materials)

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19 pages, 7270 KB

Open AccessArticle

Evaluation of Microstructure and Tensile Properties of Al-12Si-4Cu-2Ni-0.5Mg Alloy Modified with Ca/P and TCB Complex

by Yuan Sun, Xiaoming Ren, Xueting Li, Hong Duan, Weiyi Wang, Mengxia Han, Guiliang Liu, Sida Liu and Xiangfa Liu

Metals 2025, 15(11), 1276; https://doi.org/10.3390/met15111276 - 20 Nov 2025

Viewed by 588

Abstract

The room-temperature and high-temperature microstructural characteristics and tensile properties of an Al-12Si-4Cu-2Ni-0.5Mg piston alloy modified with calcium (Ca; denoted as AC sample) or phosphorus (P; denoted as AP sample) under different heat treatment conditions were systematically analyzed. Under Ca modification, the second-phase network structure of the alloy was adjusted and strengthened by an Al-TCB master alloy. Eutectic silicon (Si) particles in the AC sample possessed a fibrous structure, whereas the AP sample contained elongated eutectic Si particles, and Ca modification was found to be a potential method for simultaneously enhancing the strength and plasticity of the alloy to a matching degree at high temperatures. The T6 treatment noticeably increased the density of nanoscale precipitates; however, it also disrupted the growth of the second-phase network structure. Micron and submicron C-TiB₂ and Al₄C₃ particles formed by the in-situ reaction of TCB particles acted as bridging phases within the second-phase network structure and enhanced the strength of the piston alloy. The ultimate tensile strength of the alloy at 350 °C increased from 74 to 101 MPa, representing a 36.5% enhancement. A comprehensive analysis revealed that Orowan strengthening was the main strengthening mechanism of the alloy at room temperature, whereas load transfer and network structure strengthening were the dominant strengthening mechanisms at high temperatures. Full article

(This article belongs to the Special Issue Microstructure, Crystallography, and Mechanical Properties of Metallic Materials)

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12 pages, 4386 KB

Open AccessArticle

The Role of Local Orientations Gradients in the Formation of the Recrystallisation Texture in Cold-Rolled IF Steel

by Estefania A. Sepulveda Hernández, Felipe M. Castro Cerda and Leo A. I. Kestens

Metals 2025, 15(9), 939; https://doi.org/10.3390/met15090939 - 24 Aug 2025

Cited by 2 | Viewed by 1096

Abstract

This study investigates the subsequent stages of recrystallisation in Interstitial-Free (IF) steel subjected to an unconventional continuous annealing process with a controlled thermal gradient. A cold-rolled steel strip was exposed to varying annealing temperatures along its length, enabling the analysis of microstructural evolution during the course of recrystallisation. The microstructure and stored energy were assessed at various positions along the strip using Electron Backscatter Diffraction (EBSD). The results underscore the significant influence of local misorientation and structural inhomogeneity on orientation selection during recrystallisation. The remaining non-recrystallised volume fraction (NRF) strongly correlates with the average misorientation gradient, obeying a phenomenological power-law correspondence with an exponent of ~3.7. This indicates that the recrystallisation process is highly sensitive to small changes in local orientation gradients. These findings highlight the crucial role of stored energy distribution for texture evolution, particularly during the early stages of recrystallisation in continuous annealing. It is observed that g-fiber grains, in comparison to a-fiber grains, are much more susceptible to grain fragmentation and therefore develop more robust intra-granular misorientation gradients, allowing for successful nucleation events to occur. In the present study, these phenomena are documented in a statistically representative manner. These insights are valuable for optimising thermal processing in interstitial-free (IF) steels. Full article

(This article belongs to the Special Issue Microstructure, Crystallography, and Mechanical Properties of Metallic Materials)

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17 pages, 2280 KB

Open AccessArticle

Effect of PBF-LB/M Processing on the Microstructural Evolution and Local Mechanical Properties of Novel Al-Fe-Si-Cr-Ni Alloy

by Alessandra Martucci, Paolo Fino and Mariangela Lombardi

Metals 2025, 15(6), 661; https://doi.org/10.3390/met15060661 - 13 Jun 2025

Cited by 1 | Viewed by 884

Abstract

The present study aims to investigate the microstructural evolution and local mechanical properties of an AlFe18Si8Cr5Ni2 alloy processed via Powder Bed Fusion–Laser-Based Manufacturing (PBF-LB/M). Designed with a focus on sustainability, this alloy was produced by deriving the necessary elements from AlSi10Mg and 304L steel, two of the most widely used alloys and, consequently, among the easiest materials to source from machining scrap. By leveraging iron, chromium, and nickel from these widespread standard compositions, the alloy mitigates the detrimental effects of Fe contamination in Al-based alloys while simultaneously enhancing mechanical performance. A comprehensive investigation of the impact of rapid solidification and thermal cycling offered novel insights into phase stability, elemental distribution, and local mechanical behavior. In particular, microstructural analyses using scanning electron microscopy (SEM), field emission SEM, energy-dispersive X-ray spectroscopy, X-ray diffraction, and differential scanning calorimetry revealed significant phase modifications post PBF-LB/M processing, including Fe-rich acicular phase segregation at melt pool boundaries and enhanced strengthening phase formation. In addition, nanoindentation mapping was used to demonstrate the correlation between microstructural heterogeneity and local mechanical properties. The findings contribute to a deeper understanding of Al-Fe-Si-Cr-Ni alloy changes after the interaction with the laser, supporting the development of high-performance, sustainable Al-based materials for PBF-LB/M applications. Full article

(This article belongs to the Special Issue Microstructure, Crystallography, and Mechanical Properties of Metallic Materials)

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18 pages, 25726 KB

Open AccessArticle

Effect of Grain Size on Mechanical Properties and Deformation Mechanism of Nano-Polycrystalline Pure Ti Simulated by Molecular Dynamics

by Xiao Zhang, Adam Ibrahem Abdalrsoul Alduma, Faqi Zhan, Wei Zhang, Junqiang Ren and Xuefeng Lu

Metals 2025, 15(3), 271; https://doi.org/10.3390/met15030271 - 1 Mar 2025

Cited by 8 | Viewed by 5185

Abstract

Nano- and microscale titanium and its alloys have potential applications in semiconductor-based micro-electromechanical systems due to their excellent mechanical properties. The uniaxial tensile mechanical properties and deformation mechanism of polycrystalline pure Ti with five different grain sizes measuring 6.74–19.69 nm were studied via molecular dynamics simulation using the embedded-atom potential function method. The Hall–Petch relationships and the critical grain size of the polycrystalline pure Ti are given. The dislocation migration of grain boundaries is the main deformation mechanism when the grain size exceeds 16.61 nm, which causes a direct Hall–Petch effect. When grain sizes are smaller than 16.61 nm, grain boundary sliding is the preferred deformation mechanism, which causes an inverse Hall–Petch effect. The polycrystalline pure Ti shows the highest tensile strength and average flow stress of 2.70 GPa and 2.15 GPa, respectively, at the 16.61 nm grain size, which is the critical grain size in the Hall–Petch relationships. The polycrystalline Ti is at its highest strength when its grain size ranges from 16 to 17 nm. The current research provides a theoretical basis for the use of pure titanium in emerging technologies at the nanoscale. Full article

(This article belongs to the Special Issue Microstructure, Crystallography, and Mechanical Properties of Metallic Materials)

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15 pages, 6647 KB

Open AccessArticle

Effects of Interstitial Oxygen Content on Microstructures and Mechanical Properties of TiZrNb Refractory Medium-Entropy Alloy

by Chen Zhang, Caiying Chen, Li Jiang, Yanhui Li, Zhibin Zhu, Fei Chen, Zhiqiang Cao and Wei Zhang

Metals 2025, 15(3), 250; https://doi.org/10.3390/met15030250 - 26 Feb 2025

Cited by 9 | Viewed by 2048

Abstract

Refractory high-entropy or medium-entropy alloys (RHEAs, RMEAs) exhibit outstanding strength and hold significant promise for high-temperature applications. However, their pronounced brittleness at room temperature restricts their industrial application. Recently, the introduction of interstitial oxygen has proven effective in refining the microstructure and improving the mechanical properties of RMEAs. In this study, we investigated the effect of interstitial oxygen content ranging from 0.5 to 6 at.% on the microstructures and mechanical properties of TiZrNb MEA. The alloys display a single BCC structure, showing a dendritic crystal morphology. At an oxygen content of 4 at.%, the alloy shows a room-temperature compressive yield strength of 1300 MPa and compressive strain of over 50%, achieving a balanced strength and ductility combination. Moreover, it shows excellent high-temperature mechanical properties, with yield strength exceeding 500 MPa at 800 °C. The Toda-Caraballo and Labusch theoretical models were used in the study to clarify the strengthening mechanism of the alloys, and the theoretical yield strengths obtained by calculation coincided with the experimental yield strengths. This validation not only confirms that the primary strengthening mechanism is solid solution strengthening, but also proves the reliability of the model in predicting the mechanical properties of MEAs and provides a theoretical basis for the use of interstitial atoms to strengthen MEAs. Full article

(This article belongs to the Special Issue Microstructure, Crystallography, and Mechanical Properties of Metallic Materials)

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20 pages, 6139 KB

Open AccessArticle

Effect of Al-5Ti-1B-xCe Refiner on Microstructure and Mechanical Properties of Cast Al-5Mg-3Zn-1Cu Alloys

by Shenshen Cui, Qiang Lu, Qudong Wang, Dezhi Li and Chuan Lei

Metals 2025, 15(2), 141; https://doi.org/10.3390/met15020141 - 29 Jan 2025

Cited by 1 | Viewed by 1363

Abstract

The effects of Ce content on the microstructure and phase composition of the Al-5Ti-1B refiner and the refining effect of the Al-5Ti-1B-xCe (x = 0, 1, 5, 10 wt.%) refiner on the grain size, microstructure, and mechanical properties of Al-5Mg-3Zn-1Cu alloys were studied. The results show that the addition of 1.0 wt.% Ce in the Al-5Ti-1B refiner changes the TiAl₃ phase from block to strip, and the massive Ti₂Al₂₀Ce phase is formed. When the Ce content of the Al-5Ti-1B refiner increases to 5.0 wt.%, the plate-like TiAl₃ phase is surrounded by the Ti₂Al₂₀Ce phase, and the reticulate Al₄Ce phase is formed. With the Ce content of the Al-5Ti-1B refiner further increasing to 10.0 wt.%, a lot of network distribution Al₄Ce phase is formed. The volume of the Mg₃₂(AlCuZn)₄₉ phase of the as-cast Al-5Mg-3Zn-1Cu alloys is reduced after refining with the Al-5Ti-1B-xCe refiner. The Al-5Ti-1B-1Ce refiner has the best refining effect on as-cast Al-5Mg-3Zn-1Cu alloys, and the grain size of as-cast Al-5Mg-3Zn-1Cu alloys refined by the Al-5Ti-1B-1Ce refiner is reduced by 43% compared with as-cast Al-5Mg-3Zn-1Cu alloys refined by the Al-5Ti-1B refiner. Compared to the aged Al-5Mg-3Zn-1Cu alloys refined by the Al-5Ti-1B refiner, the yield strength, ultimate tensile strength, and fracture elongation of aged Al-5Mg-3Zn-1Cu alloys refined by the Al-5Ti-1B-5Ce refiner are improved by 4.0%, 4.6%, and 25.6%, respectively. Therefore, it can be seen that Al-5Ti-1B-1Ce refiner and Al-5Ti-1B-5Ce refiner have broad application prospects. Full article

(This article belongs to the Special Issue Microstructure, Crystallography, and Mechanical Properties of Metallic Materials)

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