Synthesis and microstructural characterization of nanostructured Fe50Ni50 alloy prepared by mechanical alloying

Mohsen Abaei

doi:10.53063/synsint.2026.63344

Mohsen Abaei ¹

¹ Department of Materials Engineering, University of Kashan, Kashan, Iran

https://doi.org/10.53063/synsint.2026.63344

Abstract

In this comprehensive study, the synthesis, phase evolution, and microstructural characteristics of nanostructured Fe₅₀Ni₅₀ alloy powders produced via high-energy mechanical alloying (MA) were systematically investigated. Elemental iron and nickel powders were processed in a high-energy planetary ball mill under a controlled argon protective atmosphere to prevent oxidation, utilizing a constant ball-to-powder weight ratio (BPR) of 20:1 and a rotational speed of 350 rpm across cumulative milling durations of 0, 4, 8, 32, 48, and 96 hours. The structural transformations, crystallite size refinement, internal lattice strain accumulation, and lattice parameter expansion were evaluated using X-ray diffraction (XRD) data interpreted through Scherrer and Williamson–Hall analytical approaches. Furthermore, morphological alterations, particle size distributions, and microstructural transitions were examined using scanning electron microscopy (SEM) equipped with secondary electron detectors and Image Tool software. The XRD results indicate that continuous high-energy mechanical deformation up to 96 hours induces complete mechanical alloying, resulting in the formation of a random (Ni,Fe) solid solution with a face-centered cubic (fcc) crystal structure, as evidenced by the disappearance of the individual bcc iron diffraction peaks and significant broadening of the nickel-related peaks. The crystallite size exhibited a sharp initial decline followed by a relatively stable trend, decreasing from an initial value of 65 nm to a minimum of 9 nm after 96 hours. Simultaneously, the internal lattice strain increased progressively, reaching a maximum value of 0.58%. Morphological analyses revealed that initial microforging, cold welding, and particle flattening predominated during the early milling stages, whereas extended milling induced severe work hardening and fracture, ultimately achieving a dynamic steady-state balance at 96 hours, with refined, relatively uniform, and spherical particles possessing an average size of 10 μm.

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Keywords: Mechanical alloying, Fe-Ni alloy, Nanostructured materials, Phase evolution, Microstructural characterization, X-ray diffraction

References

[1] A.V. Rane, K. Kanny, V.K. Abitha, S. Thomas, Methods for Synthesis of Nanoparticles and Fabrication of Nanocomposites, Synthesis of Inorganic Nanomaterials, Woodhead Publishing. (2018) 121–139. https://doi.org/10.1016/B978-0-08-101975-7.00005-1.

[2] V. Harish, M.M. Ansari, D. Tewari, M. Gaur, A.B. Yadav, et al, Nanoparticle and nanostructure synthesis and controlled growth methods, Nanomaterials. 12 (2022) 3226. https://doi.org/10.3390/nano12183226.

[3] M. Aliofkhazraei, Handbook of Mechanical Nanostructuring, Wiley. (2015). https://doi.org/10.1002/9783527674947.

[4] C. Suryanarayana, A.A. Al-Joubori, Z. Wang, Nanostructured materials and nanocomposites by mechanical alloying: an overview, Met. Mater. Int. 28 (2022) 41–53. https://doi.org/10.1007/s12540-021-00998-5.

[5] M. Bassyouni, M.S. Zahid, F.A. Alabdullah, Sustainable approaches to nanomaterial synthesis using mechanical grinding methods, Int. J. Ind. Sustain. Dev. 7 (2026) 1–28. https://doi.org/10.21608/ijisd.2026.446142.1094.

[6] S. Saddique, I. Ullah, M. Irfan, W. Wang, S. Ali, et al., A Review of Synthesis Techniques for Thermoelectric Materials: From Bulk Processing and Nanostructuring to Thin‐Film Deposition, Chem. Rec. 26 (2026) e202500299. https://doi.org/10.1002/tcr.202500299.

[7] G. Gorrasi, A. Sorrentino, Mechanical milling as a technology to produce structural and functional bio-nanocomposites, Green Chem. 17 (2015) 2610–2625. https://doi.org/10.1039/C5GC00029G.

[8] D. Moskovskikh, Overview of Planetary Ball Milling Strategies for Tailoring Composite Powder Morphology and Reactivity, Int. J. Self-Propagating High-Temp. Synth. 34 (2025) 330–341. https://doi.org/10.3103/S1061386225700335.

[9] M. Toozandehjani, K. Matori, F. Ostovan, S. Abdul Aziz, M. Mamat, Effect of milling time on the microstructure, physical and mechanical properties of Al-Al2O3 nanocomposite synthesized by ball milling and powder metallurgy, Materials (Basel). 10 (2017) 1232. https://doi.org/10.3390/ma10111232.

[10] S.B. Gasha, M. Trautmann, G. Wagner, Effect of Milling Time and Reinforcement Volume Fraction on Microstructure and Mechanical Properties of SiCp-Reinforced AA2017 Composite Powder Produced by High-Energy Ball Milling, Materials (Basel). 17 (2024) 435. https://doi.org/10.3390/ma17020435.

[11] B. Tunç, İ. Somunkıran, S. Özkaya, M. Çelebi, A. Çanakçı, Powder evolution and microstructural development of rare-earth modified AlGdNiCoMn high-entropy alloy during mechanical milling, Adv. Powder Technol. 37 (2026) 105409. https://doi.org/10.1016/j.apt.2026.105409.

[12] M. Bouras, N. Loudjani, T. Gouasmia, R. Amraoui, A. Younes, N. Keghouche, Magnetic Properties of Multi-component Alloy Co30Fe30Ni30Cr10, J. Mater. Eng. Perform. 35 (2026) 32353–32371. https://doi.org/10.1007/s11665-026-14038-z.

[13] I. Moravcik, J. Cizek, J. Zapletal, Z. Kovacova, J. Vesely, et al., Microstructure and mechanical properties of Ni1,5Co1,5CrFeTi0,5 high entropy alloy fabricated by mechanical alloying and spark plasma sintering, Mater. Des. 119 (2017) 141–150. https://doi.org/10.1016/j.matdes.2017.01.036.

[14] C. Suryanarayana, Mechanical Alloying: A Novel Technique to Synthesize Advanced Materials, Research. 2019 (2019) 4219812. https://doi.org/10.34133/2019/4219812.

[15] C. Suryanarayana, Mechanical alloying: a critical review, Mater. Res. Lett. 10 (2022) 619–647. https://doi.org/10.1080/21663831.2022.2075243.

[16] S. Liu, C. Dun, J.J. Urban, M.T. Swihart, Non‐Equilibrium Synthesis methods to create metastable and high‐entropy nanomaterials, Adv. Sci. 13 (2026) e21953. https://doi.org/10.1002/advs.202521953.

[17] H. Ren, G. Li, M. Wang, X. Zuo, Effect of sintering temperature on the microstructure and integrated properties of MgAlTiVFeCo lightweight high-entropy alloy, Materials (Basel). 19 (2026) 770. https://doi.org/10.3390/ma19040770.

[18] A. Canakci, F. Erdemir, T. Varol, A. Patir, Determining the effect of process parameters on particle size in mechanical milling using the Taguchi method: measurement and analysis, Measurement. 46 (2013) 3532–3540. https://doi.org/10.1016/j.measurement.2013.06.035.

[19] M. Cabeza, I. Feijoo, P. Merino, G. Pena, M.C. Pérez, et al., Effect of high energy ball milling on the morphology, microstructure and properties of nano-sized TiC particle-reinforced 6005A aluminium alloy matrix composite, Powder Technol. 321 (2017) 31–43. https://doi.org/10.1016/j.powtec.2017.07.089.

[20] S. Kutuk, Influence of milling parameters on particle size of ulexite material, Powder Technol. 301 (2016) 421–428. https://doi.org/10.1016/j.powtec.2016.06.020.

[21] N.V. Mushnikov, A.G. Popov, V.S. Gaviko, A.V. Protasov, N.M. Kleinerman, et al., Peculiarities of phase diagram of Fe-Ni system at Ni concentrations 0 – 20 at.%., Acta Mater. 240 (2022) 118330. https://doi.org/10.1016/j.actamat.2022.118330.

[22] A. Sahoo, V.R.R. Medicherla, Fe-Ni Invar alloys: A review, Mater. Today Proc. 43 (2021) 2242–2244. https://doi.org/10.1016/j.matpr.2020.12.527.

[23] T. Gouasmia, N. Loudjani, M. Boulkra, M. Benchiheub, K. Belakroum, M. Bououdina, Morphology, structural and microstructural characterizations of mechanically alloyed Fe50Co40Ni10 powder mixture, Appl. Phys. A. 128 (2022) 935. https://doi.org/10.1007/s00339-022-06074-y.

[24] Y. Qiao, Y. Ni, K. Yang, P. Wang, X. Wang, et al., Iron-based high-temperature alloys: alloying strategies and new opportunities, Materials (Basel). 18 (2025) 2989. https://doi.org/10.3390/ma18132989.

[25] S. Ni, Y.B. Wang, X.Z. Liao, S.N. Alhajeri, H.Q. Li, et al., Strain hardening and softening in a nanocrystalline Ni–Fe alloy induced by severe plastic deformation, Mater. Sci. Eng. A. 528 (2011) 3398–3403. https://doi.org/10.1016/j.msea.2011.01.017.

[26] S. Kuramoto, T. Furuta, Severe Plastic Deformation to Achieve High Strength and High Ductility in Fe–Ni Based Alloys with Lattice Softening, Mater. Trans. 60 (2019) 1116–1122. https://doi.org/10.2320/matertrans.MF201920.

[27] M.D.A. Valentine, V. Dhokia, J. Flynn, S.A.M. McNair, A.J.G. Lunt, Characterisation of residual stresses and oxides in titanium, nickel, and aluminium alloy additive manufacturing powders via synchrotron X-ray diffraction, Mater. Today Commun. 35 (2023) 105900. https://doi.org/10.1016/j.mtcomm.2023.105900.

[28] T. Gouasmia, N. Loudjani, M. Bououdina, Structural Evolution, Magnetic Behavior and Thermal Stability of Mechanically Alloyed Fe50Co40Ni10 Nanocrystalline Powders, J. Mater. Eng. Perform. 35 (2026) 2120–2134. https://doi.org/10.1007/s11665-025-11758-6.

[29] M.W.R. Volk, M.R. Wack, B.J. Maier, Monitoring the alloying process of mechanically synthesized Fe80Ni20 through changes in magnetic properties, J. Alloys Compd. 732 (2018) 336–342. https://doi.org/10.1016/j.jallcom.2017.10.090.

[30] H. Wang, Q. He, X. Gao, Y. Shang, W. Zhu, et al., Multifunctional High Entropy Alloys Enabled by Severe Lattice Distortion, Adv. Mater. 36 (2024) 2305453. https://doi.org/10.1002/adma.202305453.

[31] A. Ali, Y.W. Chiang, R.M. Santos, X-ray Diffraction Techniques for Mineral Characterization: A Review for Engineers of the Fundamentals, Applications, and Research Directions, Minerals. 12 (2022) 205. https://doi.org/10.3390/min12020205.

[32] J. Epp, X-ray diffraction (XRD) techniques for materials characterization, Materials Characterization Using Nondestructive Evaluation (NDE) Methods, Woodhead Publishing. (2016) 81–124. https://doi.org/10.1016/B978-0-08-100040-3.00004-3.

[33] B. Himabindu, N.S.M.P. Latha Devi, B. Rajini Kanth, Microstructural parameters from X-ray peak profile analysis by Williamson-Hall models; A review, Mater. Today Proc. 47 (2021) 4891–4896. https://doi.org/10.1016/j.matpr.2021.06.256.

[34] A. Pal, A dimensionally consistent size–strain plot method for crystallite size and microstrain estimation, J. Alloys Compd. 1048 (2025) 185324. https://doi.org/10.1016/j.jallcom.2025.185324.

[35] S.A. Disha, M. Sahadat Hossain, M.L. Habib, S. Ahmed, Calculation of crystallite sizes of pure and metals doped hydroxyapatite engaging Scherrer method, Halder-Wagner method, Williamson-Hall model, and size-strain plot, Results Mater. 21 (2024) 100496. https://doi.org/10.1016/j.rinma.2023.100496.

[36] M.H. Enayati, F.A. Mohamed, Application of mechanical alloying/milling for synthesis of nanocrystalline and amorphous materials, Int. Mater. Rev. 59 (2014) 394–416. https://doi.org/10.1179/1743280414Y.0000000036.

[37] A.O. Adeoye, A.R. Damanpack, C. Spitas, R. Shoja Razavi, Y. Ren, Y. Nie, Optimizing ball milling duration for microstructural homogeneity and interfacial bonding in Mg-HA-graphene nanocomposites for biomedical implants, Ceram. Int. 52 (2026) 17957–17973. https://doi.org/10.1016/j.ceramint.2026.02.373.

[38] N. Loudjani, T. Gouasmia, M. Bououdina, J.L. Bobet, Phase formation and magnetic properties of nanocrytalline Ni70Co30 alloy prepared by mechanical alloying, J. Alloys Compd. 846 (2020) 156392. https://doi.org/10.1016/j.jallcom.2020.156392.

[39] T.P. Yadav, R.M. Yadav, D.P. Singh, Mechanical milling: a top down approach for the synthesis of nanomaterials and nanocomposites, Nanosci. Nanotechnol. 2 (2012) 22–48. https://doi.org/10.5923/j.nn.20120203.01.

[40] R. Mitra, A. Bajpai, K. Biswas, A Critical Review on Mechanical Alloying of High-Entropy Materials, High Entropy Alloy. Mater. 3 (2025) 1–40. https://doi.org/10.1007/s44210-025-00056-4.

[41] P. Moazzen, M. Toroghinejad, Y. Aghayar, T. Zargar, F. Davoodi, M. Mohammadi, Exploring Nanocrystalline High Entropy Alloys Fabricated via Mechanical Alloying (MA) and Spark Plasma Sintering (SPS): A Review, High Entropy Alloy. Mater. 2 (2024) 175–218. https://doi.org/10.1007/s44210-024-00038-y.

[42] M. Azabou, W. Ben Mbarek, A. Wederni, S. Almenia, M. Khitouni, J.-J. Suñol, Mechanosynthesis of Nanocrystalline Biphasic Ni-Fe Alloy Powders by Mechanical Alloying and Their Structural and Thermal Characterization, Metals (Basel). 15 (2025) 270. https://doi.org/10.3390/met15030270.

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