Microstructure-Mechanical Properties of Mg-xCa Alloys Produced by Mechanical Alloying-Hot Pressing Process and Their Optimization Using Central Composite Design Method

Year 2025, Volume: 12 Issue: 2, 141 - 154, 31.05.2025

Lütfiye Feray Güleryüz , Rasim İpek

https://doi.org/10.18596/jotcsa.1630114

Abstract

In the study, Mg-xCa alloys with high mechanical performance were developed using a statistical model central composite design (CCD) method to predict the mechanical properties of Mg and Ca powders produced by powder metallurgy. Powder metallurgy (TM) is a production method that offers great advantages over other production methods. However, there are limited studies in the literature on the production of alloying Ca to eliminate the high degradation rate of pure Mg loss. Mg and Ca powders were subjected to the alloying process for different times as 11.99-14.43-18-21.5-24 h, and after mechanical alloying (MA), grain size measurements of the powders and XRD and SEM-EDS analyses were performed. After MA, the powders were sintered at different temperatures, such as 325-370-437-504-549°C in an argon gas environment under 46 MPa pressure, and samples were obtained. The microstructures, mechanical properties, compressive strength, density values, and XRD-SEM results showed that the secondary phase Mg2Ca increased with increasing Ca content, which indicates the increasing hardness of Mg-xCa alloy. Using the CCD method, the sample's compressive strength, hardness, and density results with optimal values produced from Mg-xCa alloys were determined as 251 MPa, 146 Brinell, and 1.7 g/cm3, respectively. The compatibility of the experimental results with the Regression formula confirms the reliability of the equation.

Keywords

powder metallurgy, CCD method, XRD, SEM-EDS, Mg-xCa alloys

References

• 1. Box GEP, Wilson KB. On the experimental attainment of optimum conditions. In: Kotz S, Johnson NL, editors. Breakthroughs in Statistics [Internet]. Springer, New York, NY; 1992. p. 270–310. Available from: <URL>.
• 2. Kuehl RO. Design of experiments: statistical principles of research design and analysis. Duxbury Press; 2000.
• 3. Wang J, Wan W. Experimental design methods for fermentative hydrogen production: A review. Int J Hydrogen Energy [Internet]. 2009 Jan;34(1):235–44. Available from: <URL>.
• 4. Li Z, Lu D, Gao X. Optimization of mixture proportions by statistical experimental design using response surface method - A review. J Build Eng [Internet]. 2021 Apr;36:102101. Available from: <URL>.
• 5. O-Thong S, Prasertsan P, Intrasungkha N, Dhamwichukorn S, Birkeland NKå. Optimization of simultaneous thermophilic fermentative hydrogen production and COD reduction from palm oil mill effluent by Thermoanaerobacterium-rich sludge. Int J Hydrogen Energy [Internet]. 2008 Feb;33(4):1221–31. Available from: <URL>.
• 6. Mohapatra S, Pradhan N, Mohanty S, Sukla LB. Recovery of nickel from lateritic nickel ore using Aspergillus niger and optimization of parameters. Miner Eng [Internet]. 2009 Feb;22(3):311–3. Available from: <URL>.
• 7. Solanki N, Saini S, Singh SK, Paudel KR, Goh BH, Dua K, et al. Central composite designed boswellic acids loaded nanoparticles for enhanced cellular uptake in human lung cancer cell line A549. J Drug Deliv Sci Technol [Internet]. 2025 Mar;105:106591. Available from: <URL>.
• 8. Ndlovu A, Cornish LA, Sithebe HSL. Relationship between sintering pressure and leach rate of polycrystalline diamond compacts (PDCs) using central composite design (CCD) modelling. Int J Refract Met Hard Mater [Internet]. 2024 Nov;124:106854. Available from: <URL>.
• 9. Verma S, Verma B. Optimizing carbon nanotube-doped ternary composite for high-energy-density hybrid supercapacitors: A comprehensive electrochemical assessment through central composite design. J Ind Eng Chem [Internet]. 2024 Dec;140:354–63. Available from: <URL>.
• 10. Zhao H, Wang W, Fu Z, Wang H. Thermal conductivity and dielectric property of hot-pressing sintered AlN–BN ceramic composites. Ceram Int [Internet]. 2009 Jan;35(1):105–9. Available from: <URL>.
• 11. İlhan M, Mergen A, Yaman C. Removal of iron from BaTa2O6 ceramic powder produced by high energy milling. Ceram Int [Internet]. 2013 Jul;39(5):5741–50. Available from: <URL>.
• 12. İlhan M, Mergen A, Yaman C. Mechanochemical synthesis and characterisation of BaTa2O6 ceramic powders. Ceram Int [Internet]. 2011 Jul;37(5):1507–14. Available from: <URL>.
• 13. Suryanarayana C, Ivanov E, Boldyrev V. The science and technology of mechanical alloying. Mater Sci Eng A [Internet]. 2001 May;304–306:151–8. Available from: <URL>.
• 14. Song SG, Shi N, Gray GT, Roberts JA. Reinforcement shape effects on the fracture behavior and ductility of particulate-reinforced 6061-Al matrix composites. Metall Mater Trans A [Internet]. 1996 Nov;27(11):3739–46. Available from: <URL>.
• 15. Bamberger M, Dehm G. Trends in the development of new Mg alloys. Annu Rev Mater Res [Internet]. 2008 Aug 1;38(1):505–33. Available from: <URL>.
• 16. Li Z, Gu X, Lou S, Zheng Y. The development of binary Mg–Ca alloys for use as biodegradable materials within bone. Biomaterials [Internet]. 2008 Apr;29(10):1329–44. Available from: <URL>.
• 17. Bronzino JD. Medical devices and systems, the biomedical engineering handbook [Internet]. Bronzino JD, editor. CRC Press; 2006. Available from: <URL>.
• 18. Park JB, Lakes RS. Biomaterials [Internet]. New York, NY: Springer New York; 2007. Available from: <URL>.
• 19. Chen Y, Xu Z, Smith C, Sankar J. Recent advances on the development of magnesium alloys for biodegradable implants. Acta Biomater [Internet]. 2014 Nov;10(11):4561–73. Available from: <URL>.
• 20. Zberg B, Uggowitzer PJ, Löffler JF. MgZnCa glasses without clinically observable hydrogen evolution for biodegradable implants. Nat Mater [Internet]. 2009 Nov 27;8(11):887–91. Available from: <URL>.
• 21. Carney CM, Mah T. Current isolation in spark plasma sintering of conductive and nonconductive ceramics. J Am Ceram Soc [Internet]. 2008 Oct;91(10):3448–50. Available from: <URL>.
• 22. Song X, Liu X, Zhang J. Neck formation and self‐adjusting mechanism of neck growth of conducting powders in spark plasma sintering. J Am Ceram Soc [Internet]. 2006 Feb 14;89(2):494–500. Available from: <URL>.
• 23. Jha SK, Raj R. The effect of electric field on sintering and electrical conductivity of titania. Chen I ‐W., editor. J Am Ceram Soc [Internet]. 2014 Feb 13;97(2):527–34. Available from: <URL>.
• 24. İlhan M, Ekmekçi MK, Güleryüz LF. Effect of boron incorporation on the structural, morphological, and spectral properties of CdNb2O6:Dy3+ phosphor synthesized by molten salt process. Mater Sci Eng B [Internet]. 2023 Dec;298:116858. Available from: <URL>.
• 25. İlhan M, Güleryüz LF, Ekmekci MK. Structural properties, photoluminescence, and judd-ofelt parameters of Eu3+-doped CoNb2O6 phosphor. J Turkish Chem Soc Sect A Chem [Internet]. 2023 Aug 30;10(3):745–56. Available from: <URL>.
• 26. Yoon KH, Park HS, Cho JY, Kim ES. Microwave dielectric properties of (Pb0.4Ca0.6)(Fe0.5Ta0.5)O3 ceramics prepared by mechanochemical processing. J Eur Ceram Soc [Internet]. 2003 Jan;23(14):2579–82. Available from: <URL>.
• 27. Mergen A. Mechanochemical synthesis of MgTa2O6 ceramic. Ceram Int [Internet]. 2009 Apr;35(3):1151–7. Available from: <URL>.
• 28. Moure A, Castro A, Tartaj J, Moure C. Mechanosynthesis of perovskite LaGaO3 and its effect on the sintering of ceramics. Ceram Int [Internet]. 2009 Sep;35(7):2659–65. Available from: <URL>.
• 29. Yahşi Y, İpek R. Effect of ball milling time on microstructural properties of Mg/MgO. Hacettepe J Biol Chem [Internet]. 2022 Aug 1;50(3):269–74. Available from: <URL>.
• 30. Hirata Y, Fujita H, Shimonosono T. Compressive mechanical properties of partially sintered porous alumina of bimodal particle size system. Ceram Int [Internet]. 2017 Feb;43(2):1895–903. Available from: <URL>.
• 31. Yahsi Y, Yusan S, Akgol S, Ipek R. Experimental investigation of sinterability of PVA-coated Magnesium powders via mechanical milling using electric field-assisted sintering technique. Kov Mater Mater [Internet]. 2024 Nov 6;62(4):211–22. Available from: <URL>.
• 32. Myers RH, Montgomery DC. Response surface methodology: Process and product optimization using designed experiment [Internet]. John Wiley & Sons. Inc.; 1995. Available from: <URL>.