Evaluation of mechanical properties of ultrafine-grained pure titanium produced via warm ECAP process by concurrently utilizing casing and back pressure

Document Type : Original Article

Author
1.Assistant Professor, Department of Mechanical Engineering, Technical and Vocational University (TVU), Tehran, Iran
Abstract
The application of the Equal Channel Angular Pressing (ECAP) process imposes severe plastic strains on the metallic billet. As a result of these imposed strains, the initially coarse grains are transformed into ultra-fined or nanostructured grains, and beneficial microstructural evolutions occur in the texture of the material, which lead to improvements in mechanical properties. In this study, commercially pure titanium (CP-Ti) BT1-0, as a hard-to-deform material, was placed inside a casing made of pure copper and subjected to four passes of warm ECAP at a temperature of 250°C in a 135° channel using route Bc, accompanied by the application of back pressure through extrusion in the end of die. The simultaneous effect of back pressure and the casing on the grain structure and mechanical properties of the target material, i.e., CP-Ti, was evaluated. Experimental results showed that the grain size was refined from 49 µm in the initial annealed state to 710 nm after four ECAP passes. The compressive yield and ultimate strength, and also compressive elongation changed from 267 MPa, 899 MPa, and 51.8 mm/mm in the non-ECAPed condition to 958 MPa, 1375 MPa, and 30.7 mm/mm after ECAP processes, corresponding to increases of 359% and 153%, and a decrease of 59%, respectively. The average Vickers hardness also increased from 163 Hv in the initial annealed state to 289 Hv after four ECAP passes, representing a 77% enhancement.
Keywords
Subjects

اصل مقاله

[1] M. Geetha, A. K. Singh, R. Asokamani, and A. K. Gogia, "Ti based biomaterials, the ultimate choice for orthopaedic implants–a review," Prog. Mater. Sci., Vol. 54, No. 3, pp. 397–425, May 2009. [Online]. Available: doi: 10.1016/j.pmatsci.2008.06.004.
[2] H. J. Rack and J. I. Qazi, "Titanium alloys for biomedical applications," Mater. Sci. Eng. C, Vol. 26, No. 8, pp. 1269–1277, Sep. 2006. [Online]. Available: doi: 10.1016/j.msec.2005.08.032.
[3] P. S. Roodposhti, N. Farahbakhsh, A. Sarkar, and K. L. Murty, "Microstructural approach to equal channel angular processing of commercially pure titanium—A review," Trans. Nonferrous Met. Soc. China, Vol. 25, No. 5, pp. 1353–1366, May 2015. [Online]. Available: doi: 10.1016/S1003-6326(15)63734-7.
[4] S. Nag, R. Banerjee, and H. L. Fraser, "Microstructural evolution and strengthening mechanisms in Ti–Nb–Zr–Ta, Ti–Mo–Zr–Fe and Ti–15Mo biocompatible alloys," Mater. Sci. Eng. C, Vol. 25, No. 3, pp. 357–362, May 2005. [Online]. Available: doi: 10.1016/j.msec.2004.12.013.
[5] Y. J. Chen, Y. J. Li, J. C. Walmsley, S. Dumoulin, P. C. Skaret, and H. J. Roven, "Microstructure evolution of commercial pure titanium during equal channel angular pressing," Mater. Sci. Eng. A, Vol. 527, No. 3, pp. 789–796, Jan. 2010. [Online]. Available: doi: 10.1016/j.msea.2009.09.005.
[6] R. Z. Valiev and T. G. Langdon, "Principles of equal-channel angular pressing as a processing tool for grain refinement," Prog. Mater. Sci., Vol. 51, No. 7, pp. 881–981, Sep. 2006. [Online]. Available:  doi: 10.1016/j.pmatsci.2006.02.003.
[7] R. Naseri, M. Kadkhodayan, and M. Shariati, "Static mechanical properties and ductility of biomedical ultrafine-grained commercially pure titanium produced by ECAP process," Trans. Nonferrous Met. Soc. China, Vol. 27, No. 9, pp. 1964–1975, Sep. 2017. [Online]. Available:  doi: 10.1016/S1003-6326(17)60221-8.
[8] V. M. Segal, "Equal channel angular extrusion: from macromechanics to structure formation," Mater. Sci. Eng. A, Vol. 271, No. 1, pp. 322–333, 1999. [Online]. Available:  doi: 10.1016/S0921-5093(99)00248-8.
[9] V. M. Segal, "Materials processing by simple shear," Mater. Sci. Eng. A, Vol. 197, No. 2, pp. 157–164, Jul. 1995. [Online]. Available: doi: 10.1016/0921-5093(95)09705-8.
[10] R. Z. Valiev, R. K. Islamgaliev, and I. V. Alexandrov, "Bulk nanostructured materials from severe plastic deformation," Prog. Mater. Sci., Vol. 45, No. 2, pp. 103–189, Jan. 2000. [Online]. Available: doi: 10.1016/S0079-6425(99)00007-9.
[11] M. R. Roshan, S. A. J. Jahromi, and R. Ebrahimi, "Predicting the critical pre-aging time in ECAP processing of age-hardenable aluminum alloys," J. Alloys Compd., Vol. 509, No. 30, pp. 7833–7839, Aug. 2011. [Online]. Available: doi: 10.1016/j.jallcom.2011.05.065
[12] M. H. Shaeri, F. Djavanroodi, M. Sedighi, S. Ahmadi, M. T. Salehi, and S. H. Seyyedein, "Effect of copper tube casing on strain distribution and mechanical properties of Al-7075 alloy processed by equal channel angular pressing," J. Strain Anal. Eng. Des. Vol. 48, No. 8, pp. 512–521, Dec. 2013. [Online]. Available: doi: 10.1177/0309324713495251
[13] R. B. Figueiredo, P. R. Cetlin, and T. G. Langdon, "The processing of difficult-to-work alloys by ECAP with an emphasis on magnesium alloys," Acta Mater. Vol. 55, No. 14, pp. 4769–4779, Sep. 2007. [Online]. Available: doi: 10.1016/j.actamat.2007.04.019
[14] S. L. Semiatin, D. P. DeLo, V. M. Segal, R. E. Goforth, and N. D. Frey, "Workability of commercial-purity titanium and 4340 steel during equal channel angular extrusion at cold-working temperatures," Metall. Mater. Trans. A, Vol. 30, No. 5, pp. 1425–1435, May 1999. [Online]. Available: doi: 10.1007/s11661-999-0155-7
[15] P. R. Cetlin, M. T. P. Aguilar, R. B. Figueiredo, and T. G. Langdon, "Avoiding cracks and inhomogeneities in billets processed by ECAP," J. Mater. Sci., Vol. 45, No. 17, pp. 4561–4570, Sep. 2010. [Online]. Available: doi:10.1007/s10853-010-4595-x
[16] R. Naseri, M. Kadkhodayan, and M. Shariati, "An experimental investigation of casing effect on mechanical properties of billet in ECAP process," Int. J. Adv. Manuf. Technol., pp. 1–14, 2016. [Online]. Available: doi:10.1007/s00170-016-8701-5
[17] R. Naseri, H. Hiradfar, M. Shariati, and M. Kadkhodayan, "A comparison of axial fatigue strength of coarse and ultrafine grain commercially pure titanium produced by ECAP," Arch. Civ. Mech. Eng., Vol. 18, No. 3, pp. 755–767, Sep. 2018. [Online]. Available: doi:10.1016/j.acme.2017.11.007
[18] R. Naseri, H. Hiradfar, M. Shariati, and M. Kadkhodayan, "Corrosion-fatigue resistance of ultrafine grain commercially pure titanium in simulated body fluid," Proc. Inst. Mech. Eng. Part E: J. Process Mech. Eng., Vol. 237, No. 6, pp. 2181–2191, Jul. 2022. [Online]. Available: doi: 10.1177/09544089211045285
[19] R. Naseri, "Experimental evaluation of back-pressure effect on workability and mechanical properties of commercially pure titanium in cold-ECAP process," J. Solid Fluid Mech., Vol. 12, No. 6, pp. 67–81, 2023. (in Persian)
[20] N. Krasil Nikov, "Strength and ductility of copper subjected to equal-channel angular pressing with backpressure," Russ. Metall., Vol. 3, p. 220, 2005. [Online]. Available: doi: 10.1007/s11182-005-0127-3
[21] W. J. Kim and J. Y. Wang, "Microstructure of the post-ECAP aging processed 6061 Al alloys," Mater. Sci. Eng. A, Vol. 464, No. 1, pp. 23–27, Mar. 2007. [Online]. Available: doi: 10.1016/j.msea.2007.02.027
[22] R. Naseri, M. Kadkhodayan, and M. Shariati, "Theoretical analysis of equal channel angular pressing process by upper bound method and its experimental investigation in condition of circular cross-section channel," Amirkabir J. Mech. Eng., Vol. 53, No. 8, pp. 4729–4744, 2021.  doi: 10.22060/mej.2021.18754.6883. (in Persian)
[23] R. Y. Lapovok, "The role of back-pressure in equal channel angular extrusion," J. Mater. Sci., Vol. 40, pp. 341–346, 2005. [Online]. Available: doi:10.1007/s10853-005-3372-8
[24] T. G. Langdon, "Processing of ultrafine-grained materials using severe plastic deformation: Potential for achieving exceptional properties," Rev. Metal., Vol. 44, No. 6, pp. 556–564, 2008. [Online]. Available: doi:10.3989/revmetalm.08.065
[25] R. Naseri, M. Kadkhodayan, and M. Shariati, "The investigation of springback of UFG commercially pure titanium in three-point bending test," Modares Mech. Eng., Vol. 16, No. 11, pp. 266–276, 2017. (in Persian)
[26] A. R. Eivani and A. K. Taheri, "A new method for producing bimetallic rods," Mater. Lett., Vol. 61, No. 19, pp. 4110–4113, 2007. [Online]. Available: doi:10.1016/j.matlet.2007.02.057
[27] M. Zebardast and A. K. Taheri, "The cold welding of copper to aluminum using equal channel angular extrusion (ECAE) process," J. Mater. Process. Technol., Vol. 211, No. 6, pp. 1034–1043, Mar. 2011. [Online]. Available: doi:10.1016/j.jmatprotec.2011.01.015
[28] F. Djavanroodi, M. Daneshtalab, and M. Ebrahimi, "A novel technique to increase strain distribution homogeneity for ECAPed materials," Mater. Sci. Eng. A, Vol. 535, pp. 115–121, 2012. [Online]. Available: doi:10.1016/j.msea.2012.01.037
[29] P. W. J. Mckenzie and R. Lapovok, "ECAP with back pressure for optimum strength and ductility in aluminium alloy 6016. Part 1: Microstructure," Acta Mater., Vol. 58, No. 9, pp. 3198–3211, May 2010. [Online]. Available: doi:10.1016/j.actamat.2010.02.028
[30] P. W. J. Mckenzie and R. Lapovok, "ECAP with back pressure for optimum strength and ductility in aluminium alloy 6016. Part 2: Mechanical properties and texture," Acta Mater., Vol. 58, No. 9, pp. 3212–3222, May 2010. [Online]. Available: doi:10.1016/j.actamat.2010.02.029
[31] A. Panigrahi et al., "Effect of back pressure on material flow and texture in ECAP of aluminum," in IOP Conf. Ser.: Mater. Sci. Eng., Vol. 63, No. 1, p. 012153, 2014. [Online]. Available: doi:10.1088/1757-899X/63/1/012153
[32] B. Raddad, A. Frefer, M. Abdel‐Rahman, and A. Tajouri, "Some aspects of workability of engineering materials," TMS2013 Supplemental Proceedings, pp. 593–600, 2013. [Online]. Available: doi:10.7449/2013SP_593
[33] K. Xia, J. T. Wang, X. Wu, G. Chen, and M. Gurvan, "Equal channel angular pressing of magnesium alloy AZ31," Mater. Sci. Eng. A, Vol. 410, pp. 324–327, 2005. [Online]. Available:  doi:10.1016/j.msea.2005.08.001
[34] V. V. Stolyarov, R. Lapovok, I. G. Brodova, and P. F. Thomson, "Ultrafine-grained Al–5 wt.% Fe alloy processed by ECAP with backpressure," Mater. Sci. Eng. A, Vol. 357, No. 1, pp. 159–167, 2003. [Online]. Available:  doi:10.1016/S0921-5093(03)00451-0
[35] G. I. Raab, E. P. Soshnikova, and R. Z. Valiev, "Influence of temperature and hydrostatic pressure during equal-channel angular pressing on the microstructure of commercial-purity Ti," Mater. Sci. Eng. A, Vol. 387, pp. 674–677, 2004. [Online]. Available: doi:10.1016/j.msea.2004.08.042
[36] A. Czerwinski, R. Lapovok, D. Tomus, Y. Estrin, and A. Vinogradov, "The influence of temporary hydrogenation on ECAP formability and low cycle fatigue life of CP titanium," J. Alloys Compd., Vol. 509, No. 6, pp. 2709–2715, Mar. 2011. [Online]. Available: doi:10.1016/j.jallcom.2010.11.125
[37] Y. Estrin, H. E. Kim, R. Lapovok, H. P. Ng, and J. H. Jo, "Mechanical strength and biocompatibility of ultrafine-grained commercial purity titanium," BioMed Res. Int., Vol. 2013, pp. 1–6, 2013. [Online]. Available: doi:10.1155/2013/980572
[38] A. Jäger, V. Gärtnerova, and K. Tesař, "Microstructure and anisotropy of the mechanical properties in commercially pure titanium after equal channel angular pressing with back pressure at room temperature," Mater. Sci. Eng. A, Vol. 644, pp. 114–120, 2015. [Online]. Available:  doi:10.1016/j.msea.2015.06.009
[39] R. Naseri, H. Heirani, M. H. Mozaffari, and R. Babaei Spouei, "A comparison of corrosion behavior of coarse and ultrafine grain commercially pure titanium in simulated body fluid," Iran. J. Mech. Eng. Trans. ISME, Vol. 26, No. 1, 2025. (in Persian)
[40] X. Zhao, X. Yang, X. Liu, C. T. Wang, Y. Huang, and T. G. Langdon, "Processing of commercial purity titanium by ECAP using a 90 degrees die at room temperature," Mater. Sci. Eng. A, Vol. 607, pp. 482–489, 2014. [Online]. Available:  doi:10.1016/j.msea.2014.03.030
[41] A. Medvedev, H. P. Ng, R. Lapovok, Y. Estrin, T. C. Lowe, and V. N. Anumalasetty, "Comparison of laboratory-scale and industrial-scale equal channel angular pressing of commercial purity titanium," Mater. Lett., Vol. 145, pp. 308–311, 2015. [Online]. Available:  doi:10.1016/j.matlet.2015.01.007
[42] S. Zhang et al., "Effect of temperature on microstructural stabilization and mechanical properties in the dynamic testing of nanocrystalline pure Ti," Mater. Sci. Eng. A, Vol. 634, pp. 64–70, 2015. [Online]. Available:  doi:10.1016/j.msea.2015.02.023
[43] P. Rodriguez Calvillo and J. M. Cabrera, "Microstructure and mechanical properties of a commercially pure Ti processed by warm equal channel angular pressing," Mater. Sci. Eng. A, Vol. 625, pp. 311–320, 2015. [Online]. Available: doi:10.1016/j.msea.2014.12.079
[44] C. S. Meredith and A. S. Khan, "The microstructural evolution and thermo-mechanical behavior of UFG Ti processed via equal channel angular pressing," J. Mater. Process. Technol., Vol. 219, pp. 257–270, 2015. [Online]. Available:  doi:10.1016/j.jmatprotec.2014.11.015
[45] X. R. Yang et al., "Evolution of microstructure, macrotexture and mechanical properties of high strength biomedical TA4 pure titanium during multi-pass ECAP," J. Mater. Res. Technol., Vol. 28, pp. 3976–3987, 2024. [Online]. Available: https://doi.org/10.1016/j.jmrt.2024.01.062
[46] W. J. Kim, C. Y. Hyun, and H. K. Kim, "Fatigue strength of ultrafine-grained pure Ti after severe plastic deformation," Scr. Mater., Vol. 54, No. 10, pp. 1745–1750, 2006. [Online]. Available:  doi:10.1016/j.scriptamat.2006.02.005
[47] M. Ebrahimi, K. H. Tabei, R. Naseri, and F. Djavanroodi, "Effect of flow-forming parameters on surface quality, geometrical precision and mechanical properties of titanium tube," Proc. Inst. Mech. Eng. Part E, Vol. 232, No. 6, pp. 702–708, 2018. [Online]. Available:  doi:10.1177/0954408917702227
[48] R. Naseri, M. Shariati, and M. Kadkhodayan, "Effect of work-piece cross section on the mechanical properties of commercially pure titanium produced by Equal Channel Angular Pressing," Modares Mech. Eng., Vol. 15, No. 6, pp. 157–166, 2015. (in Persian)
[49] K. Hajizadeh, B. Eghbali, K. Topolski, and K. J. Kurzydlowski, "Ultra-fine grained bulk CP-Ti processed by multi-pass ECAP at warm deformation region," Mater. Chem. Phys., Vol. 143, No. 3, pp. 1032–1038, 2014. [Online]. Available:  doi:10.1016/j.matchemphys.2013.12.047
[50] C. T. Wang, A. G. Fox, and T. G. Langdon, "Microstructural evolution in ultrafine-grained titanium processed by high-pressure torsion under different pressures," J. Mater. Sci., Vol. 49, No. 19, pp. 6558–6564, 2014. [Online]. Available:  doi:10.1007/s10853-014-8412-0
[51] S. N. Alhajeri, N. Gao, and T. G. Langdon, "Hardness homogeneity on longitudinal and transverse sections of an aluminum alloy processed by ECAP," Mater. Sci. Eng. A, Vol. 528, No. 10, pp. 3833–3840, 2011. [Online]. Available: doi:10.1016/j.msea.2010.11.056
[52] A. V. Polyakov, L. Dluhoš, G. S. Dyakonov, G. I. Raab, and R. Z. Valiev, "Recent advances in processing and application of nanostructured titanium for dental implants," Adv. Eng. Mater., Vol. 17, No. 12, pp. 1869–1875, 2015. [Online]. Available: doi:10.1002/adem.201500139
[53] C. N. Elias, D. J. Fernandes, C. R. S. Resende, and J. Roestel, "Mechanical properties, surface morphology and stability of a modified commercially pure high strength titanium alloy for dental implants," Dent. Mater., Vol. 31, No. 2, pp. e1–e13, 2015. [Online]. Available:  doi:10.1016/j.dental.2014.11.001
[54] R. B. Figueiredo et al., "Improving the fatigue behavior of dental implants through processing commercial purity titanium by equal-channel angular pressing," Mater. Sci. Eng. A, Vol. 619, pp. 312–318, 2014. [Online]. Available:  doi:10.1016/j.msea.2014.07.084
[55] L. Wang et al., "Microstructure and texture evolution in ultrafine-grained pure Ti processed by equal-channel angular pressing with subsequent dynamic compression," Scr. Mater., Vol. 77, pp. 33–36, 2014. [Online]. Available:  doi:10.1016/j.scriptamat.2014.02.012
[56] X. Zhao, X. Yang, X. Liu, X. Wang, and T. G. Langdon, "The processing of pure titanium through multiple passes of ECAP at room temperature," Mater. Sci. Eng. A, Vol. 527, No. 23, pp. 6335–6339, 2010. [Online]. Available:  doi:10.1016/j.msea.2010.07.011
[57] M. Ebrahimi, M. H. Shaeri, R. Naseri, and C. Gode, "Equal channel angular extrusion for tube configuration of Al-Zn-Mg-Cu alloy," Mater. Sci. Eng. A, Vol. 731, pp. 569–576, 2018. [Online]. Available: doi:10.1016/j.msea.2018.07.025
[58] X. Y. Liu, X. C. Zhao, X. R. Yang, C. Xie, and G. J. Wang, "Compression deformation behaviours of ultrafine and coarse grained commercially pure titanium," Mater. Sci. Technol., Vol. 29, No. 4, pp. 474–479, 2013. [Online]. Available: doi:10.1179/1743284712Y.0000000272
[59] F. Fakheri, S. Pour-Ali, R. Tavangar, and R. Naseri, "Effect of ultrasonic assisted-ECAP processing on the microstructure, mechanical properties, and fluoride-induced corrosion performance of pure titanium," Mater. Today Commun., Vol. 40, p. 109863, 2024. [Online]. Available: doi:10.1016/j.mtcomm.2023.109863
[60] K. R. Gopi, H. Shivananda Nayaka, and S. Sahu, "Microstructural evolution and strengthening of AM90 magnesium alloy processed by ECAP," Arab. J. Sci. Eng., Vol. 42, pp. 4635–4647, 2017. [Online]. Available:  doi:10.1007/s13369-017-2508-0
[61] R. Jahadi, M. Sedighi, and H. Jahed, "ECAP effect on the micro-structure and mechanical properties of AM30 magnesium alloy," Mater. Sci. Eng. A, Vol. 593, pp. 178–184, 2014. [Online]. Available: doi:10.1016/j.msea.2013.12.033
[62] V. V. Stolyarov, Y. T. Zhu, I. V. Alexandrov, T. C. Lowe, and R. Z. Valiev, "Grain refinement and properties of pure Ti processed by warm ECAP and cold rolling," Mater. Sci. Eng. A, Vol. 343, No. 1, pp. 43–50, 2003. [Online]. Available:  doi:10.1016/S0921-5093(02)00387-9
 
 
Volume 4, Issue 2 - Serial Number 7
February 2026
Pages 47-63

  • Receive Date 12 June 2025
  • Revise Date 06 August 2025
  • Accept Date 27 August 2025
  • First Publish Date 27 August 2025
  • Publish Date 21 January 2026