Structural evolution of mechanically alloyed ODS steel powders during ball milling and subsequent annealing treatment

Abstract

In the present work, a novel 9Cr oxide-dispersion strengthened (ODS) steel powders with Y2O3 (0.5 wt%) dispersoids were synthesized by high planetary ball milling at different time intervals (2, 8, and 16 hours). The structural and crystallographical evolution of the produced powders during the ball milling and post-annealing treatment were evaluated by SEM, XRD, and micro-Vickers hardness analyses. The SEM results showed that the fine dispersions of powders were achieved with the extending milling time. When milling time was 8h, it was observed that the mean size of powders increased maximum level of 101 μm and then dramatically reduced to 5 μm at latest milling time (16h). The XRD data revealed that the crystallite size of ODS powders diminished gradually with increasing milling time. Plus, all reflection peaks of the Fe, Cr, W, Mo expanded and the diffraction peaks of the Y2O3, W progressively disappeared with the increasing milling time. The hardness results revealed that the increasing milling time was beneficial for hardness improvement, due to dominant strain hardening mechanism and it developed from 160 to 334 Hv after 16h of milling protocol. To understand high temperatures characteristics such as grain growth, phase transformation, and hardness of produced powders, 16h milled powders subjected to post-annealing treatments at 700 oC and 900 oC for 1 h. When pure Fe and Cr peaks were observed in the non-annealed powders, no evident reflection peak of Y2O3 was observed. However, all pure Fe and Cr reflection peaks became narrower and Y2O3 reflection exhibited more sharper tendency with increased annealing temperatures, which resulted in increased grain growth and formation of Fe-based oxide structures.

Keywords

• Annealing
• Ball milling
• Hardness
• 9Cr-ODS

References

1. 1. McClintock, D.A., M.A. Sokolov, D.T. Hoelzer, and R.K. Nanstad, Mechanical properties of irradiated ODS-EUROFER and nanocluster strengthened 14YWT. Journal of Nuclear Materials, 2009. 392(2): p. 353-359.
2. 2. Li, S., Z. Zhou, J. Jang, M. Wang, H. Hu, H. Sun, and L. Zhang, The influence of Cr content on the mechanical properties of ODS ferritic steels. Journal of Nuclear Materials, 2014. 455(1-3): p. 194-200.
3. 3. Li, W., T. Hao, R. Gao, X. Wang, T. Zhang, Q. Fang, and C. Liu, The effect of Zr, Ti addition on the particle size and microstructure evolution of yttria nanoparticle in ODS steel. Powder Technology, 2017. 319: p. 172-182.
4. 4. Chen, C.L. and Y.M. Dong, Effect of mechanical alloying and consolidation process on microstructure and hardness of nanostructured Fe–Cr–Al ODS alloys. Materials Science and Engineering: A, 2011. 528(29-30): p. 8374-8380.
5. 5. Zinkle, S. and N. Ghoniem, Operating temperature windows for fusion reactor structural materials. Fusion Engineering and Design, 2000. 51: p. 55-71.
6. 6. Klueh, R.L., J.P. Shingledecker, R.W. Swindeman, and D.T. Hoelzer, Oxide dispersion-strengthened steels: A comparison of some commercial and experimental alloys. Journal of Nuclear Materials, 2005. 341(2-3): p. 103-114.
7. 7. Li, Z., Z. Lu, R. Xie, C. Lu, Y. Shi, and C. Liu, Effects of Y2O3, La2O3 and CeO2 additions on microstructure and mechanical properties of 14Cr-ODS ferrite alloys produced by spark plasma sintering. Fusion Engineering and Design, 2017. 121: p. 159-166.
8. 8. Chen, C., P. Wang, and G. Tatlock, Phase transformations in yttrium–aluminium oxides in friction stir welded and recrystallised PM2000 alloys. Materials at High Temperatures, 2009. 26(3): p. 299-303.

9. 9. He, P., J. Hoffmann, and A. Möslang, Effect of milling time and annealing temperature on nanoparticles evolution for 13.5% Cr ODS ferritic steel powders by joint application of XAFS and TEM. Journal of Nuclear Materials, 2018. 501: p. 381-387.
10. 10. Gökmese, H., B. Bostan, T.A Yilmaz, and U. Tasci, TEM characterization and synthesis of nanoparticle B4C by high-energy milling. International Advanced Researches and Engineering Journal, 2019. 3(3): p. 195-201.
11. 11. Aktas, S. and E.A. Diler, A review on the effects of micro-nano particle size and volume fraction on microstructure and mechanical properties of metal matrix composites manufactured via mechanical alloying. International Advanced Researches and Engineering Journal, 2018. 2(1): p. 68-74.
12. 12. Raghavendra, K.G., A. Dasgupta, P. Bhaskar, K. Jayasankar, C.N. Athreya, P. Panda, S. Saroja, V.S. Sarma, and R. Ramaseshan, Synthesis and characterization of Fe-15 wt.% ZrO2 nanocomposite powders by mechanical milling. Powder Technology, 2016. 287: p. 190-200.
13. 13. Hoffmann, J., M. Rieth, R. Lindau, M. Klimenkov, A. Möslang, and H.R.Z Sandim, Investigation on different oxides as candidates for nano-sized ODS particles in reduced-activation ferritic (RAF) steels. Journal of Nuclear Materials, 2013. 442(1-3): p. 444-448.
14. 14. Kotan, H., K.A. Darling, R.O. Scattergood, and C.C Koch, Influence of Zr and nano-Y2O3 additions on thermal stability and improved hardness in mechanically alloyed Fe base ferritic alloys. Journal of alloys and compounds, 2014. 615: p. 1013-1018.
15. 15. Ukai, S., M. Harada, H. Okada, S. Nomura, S. Shikakura, K. Asabe, T. Nishida, and M. Fujiwara, Alloying design of oxide dispersion strengthened ferritic steel for long life FBRs core materials. Journal of Nuclear Materials, 1993. 204: p. 65-73.
16. 16. Kimura, A., R. Kasada, N. Iwata, H. Kishimoto, C.H. Zhang, J. Isselin, P. Dou, J.H. Lee, N. Muthukumar, T. Okuda, M. Inoue, S. Ukai, S. Ohnuki, T. Fujisawa, and F. Abe, Development of Al added high-Cr ODS steels for fuel cladding of next generation nuclear systems. Journal of Nuclear Materials, 2011. 417(1-3): p. 176-179.
17. 17. Isselin, J., R. Kasada, A. Kimura, T. Okuda, M. Inoue, S. Ukai, S. Ohnuki, T. Fujisawa, and F. Abe, Effects of Zr addition on the microstructure of 14% Cr4% Al ODS ferritic steels. Materials transactions, 2010. 51(5): p. 1011-1015.
18. 18. Hoelzer, D. T., J. Bentley, M.A. Sokolov, M.K. Miller, G.R. Odette, and M.J. Alinger, Influence of particle dispersions on the high-temperature strength of ferritic alloys. Journal of Nuclear Materials, 2007. 367: p. 166-172.
19. 19. Xu, H., Z. Lu, S. Ukai, N. Oono, and C. Liu, Effects of annealing temperature on nanoscale particles in oxide dispersion strengthened Fe-15Cr alloy powders with Ti and Zr additions. Journal of Alloys and Compounds, 2017. 693: p. 177-187.
20. 20. Toloczko, M.B., D.S. Gelles, F.A. Garner, R.J. Kurtz, and K. Abe, Irradiation creep and swelling from 400 to 600 C of the oxide dispersion strengthened ferritic alloy MA957. Journal of nuclear materials, 2004. 329: p. 352-355.
21. 21. Xu, Z., S. Liu, L. Song, X. Yang, Y. Zhao, and X. Mao, Effect of silicon on oxidation behavior of 9Cr-ODS steel at 650° C. Fusion Engineering and Design, 2021. 167: p. 112384.
22. 22. Polat, G., A.B. Batibay, and H. Kotan, Understanding microstructural evolution and hardness of nanostructured Fe89.5Ni8Zr2.5 alloy produced by mechanical alloying and pressureless sintering. Engineering Science and Technology, an International Journal, 2020. 23(5): p. 1279-1284.
23. 23. Xu, S., Z. Zhou, F. Long, H. Jia, N. Guo, Z. Yao, and M.R. Daymond, Combination of back stress strengthening and Orowan strengthening in bimodal structured Fe–9Cr–Al ODS steel with high Al addition. Materials Science and Engineering: A, 2019. 739: p. 45-52.
24. 24. Kotan, H., Effect of Y and nano Y2O3 additions on grain growth and hardness of nanocrystalline austenitic stainless steels produced by mechanical alloying. Journal of the Faculty of Engineering and Architecture of Gazi University, 2019. 34(3): p. 1266-1272.
25. 25. Kotan, H., Thermal stability, phase transformation and hardness of mechanically alloyed nanocrystalline Fe-18Cr-8Ni stainless steel with Zr and Y2O3 additions. Journal of Alloys and Compounds, 2018. 749: p. 948-954.
26. 26. Darling, K.A., M. Kapoor, H. Kotan, B.C. Hornbuckle, S.D. Walck, G.B. Thompson, M.A. Tschopp, L.J. Kecskes, Structure and mechanical properties of Fe–Ni–Zr oxide-dispersion-strengthened (ODS) alloys. Journal of Nuclear Materials, 2015. 467: p. 205-213.
27. 27. Mihalache, V. I. Mercioniu, A. Velea, P. Palade, Effect of the process control agent in the ball-milled powders and SPS-consolidation temperature on the grain refinement, density and Vickers hardness of Fe14Cr ODS ferritic alloys. Powder Technology, 2019. 347: p. 103-113.
28. 28. Sandim, H.R.Z., R.A. Renzetti, A.F. Padilha, D. Raabe, M. Klimenkov, R. Lindau, and A. Möslang, Annealing behavior of ferritic–martensitic 9% Cr–ODS–Eurofer steel. Materials Science and Engineering: A, 2010. 527(15): p. 3602-3608.
29. 29. Shi, W., L. Yu, C. Liu, Z. Ma, H. Li, Z. Wang, Y. Liu, Q. Gao, and H. Wang, Evolution of Y2O3 precipitates in ODS-316 L steel during reactive-inspired ball-milling and spark plasma sintering processes. Powder Technology, 2022. 398: p. 117072.
30. 30. Song, Q.S., Y. Zhang, Y.F. Wei, X.Y. Zhou, Y.F. Shen, Y.M. Zhou, and X.M. Feng, Microstructure and mechanical performance of ODS superalloys manufactured by selective laser melting. Optics & Laser Technology, 2021. 144: p. 107423.
31. 31. Salur, E., C. Nazik, M. Acarer, I. Savkliyildiz, and E.K. Akdogan, Ultrahigh hardness in Y2O3 dispersed ferrous multicomponent nanocomposites. Materials Today Communications, 2021. 28: p. 102637.
32. 32. Salur, E., M. Acarer, and İ. Şavkliyildiz, Improving mechanical properties of nano-sized TiC particle reinforced AA7075 Al alloy composites produced by ball milling and hot pressing. Materials Today Communications, 2021. 27: p. 102202.
33. 33. Salur, E., A. Aslan, M. Kuntoglu, and M. Acarer, Effect of ball milling time on the structural characteristics and mechanical properties of nano-sized Y2O3 particle reinforced aluminum matrix composites produced by powder metallurgy route. Advanced Powder Technology, 2021. 32(10): p. 3826-3844.
34. 34. Salur, E., Synergistic effect of ball milling time and nano-sized Y2O3 addition on hardening of Cu-based nanocomposites. Archives of Civil and Mechanical Engineering, 2022. 22(2): p. 1-18.
35. 35. Doğan, K., M.I. Ozgun, H. Subutay, E. Salur, Y.R. Eker, M. Kuntoglu, A. Aslan, M.K. Gupta, M. Acarer, Dispersion mechanism-induced variations in microstructural and mechanical behavior of CNT-reinforced aluminum nanocomposites. Archives of Civil and Mechanical Engineering, 2022. 22(1): p. 1-17.
36. 36. Patterson, A., The Scherrer formula for X-ray particle size determination. Physical review, 1939. 56(10): p. 978.
37. 37. Bicer, H., E.K. Akdogan, I. Savkliyildiz, C. Haines, Z. Zhong, and T. Tsakalakos, Thermal expansion of nano–boron carbide under constant DC electric field: An in situ energy dispersive X-ray diffraction study using a synchrotron probe. Journal of Materials Research, 2020. 35(1): p. 90-97.
38. 38. Albaaji, A.J., E.G. Castle, M.J. Reece, J.P. Hall, and S.L. Evans, Effect of ball-milling time on mechanical and magnetic properties of carbon nanotube reinforced FeCo alloy composites. Materials & Design, 2017. 122: p. 296-306.
39. 39. Xiong, H., Z. Li, X. Gan, L. Chai, and K. Zhou, High-energy ball-milling combined with annealing of TiC powders and its influence on the microstructure and mechanical properties of the TiC-based cermets. Materials Science and Engineering: A, 2017. 694: p. 33-40.
40. 40. Tekin, M., G. Polat, Y.E. Kalay, and H. Kotan, Grain size stabilization of oxide dispersion strengthened CoCrFeNi-Y2O3 high entropy alloys synthesized by mechanical alloying. Journal of Alloys and Compounds, 2021. 887: p. 161363.
41. 41. Ohtsuka, S., S. Ukai, M. Fujiwara, T. Kaito, and T. Narita, Improvement of 9Cr-ODS martensitic steel properties by controlling excess oxygen and titanium contents. Journal of Nuclear Materials, 2004. 329: p. 372-376.
42. 42. Nowik, K. and Z. Oksiuta, Microstructure, Grain Growth and Hardness of Nanostructured Ferritic ODS Steel Powder during Annealing. Metallography, Microstructure, and Analysis, 2021. 10(3): p. 355-366.