ОСОБЕННОСТИ ПОВЕДЕНИЯ БОРА ПРИ ДИНАМИЧЕСКОМ ДЕФОРМАЦИОННОМ СТАРЕНИИ В ЖАРОПРОЧНОМ НИКЕЛЕВОМ СУПЕРСПЛАВЕ, ПОЛУЧЕННОМ ПО PM HIP ТЕХНОЛОГИИ – II. ИСПЫТАНИЕ НА ВЫСОКОТЕМПЕРАТУРНОЕ СЖАТИЕ

Представлены результаты детального изучения особенностей структуры и поведения бора в жаропрочном никелевом суперсплаве EP741NP, полученном по PM HIP технологии с использованием быстрозакаленного PREP порошка, при высокотемпературном испытании на сжатие. Испытания на сжатие цилиндрических образцов проводились при температуре 1050°С и скоростях деформации 10^–3 и 10^–4 с^–1. Метод трековой авторадиографии по бору в сочетании с методами металлографии LM, SEM, EDX и OIM применялись для выявления закономерностей влияния изменения структурно-фазового состояния при высокотемпературной деформации на особенности распределения бора. Метод трековой авторадиографии по бору обеспечивает возможность изучения макро-, мезо- и микро неоднородности распределения бора в корреляции с особенностями структурно-фазового состояния. Выявлен эффект динамического деформационного старения DSA с участием бора в зоне интенсивной пластической деформации и протекания динамической рекристаллизации DRX с образованием структуры DRX “ожерелье” при скорости деформации 10^–3 с^–1, заключающийся в интенсивной миграции бора в зоне пластической деформации с обогащением “ожерелья” бором и декорированием его дисперсными выделениями боридной фазы типа M₃B₂. Снижение скорости деформации до 10^–4 с^–1 приводит к нестабильности течения с проявлением эффекта типа Портевена–Ле Шателье PLC и локализации течения с проявлением зуба (PLC type serration) на кривой течения, на стадии разупрочнения (DRX softening) в условиях повышения неоднородности DRX структуры с образованием мезо полос сдвига PLC типа (PLC type shear bands), по сравнению со структурой DRX “ожерелье”. Выявленный эффект DSA с участием бора с образованием мезо полос сдвига PLC типа на стадии разупрочнения (DRX softening) аналогичен эффекту DSA с участием углерода и образованием полос сдвига PLC типа, декорированных дисперсными карбидами в суперсплавах на основе никеля и аустенитных коррозионно-стойких сталях на стадии деформационного упрочнения (Work hardening).

1. Pollock T.M. Alloy design for aircraft engines // Nat. Mater. 2016. V. 15. P. 809–815. https://doi.org/10.1038/nmat4709

2. He Z., Jiang Y., Chang L., Huang H. Helium ion irradiation-induced damage of powder metallurgy-hot isostatic pressed Ni-based alloy GH3535 for molten salt reactor applications // J. Nucl. Mater. 2024. V. 589. P. 154871. https://doi.org/10.1016/j.jnucmat.2023.154871

3. Shulga A.V., Ofitserov A.A., Kuzmicheva L.G. Analysis of carbon and boron behavior in PM Ni base superalloys of the type EP741NP. Proc. World PM Congress and Exhibition. Vienna, Austria. 2004. V. 4. P. 731–736.

4. Shulga A.V. A multiscale study of boron and carbon behavior in the necking and fracture zones of the high temperature Ni-based superalloy under high temperature tensile testing. Proc. World PM Congress and Exhibition. October 9–13, 2022. Lyon, France. High Temperature Materials. P. 1–6.

5. Shulga A.V. Effect of the heat treatment on the microstructure, boron distribution and flow stress of the Ni-based superalloy PM HIP compact under high temperature compression tests. Proc. World PM Congress and Exhibition. October 9–13, 2016. Hamburg, Germany. HIP – Process. P. 1–6.

6. Shulga A.V. A comparative study of the mechanical properties and the behavior of carbon and boron in stainless steel cladding tubes fabricated by PM HIP and traditional technologies // J. Nucl. Mater. 2013. V. 434. P. 133–140. https://doi.org/10.1016/j.jnucmat.2012.11.008

7. Beese A.M., Wang Z., Stoica A.D., Ma D. Absence of dynamic strain aging in an additively manufactured nickel-base superalloy // Nat. Commun. 2018. V. 9. P. 2083. https://doi.org/10.1038/s41467-018-04473-5

8. Yu H., Fu J., Wang C., Chen Y., Wang L., Fang H., Li J., Zwaag S. v. d., Xu W. Robust additive manufacturable Ni superalloys designed by the integrated optimization of local elemental segregation and cracking susceptibility criteria // Acta Mater. 2024. V. 266. P. 119658. https://doi.org/10.1016/j.actamat.2024.119658

9. Ren N., Li J., Zhang R., Panwisawas C., Xia1 M., Dong H., Li J. Solute trapping and non-equilibrium microstructure during rapid solidification of additive manufacturing // Nat Commun. 2023. V. 14. P. 7990. https://doi.org/10.1038/s41467-023-43563-x

10. Dörries K., Haberland C., Burow J., Rösler J., Gehrmann B., Somsen C., Piegert S., Brodin H. Beyond Hot Cracking: Impact of Minor Elements on a Novel Ni-Based Superalloy for Additive Manufacturing. In: Superalloys 2024. J. Cormier, I. Edmonds, S. Forsik, P. Kontis, C. O’Connell, T. Smith, A. Suzuki, S. Tin, J. Zhang (Eds.) The Minerals, Metals and Materials Series. 2024. Cham: Springer. P. 871–882. https://doi.org/10.1007/978-3-031-63937-1_81

11. Bagot P.A.J., Silk O.B.W., Douglas J.O., Pedrazzini S., Crudden D.J., Martin T.L., Hardy M.C., Moody M.P., Reed R.C. An Atom Probe Tomography study of site preference and partitioning in a nickel-based superalloy // Acta Mater. 2017. V. 125. P. 156–165. https://doi.org/10.1016/j.actamat.2016.11.053

12. Kontis P., Mohd Yusof H.A., Pedrazzini S., Danaie M., Moore K.L., Bagot P.A.J., Moody M.P., Grovenor C.R.M., Reed R.C. On the effect of boron on grain boundary character in a new polycrystalline superalloy // Acta Mater. 2016. V. 103. P. 688–699. https://doi.org/10.1016/j.actamat.2015.10.006

13. Gopinath K., Gogia A.K., Kamat S.V., Ramamurty U. Dynamic strain ageing in Ni-base superalloy 720Li // Acta Mater. 2009. V. 57 (4). P. 1243–1253. https://doi.org/10.1016/j.actamat.2008.11.005

14. Shulga A.V. Comparative Study of the Structure Features of Rapidly Quenched REP Powders, PM HIP Compacts, and Products of Austenitic Stainless Steels and Their Traditional Counterparts // Phys. At. Nucl. 2023. V. 86 (9). P. 1998–2012. https://doi.org/10.1134/S1063778823090235

15. Shulga A.V. Anomalous Particles (Granules) in PREP-Powders. A Multiscale Study of the Structure Evolution of the PM HIP Stainless Steels under Hot Deformation and Heat Treatment. Proc. World PM Congress and Exibition. October 9–13, 2022. Lyon, France. Hot Isostatic Pressing. P. 1–6.

16. Porollo S.I., Konobeev Yu.V., Garner F.A. Swelling and microstructure of austenitic stainless steel ChS-68 CW after high dose neutron irradiation // J. Nucl. Mater. 2009. V. 393. P. 61–66. https://doi.org/10.1016/j.jnucmat.2009.05.005

17. Lee S.-Y., Takushima C., Hamada J., Nakada N. Macroscopic and microscopic characterizations of Portevin-LeChatelier effect in austenitic stainless steel using high-temperature digital image correlation analysis // Acta Mater. 2021. V. 205. P. 116560. https://doi.org/10.1016/j.actamat.2020.116560

18. Aboulfadl H., Deges J., Choi P., Raabe D. Dynamic strain aging studied at the atomic scale // Acta Mater. 2015. V. 86. P. 34–42. https://doi.org/10.1016/j.actamat.2014.12.028

19. Epperly E.N., Sills R.B. Transient solute drag and strain aging of dislocations // Acta Mater. 2020. V. 193. P. 1–9. https://doi.org/10.1016/j.actamat.2020.03.031

20. Charpagne M.A., Hestroffer J.M., Polonsky A.T., Echlin M.P., Texier D., Valle V., Beyerlein I.J., Pollock T.M., Stinville J.C. Slip localization in Inconel 718: A three-dimensional and statistical perspective // Acta Mater. 2021. V. 215. P. 117037. https://doi.org/10.1016/j.actamat.2021.117037

21. Ho H., Risbet M., Feaugas X. On the unified view of the contribution of plastic strain to cyclic crack initiation: impact of the progressive transformation of shear bands to persistent slip bands // Acta Mater. 2015. V. 85. P. 155–167. https://doi.org/10.1016/j.actamat.2014.11.020

22. Stinville J.C., Martin E., Karadge M., Ismonov S., Soare M., Hanlon T., Sundaram S., Echlin M.P., Callahan P.G., Lenthe W.C., Miller V.M., Miao J., Wessman A.E., Finlay R., Loghin A., Marte J., Pollock T.M. Fatigue deformation in a polycrystalline nickel base superalloy at intermediate and high temperature: competing failure modes // Acta Mater. 2018. V. 152. P. 16–33. https://doi.org/10.1016/j.actamat.2018.03.035

23. Nikulin I., Kaibyshev R. Deformation behavior and the Portevin-Le Chatelier effect in a modified 18Cr–8Ni stainless steel // Mater. Sci. Eng. A. 2011. V. 528. P. 1340–1347. https://doi.org/10.1016/j.msea.2010.10.056

24. Sills R.B., Cai W. Solute drag on perfect and extended dislocations // Philos. Mag. 2016. V. 96. P. 895–921. https://doi.org/10.1080/14786435.2016.1142677

25. Peng G., Gan X., Jiang Y., Li Z., Zhou K. Effect of dynamic strain aging on the deformation behavior and microstructure of Cu–15Ni–8Sn alloy // J. Alloys Compd. 2017. V. 718. P. 182–187. https://doi.org/10.1016/j.jallcom.2017.05.127

26. Zhang X., Zhou D., Li Y., Zhang D. Concurrent dynamic strain aging and dynamic precipitation evades strength-ductility trade-off in a high Mg-content aluminum crossover alloy // Mater. Sci. Eng. A. 2022. V. 854. P. 143800. https://doi.org/10.1016/j.msea.2022.143800

27. Caillard D. Dynamic strain ageing in iron alloys: The shielding effect of carbon // Acta Mater. 2016. V. 112. P. 273–284. https://doi.org/10.1016/j.actamat.2016.04.018

28. Zhao G., Zang X’., Jing Y., Lü N., Wu J. Role of carbides on hot deformation behavior and dynamic recrystallization of hard-deformed superalloy U720Li // Mater. Sci. Eng. A. 2021. V. 815. P. 141293.https://doi.org/10.1016/j.msea.2021.141293

29. Cui C., Zhang R., Zhou Y., Sun X. Portevin-Le Châtelier effect in wrought Ni-based superalloys: Experiments and mechanisms // J. Mater. Sci. Technol. 2020. V. 51. P. 16–31. https://doi.org/10.1016/j.jmst.2020.03.023

30. Koyama M., Sawaguchi T., Tsuzaki K. Overview of dynamic strain aging and associated phenomena in Fe–Mn–C austenitic steels // ISIJ Int. 2018. V. 58 (8). P. 1383–1395. https://doi.org/10.2355/isijinternational.ISIJINT-2018-237

31. Jin D., Li J., Shao N. The effect of dynamic strain aging on fatigue property for 316L stainless steel // J. Mater. Res. 2016. V. 31 (5). P. 627–634. https://doi.org/10.1557/jmr.2016.49

32. Kuang W., Was G.S. The effects of strain rate and carbon concentration on the dynamic strain aging of cold rolled Ni-based alloy in high temperature water // Scr. Mater. 2015. V. 107. P. 107–110. https://doi.org/10.1016/j.scriptamat.2015.05.033

33. Hayes R.W., Hayes R.W., Hayes W.C. On the mechanism of delayed discontinuous plastic flow in an age-hardened nickel alloy // Acta Metall. 1982. V. 30. . 1295–1301.

34. Hayes R.W. On a proposed theory for the disappearance of serrated flow in F.C.C Ni alloys // Acta Metall. 1983. V. 31. P. 365–371.

35. Karlsson L., Nordén H., Odelius H. Non-equilibrium grain boundary segregation of boron in austenitic stainless steel – I. Large scale segregation behaviour // Acta Metall. 1988. V. 36 (1). P. 1–12.

36. Shulga A.V. The Nature of Anomalous Particles (Granules) in Rapidly Quenched PREP Powders: III. Multiscale Study of Behavior of Boron and Carbon in PM HIP Compacts of High Temperature Ni-Based Superalloys under Hot Deformation and Heat Treatment // Phys. At. Nucl. 2021. V. 84 (11). P. 1801–1816. https://doi.org/10.1134/S1063778821090325

37. Wang H., Zhang H., Liu C., Ruan J., Huang H., Zhou X., Meng F., Zhu L., Zhang S., Jiang L. Hot deformation behavior, superplasticity and microstructure evolution of a new hot isostatic pressed nickel-based superalloy // Mater. Sci. Eng. A. 2024. V. 891. P. 145997. https://doi.org/10.1016/j.msea.2023.145997

38. Monajati H., Jahazi M., Yue S., Taheri A.K. Deformation Characteristics of Isothermally Forged UDIMET 720 Nickel-Base Superalloy Metall. Mater. Trans. A. 2025. V. 36a. P. 895–905.

39. Ning Y., Yao Z., Fu M.W., Guo H. Dynamic recrystallization of the hot isostatically pressed P/M superalloy FGH4096 in hot working process // Mater. Sci. Eng. A. 2010. V. 527 (26). P. 6968−6974. https://doi.org/10.1016/j.msea.2010.07.018

40. Shulga A.V. Analysis of Boron Behavior in the High-Temperature Ni-Based PM HIP Superalloys by the Use of a Firstly Proposed TTT Diagram. Proc. Euro PM 2023 Congress and Exibition. October 1–4, 2023. High Temperature Materials – Ni and Co based Superalloys. P. 1–7.

41. Chiba K., Katagiri T., Fujii K., Saga T. High temperature oxidation of Boronized nickel // J. Japan Heat. reat. 1991. V. 31. № 5. P. 273–278.

42. Kubaschewski O., Alcock C.B. Metallurgical thermochemistry 1979. Oxford: Pergamon Press.

43. He G., Liu F., Huang L., Huang Z., Jiang L. Microstructure evolutions and nucleation mechanisms of dynamic

44. recrystallization of a powder metallurgy Ni-based superalloy during hot compression // Mater. Sci. Eng. A. 2016. V. 677. P. 496–504. https://doi.org/10.1016/j.msea.2016.09.083

45. Liu Yan-Xing, Lin Y.C., Li Hong-Bin, Wen Dong-Xu, Chen Xiao-Min, Chen Ming-Song. Study of dynamic recrystallization in a Ni-based superalloyby experiments and cellular automaton model // Mater. Sci. Eng. A. 2015. V. 626. P. 432–440. https://doi.org/10.1016/j.msea.2014.12.092

46. Eleti R.R., Chokshi A.H., Shibata A., Tsuji N. Unique high-temperature deformation dominated by grain boundary sliding in heterogeneous necklace structure formed by dynamic recrystallization in HfNbTaTiZr BCC refractory high entropy alloy // Acta Mater. 2020. V. 183. P. 64–77. https://doi.org/10.1016/j.actamat.2019.11.001

47. Jullien M., Black R.L., Stinville J.C., Legros M., Texier D. Strain Rate Effect on Strain Localization in Alloy 718 Ni-Based Superalloy at Intermediate Temperature. In: Superalloys 2024. J. Cormier, I. Edmonds, S. Forsik, P. Kontis, C. O’Connell, T. Smith, A. Suzuki, S. Tin, J. Zhang (Eds.). The Minerals, Metals and Materials Series. 2024. Cham: Springer. P. 278–286. https://doi.org/10.1007/978-3-031-63937-1_26

48. Wan Z., Hu L., Sun Y., Wang T., Li Z. Hot deformation behavior and processing workability of a Ni-based alloy // J. Alloys Compd. 2018. V. 769. P. 367–375. https://doi.org/10.1016/j.jallcom.2018.08.010