References

npe

Ядерная физика и инжиниринг

Nuclear Physics and Engineering

2079-56292079-5637

МИФИ

10.56304/S2079562925060296

MRFQVJ

npe-595

Research Article

Перспективные конструкционные материалы

Promising Structural Materials

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

FEATURES OF BORON BEHAVIOR DURING DYNAMIC STRAIN AGING IN A HIGH TEMPERATURE NI-BASED SUPERALLOY PRODUCED BY PM HIP TECHNOLOGY – II. HIGH TEMPERATURE COMPRESSION TESTING

Шульга

А. В.

Shulga

A. V.

Национальный исследовательский ядерный университет “МИФИ”РоссияNational Research Nuclear University MEPhI (Moscow Engineering Physics Institute)Russian Federation

2026

16042026

1712236

2026

Шульга А.В.

Shulga A.V.

Данная работа распространяется под лицензией Creative Commons Attribution 4.0.

This work is licensed under a Creative Commons Attribution 4.0 License.

https://npe.elpub.ru/jour/article/view/595

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).

The results of a detailed study of the structure and behavior of boron in the specimens of the high temperature nickel superalloy EP741NP produced by the PM HIP technology using the rapidly quenched powder PREP after high-temperature compression tests are presented. Compression tests of cylindrical specimens were carried out at a temperature of 1050°C and strain rates of 10–3 and 10–4 s–1. The method of track autoradiography on boron, in combination with methods of metallography (LM), (SEM), (EDX) and OIM, was used to identify the regularities of influence of changes in structural-phase state during high-temperature deformation on the features of boron distribution. The method of track autoradiography on boron provides an opportunity to study macro-, meso-, and micro-heterogeneity of boron distribution in correlation with the features of the structure-phase state. The effect of dynamic strain aging DSA involving boron in the zone of intensive plastic deformation and the occurrence of dynamic recrystallization DRX with the formation of a “necklace” structure at a deformation rate of 10–3 s–1 has been revealed. This effect consists in the intensive migration of boron in the zone of plastic deformation, resulting in the enrichment of the “necklace” area with boron and the decoration of it with dispersed precipitates of M3B2 boride phase. A decrease in the strain rate to 10–4 s–1 leads to flow instability with the manifestation of the PLC type effect and flow localization with the manifestation of a PLC type serration on the flow curve at the DRX softening stage under conditions of increased heterogeneity of the DRX structure with the formation of PLC type meso shear bands, compared to the DRX “necklace” structure. The revealed effect of DSA involving boron with the formation of meso shear bands PLC-type at the stage of DRX softening is similar to the effect of DSA involving carbon and the formation of PLC-type shear bands decorated with dispersed carbides in nickel-based superalloys and austenitic stainless steels at the stage of work hardening.

жаропрочный никелевый сплавPM HIP технологиябыстрозакаленный PREP порошокиспытания на сжатиединамическая рекристаллизация DRXструктура DRX “ожерелье” (necklace)структура DRX с мезо полосами сдвига PLC типабортрековая авторадиографияэффект DSA

high temperature nickel based superalloyPM HIP technologyrapidly quenched PREP powdercompression testingdynamic recrystallization DRXstructure DRX “necklace”meso shear band PLC typeborontrack autoradiographyDSA effect

References1

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

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

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.

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.

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.

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

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

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

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

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

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

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

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

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

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.

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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

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.

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.

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.

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

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

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.

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

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.

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.

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

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

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

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

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

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

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

The authors declare that there are no conflicts of interest present.