Understanding irradiation-induced nanoprecipitation in zirconium alloys using parallel TEM and APT

A. Harte; R. Prasath Babu; C. A. Hirst; Tomas L Martin; P. A.J. Bagot; M. P. Moody; P. Frankel; J. Romero; L. Hallstadius; E. C. Darby; M. Preuss

doi:10.1016/j.jnucmat.2018.08.033

Understanding irradiation-induced nanoprecipitation in zirconium alloys using parallel TEM and APT

A. Harte^*, R. Prasath Babu, C. A. Hirst, Tomas L Martin, P. A.J. Bagot, M. P. Moody, P. Frankel, J. Romero, L. Hallstadius, E. C. Darby, M. Preuss

^*Corresponding author for this work

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Abstract

We investigate nano-scale irradiation-induced precipitation in a Zr–Sn–Fe–Cr–Ni-alloy (Zircaloy-2) by combining atom probe tomography (APT) for chemical detail with scanning transmission electron microscopy (STEM) and high resolution energy dispersive X-ray (EDX) spectroscopy for wider context and complimentary and correlative TEM diffraction techniques for crystallographic relationships. We find that Fe– and Cr-rich nano-rods precipitate in Zircaloy-2 following proton irradiation at 350 °C to a low dose of ∼2 dpa. The long-axis of the nano-rods are aligned in a direction 12–15° from the Zr matrix 〈0001〉 align in the basal plane and are of width 1.5–5 nm. Smaller rods are of APT-determined composition Zr₄(Fe_0.67Cr_0.33), tending towards Zr₃(Fe_0.69Cr_0.31) as the rod volume increases to > ∼400 nm³, in agreement with STEM-EDX determination of composition resembling that of Zr₃Fe with Cr replacing some of the Fe. The Fe/Cr ratio has been shown to increase with distance from the nearest partially-dissolved Zr(Fe,Cr)₂ phase particle. The nucleation of nano rods has implications for macroscopic irradiation-induced deformation phenomena, irradiation-induced hardening and the evolution of dislocation loops and other defects.

Original language	English
Pages (from-to)	460-471
Number of pages	12
Journal	Journal of Nuclear Materials
Volume	510
Early online date	17 Aug 2018
DOIs	https://doi.org/10.1016/j.jnucmat.2018.08.033
Publication status	Published - 1 Nov 2018

Keywords

Atom probe tomography
Irradiation
Nano precipitation
Transmission electron microscopy
Zirconium

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title = "Understanding irradiation-induced nanoprecipitation in zirconium alloys using parallel TEM and APT",

abstract = "We investigate nano-scale irradiation-induced precipitation in a Zr–Sn–Fe–Cr–Ni-alloy (Zircaloy-2) by combining atom probe tomography (APT) for chemical detail with scanning transmission electron microscopy (STEM) and high resolution energy dispersive X-ray (EDX) spectroscopy for wider context and complimentary and correlative TEM diffraction techniques for crystallographic relationships. We find that Fe– and Cr-rich nano-rods precipitate in Zircaloy-2 following proton irradiation at 350 °C to a low dose of ∼2 dpa. The long-axis of the nano-rods are aligned in a direction 12–15° from the Zr matrix 〈0001〉 align in the basal plane and are of width 1.5–5 nm. Smaller rods are of APT-determined composition Zr4(Fe0.67Cr0.33), tending towards Zr3(Fe0.69Cr0.31) as the rod volume increases to > ∼400 nm3, in agreement with STEM-EDX determination of composition resembling that of Zr3Fe with Cr replacing some of the Fe. The Fe/Cr ratio has been shown to increase with distance from the nearest partially-dissolved Zr(Fe,Cr)2 phase particle. The nucleation of nano rods has implications for macroscopic irradiation-induced deformation phenomena, irradiation-induced hardening and the evolution of dislocation loops and other defects.",

keywords = "Atom probe tomography, Irradiation, Nano precipitation, Transmission electron microscopy, Zirconium",

author = "A. Harte and Babu, {R. Prasath} and Hirst, {C. A.} and Martin, {Tomas L} and Bagot, {P. A.J.} and Moody, {M. P.} and P. Frankel and J. Romero and L. Hallstadius and Darby, {E. C.} and M. Preuss",

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doi = "10.1016/j.jnucmat.2018.08.033",

language = "English",

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journal = "Journal of Nuclear Materials",

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TY - JOUR

T1 - Understanding irradiation-induced nanoprecipitation in zirconium alloys using parallel TEM and APT

AU - Harte, A.

AU - Babu, R. Prasath

AU - Hirst, C. A.

AU - Martin, Tomas L

AU - Bagot, P. A.J.

AU - Moody, M. P.

AU - Frankel, P.

AU - Romero, J.

AU - Hallstadius, L.

AU - Darby, E. C.

AU - Preuss, M.

PY - 2018/11/1

Y1 - 2018/11/1

N2 - We investigate nano-scale irradiation-induced precipitation in a Zr–Sn–Fe–Cr–Ni-alloy (Zircaloy-2) by combining atom probe tomography (APT) for chemical detail with scanning transmission electron microscopy (STEM) and high resolution energy dispersive X-ray (EDX) spectroscopy for wider context and complimentary and correlative TEM diffraction techniques for crystallographic relationships. We find that Fe– and Cr-rich nano-rods precipitate in Zircaloy-2 following proton irradiation at 350 °C to a low dose of ∼2 dpa. The long-axis of the nano-rods are aligned in a direction 12–15° from the Zr matrix 〈0001〉 align in the basal plane and are of width 1.5–5 nm. Smaller rods are of APT-determined composition Zr4(Fe0.67Cr0.33), tending towards Zr3(Fe0.69Cr0.31) as the rod volume increases to > ∼400 nm3, in agreement with STEM-EDX determination of composition resembling that of Zr3Fe with Cr replacing some of the Fe. The Fe/Cr ratio has been shown to increase with distance from the nearest partially-dissolved Zr(Fe,Cr)2 phase particle. The nucleation of nano rods has implications for macroscopic irradiation-induced deformation phenomena, irradiation-induced hardening and the evolution of dislocation loops and other defects.

AB - We investigate nano-scale irradiation-induced precipitation in a Zr–Sn–Fe–Cr–Ni-alloy (Zircaloy-2) by combining atom probe tomography (APT) for chemical detail with scanning transmission electron microscopy (STEM) and high resolution energy dispersive X-ray (EDX) spectroscopy for wider context and complimentary and correlative TEM diffraction techniques for crystallographic relationships. We find that Fe– and Cr-rich nano-rods precipitate in Zircaloy-2 following proton irradiation at 350 °C to a low dose of ∼2 dpa. The long-axis of the nano-rods are aligned in a direction 12–15° from the Zr matrix 〈0001〉 align in the basal plane and are of width 1.5–5 nm. Smaller rods are of APT-determined composition Zr4(Fe0.67Cr0.33), tending towards Zr3(Fe0.69Cr0.31) as the rod volume increases to > ∼400 nm3, in agreement with STEM-EDX determination of composition resembling that of Zr3Fe with Cr replacing some of the Fe. The Fe/Cr ratio has been shown to increase with distance from the nearest partially-dissolved Zr(Fe,Cr)2 phase particle. The nucleation of nano rods has implications for macroscopic irradiation-induced deformation phenomena, irradiation-induced hardening and the evolution of dislocation loops and other defects.

KW - Atom probe tomography

KW - Irradiation

KW - Nano precipitation

KW - Transmission electron microscopy

KW - Zirconium

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U2 - 10.1016/j.jnucmat.2018.08.033

DO - 10.1016/j.jnucmat.2018.08.033

M3 - Article (Academic Journal)

AN - SCOPUS:85052322085

SN - 0022-3115

VL - 510

SP - 460

EP - 471

JO - Journal of Nuclear Materials

JF - Journal of Nuclear Materials

ER -

Understanding irradiation-induced nanoprecipitation in zirconium alloys using parallel TEM and APT

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