“…In Figure 9b, the Fe/Ni ratio is displayed in a similar manner. The protonirradiated data fits reasonably well with that in the literature and displays a retention of the mean Fe/Ni ratio between 0 and 2.3 dpa, agreeing with the observation of Etoh and Shimada that Fe/Ni remains constant for longer than Fe/Cr at low dose neutron irradiation [42]. This supports the SPP morphology evolution in Figure 5 that suggests a resistance to irradiation-induced dissolution within the Fe-Ni SPP until between 2.3 and 4.7 dpa.…”
Section: Chemical Quantificationsupporting
confidence: 89%
“…This trend is also observed in the proton-irradiated material when comparing Figure 4 and Figure 5. Etoh and Shimada et al have noted the more irregular morphology of dissolving Fe-Ni SPPs in comparison to the Fe-Cr, as have other authors [9,12,42,63]. However, the neutron fluence onset of this morphological irregularity has not been reported.…”
Section: Spp Dissolution and Amorphisationmentioning
confidence: 91%
“…These maps were quantified in at.% and the atomic fraction Fe/Cr map in c) was calculated. [9], [35] for α-annealed and β-treated material as squares and triangles, respectively, [10], [42], [49] and [12] , and analysis by atom probe tomography by [69]. Although quantification maps in the neutron-irradiated material demonstrated a lot of noise due to low concentrations in the transmission direction, obtaining the average concentration of all pixels with an alloying element concentration above background (> ~1 at.%) at high magnification after long counting times (> 30 minutes at 20 kcps) gave reliable Fe/X (X = Cr, Ni) ratios.…”
Section: Spp Dissolutionmentioning
confidence: 99%
“…This homogeneity may be related to its resistance to irradiation-induced amorphisation at irradiation temperatures 280-330 °C [40]. The Fe-Cr SPP is known to become partially amorphous at typical BWR irradiation temperatures [6,[40][41][42]. This amorphous region starts at the matrix-SPP interfacial region and progresses inwards radially at a rate ~10-13 nm per neutron fluence 1 x10 25 n m -2 under normal power reactor operating conditions [40,43,44], but at higher rates under higher fluxes and at lower temperatures [45].…”
Section: Spp Dissolution 411 Internal Spp Diffusional Capacity and mentioning
confidence: 99%
“…This amorphous region starts at the matrix-SPP interfacial region and progresses inwards radially at a rate ~10-13 nm per neutron fluence 1 x10 25 n m -2 under normal power reactor operating conditions [40,43,44], but at higher rates under higher fluxes and at lower temperatures [45]. This amorphous zone is known to be depleted in Fe relative to the crystalline SPP core [6,[40][41][42]46], and so Fe depletion from the edge region into the surrounding matrix is thought to be responsible for the amorphous transformation.…”
Section: Spp Dissolution 411 Internal Spp Diffusional Capacity and mentioning
A. Harte et al., Nano-scale chemical evolution in a proton-and neutron-irradiated Zr alloy J. Nucl. Mater. Accepted Jan. 2017 Nano-scale chemical evolution in a proton-and neutron-irradiated Zr alloy (Fe,Ni). This is accomplished through ultra-high spatial resolution scanning transmission electron microscopy and the use of energy-dispersive X-ray spectroscopic methods. Fe-depletion is observed from both SPP types after irradiation with both irradiative species, but is heterogeneous in the case of Zr(Fe,Cr) 2 , predominantly from the edge region, and homogeneously in the case of Zr 2 (Fe,Ni). Further, there is evidence of a delay in the dissolution of the Zr 2 (Fe,Ni) SPP with respect to the Zr(Fe,Cr) 2 . As such, SPP dissolution results in matrix supersaturation with solute under both irradiative species and proton irradiation is considered well suited to emulate the effects of neutron irradiation in this context. The mechanisms of solute redistribution processes from SPPs and the consequences for irradiation-induced growth phenomena are discussed.
“…In Figure 9b, the Fe/Ni ratio is displayed in a similar manner. The protonirradiated data fits reasonably well with that in the literature and displays a retention of the mean Fe/Ni ratio between 0 and 2.3 dpa, agreeing with the observation of Etoh and Shimada that Fe/Ni remains constant for longer than Fe/Cr at low dose neutron irradiation [42]. This supports the SPP morphology evolution in Figure 5 that suggests a resistance to irradiation-induced dissolution within the Fe-Ni SPP until between 2.3 and 4.7 dpa.…”
Section: Chemical Quantificationsupporting
confidence: 89%
“…This trend is also observed in the proton-irradiated material when comparing Figure 4 and Figure 5. Etoh and Shimada et al have noted the more irregular morphology of dissolving Fe-Ni SPPs in comparison to the Fe-Cr, as have other authors [9,12,42,63]. However, the neutron fluence onset of this morphological irregularity has not been reported.…”
Section: Spp Dissolution and Amorphisationmentioning
confidence: 91%
“…These maps were quantified in at.% and the atomic fraction Fe/Cr map in c) was calculated. [9], [35] for α-annealed and β-treated material as squares and triangles, respectively, [10], [42], [49] and [12] , and analysis by atom probe tomography by [69]. Although quantification maps in the neutron-irradiated material demonstrated a lot of noise due to low concentrations in the transmission direction, obtaining the average concentration of all pixels with an alloying element concentration above background (> ~1 at.%) at high magnification after long counting times (> 30 minutes at 20 kcps) gave reliable Fe/X (X = Cr, Ni) ratios.…”
Section: Spp Dissolutionmentioning
confidence: 99%
“…This homogeneity may be related to its resistance to irradiation-induced amorphisation at irradiation temperatures 280-330 °C [40]. The Fe-Cr SPP is known to become partially amorphous at typical BWR irradiation temperatures [6,[40][41][42]. This amorphous region starts at the matrix-SPP interfacial region and progresses inwards radially at a rate ~10-13 nm per neutron fluence 1 x10 25 n m -2 under normal power reactor operating conditions [40,43,44], but at higher rates under higher fluxes and at lower temperatures [45].…”
Section: Spp Dissolution 411 Internal Spp Diffusional Capacity and mentioning
confidence: 99%
“…This amorphous region starts at the matrix-SPP interfacial region and progresses inwards radially at a rate ~10-13 nm per neutron fluence 1 x10 25 n m -2 under normal power reactor operating conditions [40,43,44], but at higher rates under higher fluxes and at lower temperatures [45]. This amorphous zone is known to be depleted in Fe relative to the crystalline SPP core [6,[40][41][42]46], and so Fe depletion from the edge region into the surrounding matrix is thought to be responsible for the amorphous transformation.…”
Section: Spp Dissolution 411 Internal Spp Diffusional Capacity and mentioning
A. Harte et al., Nano-scale chemical evolution in a proton-and neutron-irradiated Zr alloy J. Nucl. Mater. Accepted Jan. 2017 Nano-scale chemical evolution in a proton-and neutron-irradiated Zr alloy (Fe,Ni). This is accomplished through ultra-high spatial resolution scanning transmission electron microscopy and the use of energy-dispersive X-ray spectroscopic methods. Fe-depletion is observed from both SPP types after irradiation with both irradiative species, but is heterogeneous in the case of Zr(Fe,Cr) 2 , predominantly from the edge region, and homogeneously in the case of Zr 2 (Fe,Ni). Further, there is evidence of a delay in the dissolution of the Zr 2 (Fe,Ni) SPP with respect to the Zr(Fe,Cr) 2 . As such, SPP dissolution results in matrix supersaturation with solute under both irradiative species and proton irradiation is considered well suited to emulate the effects of neutron irradiation in this context. The mechanisms of solute redistribution processes from SPPs and the consequences for irradiation-induced growth phenomena are discussed.
The present work concerns an investigation of the local atomic environment of Ni-containing secondary phase precipitates (SPP) present in the metal-part of Zircaloy-2 cladding tubes. An unirradiated Zircaloy-2 and two specimens irradiated in a commercial nuclear power plant are characterized using μ-focussed synchrotron radiation, and by x-ray absorption fine structure (XAFS) spectroscopy. The patterns of Ni K-edge XANES and EXAFS of SPP in unirradiated and irradiated cladding are found different. Considering the fact that Ni-bearing SPP in the unirradiated samples are mainly Zintl phase Zr 2 (Fe, Ni) type, a detailed EX-AFS analysis of near-neighbor Ni atoms has been made. The result of a curve fit for the first two shells shows that about 2 Ni(Fe) and 8 Zr atoms are coordinated at 2.68 and 2.77 Å, respectively, around a central Ni atom in the SPP. XANES data analysis provides total electronic density of states at the Fermi level of unirradiated Zr 2 (Fe, Ni). At the Ni K-edge EXAFS spectra of irradiated SPP, however, only a single scattering peak is observed demonstrating the structural disorder introduced by the neutron irradiation. The coordination number of the Ni neighboring shells is reduced markedly due to the formation of point and extended defects in the damaged SPP lattice. Dissolution of Ni from the SPP is also evident from the data. The results of this study provide a further basis for the description of both crystallographic and electronic structures of intermetallic secondphase precipitates found in Zr-based alloys.
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