Characterization of zirconium oxides part I: Raman mapping and spectral feature analysis

被引:25
作者
Efaw, Corey M. [1 ,2 ]
Vandegrift, Jordan L. [1 ,2 ]
Reynolds, Michael [1 ]
McMurdie, Samuel [1 ]
Jaques, Brian J. [1 ,2 ]
Hu, Hongqiang [3 ]
Xiong, Hui [1 ,2 ]
Hurley, Michael F. [1 ,2 ]
机构
[1] Boise State Univ, Micron Sch Mat Sci & Engn, 1910 W Univ Dr, Boise, ID 83725 USA
[2] Ctr Adv Energy Studies, 995 Univ Blvd, Idaho Falls, ID 83401 USA
[3] Idaho Natl Lab, 2525 Fremt Ave, Idaho Falls, ID 83402 USA
关键词
Zirconium alloys; Cladding; Oxidation; Breakaway; Raman mapping; TEMPERATURE PHASE-DIAGRAM; AUTOCLAVE CORROSION; REACTOR CORROSION; STRESS-ANALYSIS; PURE ZIRCONIUM; SPECTROSCOPY; OXIDATION; ALLOYS; ZIRCALOY-4; AIR;
D O I
10.1016/j.nme.2019.100707
中图分类号
TL [原子能技术]; O571 [原子核物理学];
学科分类号
0827 ; 082701 ;
摘要
Raman mapping of sectioned zirconium cladding oxides was performed to analyze different spectral features before and after breakaway, as well as between zirconium and its alloys Zr-2.65Nb, Zry-3, and Zry-4. Oxide phase composition, or percent tetragonality, was defined to compare tetragonal to monoclinic zirconia. Percent tetragonality was spatially mapped to support distinction of zirconia phase distribution. A tetragonal-rich layer was seen at the metal/oxide interface, while post-breakaway samples exhibited increased amount of tetragonal phase in the bulk of their oxides. Spatial mapping of spectral peak location and half-width at half-maximum was accomplished to distinguish differences in stability mechanisms of tetragonal-rich zirconia phase. Shifts in monoclinic peak positions provided mapping of relative stress state, supporting the differences in stabilization of tetragonal phase near the metal/oxide interface and tetragonal phase in the bulk of the oxide. Tetragonal phase near the metal/oxide interface is stabilized through support of oxygen sub-stoichiometry and compressive stress. Tetragonal phase observed in the bulk of the oxide is stabilized through oxygen sub-stoichiometry, void of compressive stress. A linear trend between percent tetragonality and stress state was determined. This resulted in a connection between mechanism of tetragonal to monoclinic phase transformation and a cladding's ability to resist oxidation and breakaway. Poor performing samples displayed greater stress gradients, driven by lattice mismatch at the metal/oxide interface, as well as between tetragonal and monoclinic phase boundaries. Tetragonal phase at the metal/oxide interface for superior performing samples have reduced epitaxial growth of tetragonal grains, lowering compressive stress gradients and provided more resistant inner-oxide layers. With increased utility of Raman spectroscopy for characterizing zirconium cladding materials, different degradation mechanisms can be further understood.
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页数:11
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