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214 Francois Vurpillot et al.


Figure 4. a: Three-dimensional (3D) field-ion microscopy (FIM) images of two NbN Guinier–Preston (GP) zones in a model steel. A small 2D selection of FIM images around a bright contrast effect, which is interpreted as GP zones. About 1,000 FIM images were used to reconstruct a small volume containing two identified objects (b–g) and (h–i) The 3D reconstruction displays the presence of two monoatomic platelets at an angle of 90° from each other, and a 45° angle with respect to the <011> direction (atomic planes imaged using a grayscale).


intersecting the specimen’s surface. With standard FIM images it is barely possible to deduce the morphologies of the evaporated features. The algorithm described previously was utilized in the square white region of Figure 4a. 3D FIM reconstructions provided clear evidence for the planar morphology of precipitates (platelets). From the local brightness contrast, these objects can be isolated from the matrix using a simple threshold technique. Two of these platelets are present in the investigated volume, and are displayed, Figures 4h and 4i. As atomic resolution is achieved in all 3D, the crystallographic orientation and scaling of the


represented volume are straightforward. The specimen was field evaporated along the [011] direction (parallel to the specimen’s long axis). The two platelets are demonstrated to lie on perpendicular (010) and (001) planes. As the three {001} planes are equivalent in a cubic lattice, two of the three variants of precipitates are displayed in this 3D reconstruc- tion.The question of the chemical composition and coherency of the precipitates was addressed by APT and HRTEM, which provided the first evidence for Guinier–Preston (GP)


zones in steels. One of the difficulties faced classically when dealing with chemical analyses in N-bearing steels by APT, is the presence of molecular ions, in this case NbN. These molecular ions were divided into their elemental constituents for an accurate composition determination. The apparent thickness of the NbN GP zone in the 3D APT reconstruction, ~1nm, is significantly larger than one single atomic layer (0.14nm, for the {001} interplanar distance in ferrite). As the GP zones were unambiguously determined, by HREM and FIM, to be one monolayer thick, the apparent thickness in the APT reconstruction has to be interpreted in terms of an experimental artifact. As discussed with respect to the contrast observed by FIM, GP zones have a significantly higher evaporation field than the matrix. As a consequence, GP zones will be preferentially retained at a specimen’s surface, causing aberrations in the ion trajectories, and therefore biasing the 3D reconstructions. This reconstruction artifact may also affect local chemistry, as the trajectories of ions from the matrix may overlap with the trajectories of ions from


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