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Etude par Sonde Atomique Tomographique de la formation de nano ...

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tel-00751814, version 1 - 14 Nov 2012<br />

Chapter 1.Bibliography<br />

An example is the work of Okuda et al. [94] who studied the change of behaviour of a<br />

Fe-13Cr alloy during mechanical alloying (with 3wt.% of Y2O3) and subsequent annealing<br />

treatments. Another example can be the study of Alinger et al. [56] on Fe-14Cr ODS steels.<br />

He confirmed that Y2O3 dissolution in Fe-14Cr alloy matrix is the dominating process during<br />

MA, resulting in a highly supersaturated solid solutions.<br />

Studies by Larson [49], Miller [51] and Yamashita [95] are also in this direction.<br />

However, it should be mentioned that in their works, APT investigations of ODS material are<br />

performed only in the final state, passing over investigation of material immediately after MA<br />

step. Their conclusions are mainly based on size differences of <strong>nano</strong> clusters in final state and<br />

the initial size of Y2O3 pow<strong>de</strong>r (~2 nm for <strong>nano</strong>clusters in as-received state and 17-31 nm for<br />

initial Y2O3 pow<strong>de</strong>r [51]) introduced during MA process. Another argument is that, the<br />

chemical composition of <strong>nano</strong>clusters estimated by APT, is more consistent with TiO than<br />

Y2O3 stoichiometry.<br />

However, some other groups of researchers show that the <strong>formation</strong> mechanism of these<br />

<strong>nano</strong>-oxi<strong>de</strong>s is not limited to dissolution/precipitation mechanisms as reported above. Among<br />

them, recent work by Brocq [96,97] on Fe-14Cr-2W-0.25Ti ODS showed that the role of<br />

mechanical alloying appears to be more complex. It could be summarised as follow:<br />

i) Dissolution of primary oxi<strong>de</strong> and nucleation of first <strong>nano</strong>clusters can occur<br />

simultaneously during ball-milling;<br />

ii) Nucleation and growth of <strong>nano</strong>clusters continue after subsequent annealing.<br />

The <strong>nano</strong>-oxi<strong>de</strong>s formed this way can be controlled through variation of ball-milling<br />

<strong>par</strong>ameters (intensity, temperature and atmosphere) and annealing <strong>par</strong>ameters (duration and<br />

temperature). However it should be mentioned that specific conditions of ball milling<br />

(reactive ball milling: YFe3 and Fe2O3 are used as reactants) are used for this study.<br />

Nevertheless, the possibility that <strong>nano</strong>clusters in conventional ODS can originate from the<br />

same mechanism are not exclu<strong>de</strong>d.<br />

An alternative <strong>formation</strong> mechanism of <strong>nano</strong>-oxi<strong>de</strong>s is suggested by Hsiung et al<br />

[43,92,93]. HRTEM investigations of Fe-16Cr-4Al-2W-0.3Ti ODS (<strong>de</strong>signated as K3) in its<br />

final state, revealed some Y2Al2O9 crystallite (in the core) surroun<strong>de</strong>d by an amorphous shell.<br />

Based on this observation, the author suggests that the <strong>formation</strong> mechanism of <strong>nano</strong><strong>par</strong>ticles<br />

may inclu<strong>de</strong> three stages (Figure 1.13.):<br />

24

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