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J. Fornell et al. / Scripta Materialia 62 (2010) 13–16 15Figure 2. Depen<strong>de</strong>nce of hardness on the nanoin<strong>de</strong>ntation maximumload for (a) several pieces of the as-cast sample and (b) several pieces ofthe compressed specimen. The inset in (a) is a scanning electronmicroscopy image of an in<strong>de</strong>ntation performed on the as-cast specimenusing a maximum load of 500 mN.matrix. The second ring in the SAED pattern, markedwith an arrow (inset Fig. 1b), indicates the formationof a crystalline phase that may be the tetragonal Zr 2 Ni(space group I4/mcm, a = 0.649 nm and c = 0.527 nm).Therefore, our results indicate that <strong>de</strong>formation promotesnanocrystallization. It should be noted that Denget al. [27] also presented a direct high-resolution TEMobservation of nanocrystallization in a Zr–Al–Ni–CuBMG fractured by compression test. They suggestedthat, due to the concentration of p<strong>la</strong>stic flow, the loca<strong>la</strong>tomic neighbor distance increases producing nanocrystallizationin the amorphous structure. Other authorshave obtained evi<strong>de</strong>nce for nanocrystallization in shearbands [28,29]. The temperature increase associated with<strong>de</strong>formation is c<strong>la</strong>imed to p<strong>la</strong>y a role in the formation ofnanocrystals.In or<strong>de</strong>r to better un<strong>de</strong>rstand the <strong>de</strong>formation behaviorin this metallic g<strong>la</strong>ss, nanoin<strong>de</strong>ntation tests were performedat different maximum loads (P max ), both in theas-cast and the compressed specimen. Generally, in bulkmetallic g<strong>la</strong>sses, hardness is expected to <strong>de</strong>crease whenthe in<strong>de</strong>ntation <strong>de</strong>pth increases. This effect is usuallyreferred to as the in<strong>de</strong>ntation size effect [30–35] and isattributed to the softening caused by <strong>de</strong>formation-inducedcreation of free volume. In the present study (Fig. 2), hardnessof the as-cast alloy is found to <strong>de</strong>crease for P max <strong>la</strong>rgerthan 100 mN. However, it is interesting to remark that anincrease of hardness is observed when in<strong>de</strong>ntations wereperformed at lower loads (see Fig. 2a).To elucidate the physical origin of this mechanicalhar<strong>de</strong>ning, TEM specimens from the as-cast alloy, containingan array of nanoin<strong>de</strong>nts, were prepared. Figure3a is an SEM image showing a hole (created during ionmilling of the TEM sample preparation) surroun<strong>de</strong>d byFigure 3. Microstructural features in the samples in<strong>de</strong>nted at amaximum force of 100 mN (a–d) and at 10 mN (e and f). (a) SEMimage disp<strong>la</strong>ying an array of in<strong>de</strong>ntations (indicated by circles)separated by 20 lm from each other and prepared for subsequentTEM observation. The inset is a TEM bright-field image of anin<strong>de</strong>ntation which was perforated during ion milling. (b) An en<strong>la</strong>rgementcorresponding to the square drawn in the inset in (a), indicatingthe presence of nanosized crystals embed<strong>de</strong>d in an amorphous matrix.The corresponding SAED pattern confirms the presence of thecrystalline phase. (c) TEM image performed in a region located at1 lm from the edge of the hole indicated in panel (a) and en<strong>la</strong>rged inpanel (b); (d) corresponds to a region located at 10 lm from the samein<strong>de</strong>nt. (e) An en<strong>la</strong>rgement of a 10 mN in<strong>de</strong>ntation (disp<strong>la</strong>yed in thebottom right corner) revealing the presence of a high amount ofnanocrystals insi<strong>de</strong> the in<strong>de</strong>nt. (f) TEM dark-field image obtained onthe diffraction ring marked on the inset SAED pattern confirming theexistence of nanocrystallites in the amorphous matrix.an array of P max = 100 mN in<strong>de</strong>ntations separated by20 lm from each other. The inset of Figure 3a is a smallhole corresponding to one of the in<strong>de</strong>nts. Figure 3b, whichis an en<strong>la</strong>rgement of the square indicated in the inset ofFigure 3a, reveals the existence of nanocrystals with anaverage size below 7 nm near the in<strong>de</strong>nt. The correspondingSAED pattern confirms the presence of a crystallinephase. The amount of nanocrystals <strong>de</strong>creases as the distancefrom the in<strong>de</strong>nt is increased (see Fig. 3c) and nonanocrystals could be observed by TEM at 10 lm fromthe in<strong>de</strong>nt (Fig. 3d). This confirms that nanocrystallizationis in<strong>de</strong>ed induced during nanoin<strong>de</strong>ntation.The same preparation procedure was used to observenanoin<strong>de</strong>nts performed at a maximum load of 10 mN.In this case, the observed nanoin<strong>de</strong>nt (inset Fig. 3e), whichwas not perforated during the thinning process, againcontained several nanocrystals. Nanocrystallization isalso evi<strong>de</strong>nced in Figure 3f, which is a dark-field TEM imagefrom the diffraction spot highlighted in the inset, correspondingto an interp<strong>la</strong>nar distance of d = 0.204 ±