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Acta Materialia 58 (2010) 162172 www.elsevier.com/locate/actamat

Strain mapping along AlPb interfaces

Harald Ro sner a,*, Christoph T. Koch b, Gerhard Wilde a
a

Westfa lische Wilhelms-Universita t Mu nster, Institut fu r Materialphysik, Wilhelm-Klemm-Strasse 10, D-48149 Mu nster, Germany b Max-Planck-Institut fu r Metallforschung, Heisenbergstr. 3, D-70569 Stuttgart, Germany Received 11 May 2009; received in revised form 28 August 2009; accepted 30 August 2009 Available online 28 September 2009

Abstract Local strains at particlematrix hetero-interfaces in an AlPb composite produced by high-energy ball-milling were measured by means of geometric phase analysis (GPA) on the basis of high-resolution transmission electron microscope (HRTEM) images. A through-focus series of 10 experimental micrographs was used to retrieve the complex exit-face wave function and subsequently to calculate the components of the strain tensor using Pb as the reference lattice. The strain analysis revealed considerable strain for the interface regions with compressive strain for the Pb side and tensile strain for the Al side. The strained zones extend up to 23 lattice spacings on either side of the interface. The interface regions are not sheared or signicantly rotated, which shows that the whole state of the interface is elastically strained but not plastically deformed. A new possible interpretation of the melting behaviour of the Pb particles in terms of the strains is discussed. 2009 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Keywords: Mist dislocation; Strain mapping; Size-dependent melting; Focus series reconstruction

1. Introduction Internal interfaces such as phase or grain boundaries are the joints of materials and can thus be regarded as weak elements of the microstructure limiting e.g. the mechanical properties of a given material. One of the key parameters in this regard is the stress located at these sites [1]. Our current knowledge of interface stresses originating from internal interfaces or boundaries in solids and their inuence on the materials properties is incomplete. Therefore, a better understanding of stresses and strains in metallic systems and semiconductor hetero-structures has become a major research topic in materials science with special emphasis on reduced dimensions in the case of applications of nano-materials. One such fundamental aspect, where interfaces play a dominant role, is the melting of conned systems. Binary monotectic AlPb, which has been used for more than twenty years now [2], is an adequate reference system for this purpose [35]. Former transmission electron
*

Corresponding author. E-mail address: rosner@uni-muenster.de (H. Ro sner).

microscopic (TEM) investigations revealed that the metal/ metal interfaces display an epitaxial orientation relationship (cube-on-cube) even though there is a large lattice mismatch of 22% between Al and Pb [25]. The accommodation of the lattice mist was initially puzzling due to fringes that veiled a direct observation of the interMoire face structure [6]. Dahmen and Johnson suggested a model [7] that explained the accommodation of this large mist in the absence of a visible localization into interfacial dislocations by a combination of lattice vacancies and Pb particles with so-called magic sizes for which the residual mist energy is minimized, i.e. for inclusion/matrix size ratios of about 4/5. Recently, mist dislocations were found by high-resolution transmission electron microscopy (HRTEM) of uncovered Pb inclusions [8,9]. This was also conrmed by high-resolution high-angle annular dark-eld scanning transmission electron microscopy (HAADFSTEM) imaging of Pb inclusions located in the thicker part of the TEM sample [10]. This present investigation uses geometric phase analysis (GPA) [11] to investigate the strain distribution along AlPb interfaces. Strain maps displaying the symmetric

1359-6454/$36.00 2009 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.actamat.2009.08.065

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strain tensor components [11,12] were generated using Pb as the reference lattice. The interface regions reveal considerable strain and exhibit strain gradients extending up to 2 3 lattice spacings on either side. This analysis gives new insight in the understanding of AlPb interfaces at which no elastic distortions have been observed so far. 2. Experimental The AlPb samples used in this study were produced by high-energy ball-milling as described in Ref. [13]. Thin electron-transparent foils of as-milled material were prepared by low-angle (4) ion-milling (beam energy 3.0 keV) using a PIPS (Gatan). TEM investigations were performed in an FEI Tecnai F20 G2 (eld-emission gun, super-twin lens, Cs = 1.2 mm) operated at 200 kV. Since the spherical aberration of the objective lens leads to delocalization of the information [14,15] through-focus series of typically 20 images were acquired. The individual high-resolution micrographs were aligned and stacked. A ux-preserving iterative computer algorithm for the reconstruction of focal series was used [16], in which the defocus Df, the spherical aberration coecient Cs, and the twofold astigmatism were corrected. In this study 10 images with defocus values ranging from 154 to 203 nm were taken as input to retrieve the complex-valued exit-face wave function. The AlPb was oriented along the [0 1 1] zone axis. For the acquisition of the micrographs a 1 k 1 k charged-coupled device camera (Gatan) was used. The method used here for measuring and mapping strain elds from HRTEM images is the GPA developed by Hy tch et al. [11]. Within the GPA method, any displacement in the Fourier-ltered local image pattern relative to a reference lattice image is interpreted in terms of a shift of atomic positions. The strain tensor can then be obtained from the local structural displacements by numerical dierentiation. A modied version which is based on the formalism in Ref. [11] but allowing the geometric phase to be extracted from the complex-valued exit-face wave function was implemented in Digital Micrograph (Version 1.71.38, Gatan) [17] to calculate the components of the symmetric strain tensor, e.g. exx, exy, eyy and the rigid-body rotation xxy [11,12], with Pb as the reference lattice. Circular masks with radii producing a lateral resolution of 1 nm in the geometric phase images were set around the [1, 1, 1] and [1, 0, 0] reections of the Pb lattice. Strain maps were calculated with respect to this reference lattice dened by g1 = [1, 1, 1]Pb and g2 = [1, 0, 0]Pb. A cosine function which produced a gradual transition of the mask value from 1 to 0 within the outer 20% of the mask radius was used for smoothing the edges of the circular masks. It should be noted that image distortions introduced by the projector lens [18] or the imaging lter (Gatan GIF 200) as well as delocalization due to coherent aberrations of the objective lens are negligible because the complex-valued exit wave function retrieved from focus series reconstruction was used [19].

3. Analyses and results In this study our attention is focused on local strains manifested at a PbAl particlematrix heterophase-interface. The TEM investigations were performed in [0 1 1] orientation. Thus the interfaces are parallel to the electron beam. The Fourier transform given as inset in Fig. 1a conrms an epitaxial orientation relationship (cube-on-cube) between the Al matrix and the Pb nanoparticle. patterns To exclude misinterpretations related to Moire or buried structures, uncovered Pb inclusions exhibiting hetero-structures with the Al matrix, as shown in Fig. 1a, were sought [8,9]. Fig. 1a shows an example of an image from the through-focus series (image No. 2). The defocus value of this micrograph was determined to be Df = 156 nm by analysing the zero-crossings in the contrast transfer function of this image. All other defocus values were rened by the reconstruction algorithm [16] resulting in a mean defocus step of 5.86 nm between successive images. Fig. 1a contains two distinct interfaces, a [1, 1, 1] as well as a [1 0 0], on two lateral sides of the Pb nanoparticle with the Al matrix. The aspect ratio of the two facets (1 1 1)/(1 0 0) is 1.08. Mist dislocations occurred statistically on every 5.5 Al plane (55 Al {1 1 1}-planes match 45 Pb {1 1 1}-planes including 10 mist dislocations), which accommodates exactly the nominal mist of 22.2%. This fact is of importance since it shows that, although most of the Al matrix was removed around the Pb particle, the original state, as for fully embedded nanoparticles [10], is maintained. Two representative Burgers circuits, drawn around a mist dislocation on each interface, exhibit closing failures 1 1 for the (1 0 0) interface and a40  21 1 for of the type a20 0  the (1, 1, 1) interface. The latter closing failure would correspond to a compact 60 a20 h1 1 0i dislocation forming hexagonal network [8,20,21]. The result of the focus series reconstruction was the retrieval of the complex-valued exit-face wave function which was further used for calculating the strain maps. The retrieved phase and amplitude are shown in Fig. 1b and c, respectively. The phase image (Fig. 1b) shows localized dislocation cores occurring periodically at the particle matrix interface. A simplied picture using Fourier ltering to enhance the dislocation cores is shown in Fig. 1d. The slight waviness of the interface, which appears to be more pronounced for the {1 0 0}-interface, is readily apparent by the lateral oset of the individual dislocation cores from each other. To point out the strained state of the particlematrix interface, bright features in the phase image have been associated with Al (blue) and Pb (red) atomic columns (Fig. 2a). Matching peak positions of HRTEM images or phase images with the positions of atomic columns is the basis of all currently used strain mapping algorithms operating in real space, such as the peak nding [2225] and peak pairs [26] algorithms (see Ref. [27] for a comparison of peak nding and GPA).

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Fig. 1. (a) High-resolution micrograph (No. 2 of the through-focus series) at a defocus value of 156 nm showing a particlematrix hetero-interface of Al Pb projected along the [0 1 1] zone axis. Two interfaces, a [1, 1, 1] as well as a [1 0 0] (top), remain on two lateral sides of the Pb nanoparticle, which is located at the very thin edge of the foil (note the amorphous nature of the other sides). The inset displays the Fourier transform revealing an epitaxial orientation relationship (cube-on-cube) between the two lattices. Representative Burgers circuits, drawn around a mist dislocation on each interface, 1 1 (top interface) and a40  21 1 (left interface). 10 such images of the through-focus series were used as input to exhibit closing failures of the type a20 0  retrieve the complex-valued exit-face wave function. (b) Phase image retrieved from the through-focus series using 10 images with defocus values ranging from 154 to 203 nm as input. (c) Amplitude image retrieved from the through-focus series using 10 images with defocus values ranging from 154 to 203 nm as input. (d) Filtered phase image showing the (1, 1, 1) lattice fringes only. The mist dislocations are clearly visible. Note the lateral oset of the individual dislocation cores from each other.

An unrelaxed model interface (Fig. 2b) was constructed using two rigidly coupled lattices reecting the mismatch of Al and Pb. At the intersection of the {1 0 0}/{1 1 1}-interface, a few Al columns had to be removed deliberately to make a more direct association with the experimental situation (Fig. 2a) possible. This led to the formation of an atomic step of 9 Al columns in length. The interpretation of the phase image in terms of atomic column species and position

is obviously not unique. However, the presented model appears to be the most likely interpretation of the data. This unrelaxed model (Fig. 2b) has been used to generate the reference strain maps shown in Figs. 3b6b, which should reect the state of faceted Pb inclusions embedded in Al neglecting any interaction between the two lattices. Strain maps were calculated, as described in the experimental section, for the experimental image as well as for

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Fig. 2. (a) Phase image superimposed with a possible atomic model consisting of Al (blue) as well as Pb (red) atom columns. The positions of the atomic columns have been adjusted to roughly match those of the local maxima in the phase image. (b) Model interface (unrelaxed) constructed by two rigidly coupled lattices reecting the mismatch of Al and Pb. Moreover, an unrelaxed atomic step was deliberately integrated around the intersection of the {1 1 1}/{1 0 0} interface. This model interface was used as a reference to compare to the experiment situation. Al columns are blue and Pb columns are red.

the model interface shown in Fig. 2b. The corresponding results, a juxtaposition of experimental (a) and model interface (b) in each case, are depicted in Figs. 36. Consequently, each strain map of an experimental image is directly comparable with the corresponding strain map of the model interface, and signicant dierences between

strained and unstrained states can be determined immediately. The strain analysis reveals considerable strain (green colour) around the interface regions extending up to 23 lattice spacings on either side. Compressive strain is found for the Pb side and tensile strain for the Al side. Strain

Fig. 3. (a) Experimental mean dilatation (trace of the strain tensor: exx + eyy) using Pb as the reference lattice. Strains ranging from 40% to + 40% are displayed. The Al matrix is displayed in blue colour, indicating a strain state of 22%. The Pb particle is depicted in a mixture of green/red, representing the zero strain level (reference lattice). A diuse greenish zone along the interface region is discerned, indicating considerable strains. Note the oset position of the individual dislocation cores at the interfaces and the curvature (bulging nature) of the mean dilatation between them marked by arrows. (b) Mean dilatation (trace of the strain tensor: exx + eyy) using the model interfaces shown in Fig. 2b. Strains from 40% to + 40% are displayed. Note that the step in the model (Fig. 2b) evokes considerable extra strain around the bend (indicated by the arrow), which is not observed in the experimental strain map shown in (a).

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peaks (hot spots) originating from the interfacial dislocation cores are observed, accommodating the mist of 22% between the two lattices. The general appearance of

the interfaces in terms of strains is rough and wavy, which manifests a non-equilibrium state of the particlematrix interface of ball-milled material. In the following a detailed

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strain analysis based on the strain maps of the individual strain tensor components is presented. Fig. 3 shows the mean dilatation (trace of the strain tensor: exx + eyy) which summarizes the two individual strain tensor components exx and eyy in one image. The factor 0.5 was used to display the matrix and particle on the same strain level; that is, 22% (blue colour) for the Al matrix and zero (reference lattice) for the Pb particle (mixture of red and green). First of all, the wavy nature of the experimental interface compared to the model (c.f. the green line in Fig. 3a and b) is striking. The step, which was deliberately incorporated in the model to create the best match to the experimental interface, appears clearly in the strain map of the model (c.f. arrow in Fig. 3b) as a bulge where the curvature is more extreme than between the other dislocation cores. Interestingly, this step is not observed in the experimental strain map (Fig. 3a). This means that this particular atomic step must be relaxed at the particlematrix hetero-interface. However, several other bulges are seen between the dislocation cores for the {1 1 1} as well for part of the {1 0 0}interface in the experimental strain map, indicating the local roughness of the interfaces. These are marked by white arrows on Fig. 3a. It is further noticed that the dislocation cores (hot spots) show a lateral oset from each other, supporting the rough and wavy character of the interface regions. A detailed strain analysis for the {1 1 1}-interface, which is representative of both types of interfaces, is presented in the following: the mist dislocation cores show a compressive part for the Al side and tensile strains for the Pb side (Fig. 4a). This situation reects the extra Al plane (5 Al planes meet 4 Pb planes). The intermediate region between the dislocation cores exhibits considerable strains along both sides of the interface appearing in a diuse green colour (Fig. 4a). Since GPA allows us to calculate the strain values for each pixel, a strain prole was measured across the {1 1 1}-interface along the length and averaged over the width of the box in Fig. 4a. A strain gradient is discerned extending up to 3 lattice spacings on both sides (Fig. 4c). Bearing in mind that the zero strain level is the equilibrium level for the Pb particle and 22% (blue colour) displays the equilibrium state of the Al matrix, compressive strain is identied for the Pb side of the interface region whereas the Al side is under tension. This nding is now compared with the model {1 1 1}-interface shown in Fig. 4b. The general appearance of the model interface region is much

smoother. Again, a strain prole was measured across the interface along the length and averaged over the width of the box in Fig. 4b. Here (Fig. 4d) the strain gradient extends over 0.7 nm in total only roughly half of the extent of the experimental gradient and is consistent with the mask sizes (radius 1 nm1 in reciprocal space) used to generate the strain maps. For this reason, the pronounced strain states of the experimental interface regions are ascertained. Similar results were found for the {1 0 0}-interface region which are not graphically represented. Fig. 5 compares the shear components of the strain tensor. Strain peaks are located along the particlematrix interface matching with the position of the mist dislocation cores. It is apparent that the dislocation cores are aligned in dierent ways, i.e. parallel at the {1 1 1}-interface and perpendicular at the {1 0 0}-interface. This reects the dierent character of the mist dislocations, namely 60 dislocations at the {1 1 1}-interface and pure edge dislocations at the {1 0 0}-interface. Compression strains are found on the Al side reecting the presence of the extra plane compared with the Pb side, which is under tension. The analysis shows that the shear strain originates from the dislocation cores, and that the interface regions in between the dislocation cores (hot spots) do not show appreciable shear strains. However, pre-located shear strain zones (indicated by black arrows on Fig. 5a) in the Al matrix near the {1 0 0}-interface are noticeable. Because of their distance from the interface, they are categorized as defects of the Al matrix having minor importance for the interface region itself. Moreover, it is noted that the deliberately incorporated step in the model interface at the intersection of the {1 1 1} and {1 0 0} interfaces (Fig. 2b) led to noticeable shear strains (Fig. 5b), which are not observed in the experimental case shown in Fig. 5a. The strain analysis is completed by looking at the rigidbody rotation maps presented in Fig. 6. Again, the dislocation cores are clearly observable as hot spots. They are all aligned parallel with the interfaces, some appearing slightly twisted and asymmetric compared to the model interface (Fig. 6b). Certain areas (indicated by white arrows) along the experimental interface in Fig. 6a appear slightly rotated (60.1). The accuracy of the rotation measurement is about 0.1 [12]. However, the articial step in the model (Fig. 6b) is not found in the experimental interface (Fig. 6a). Again, pre-located zones (indicated by black arrows) in the Al matrix near the [1 0 0] interface are noticeable but extraneous to the interface region.

3
Fig. 4. (a) Enlarged view of the strain map (mean dilatation) of the experimental {1 1 1}-interface region shown in Fig. 3a, revealing details of: (i) the strained state (diuse green colour) and, (ii) the dislocation cores (four hot spots). The colour legend is the same as shown in Fig. 3a. (b) Enlarged view of the strain map of the model {1 1 1}-interface region shown in Fig. 3b. (c) The strain prole was measured across the interface along the length and averaged over the width of the box shown in (a). A strain gradient is seen across the interface region starting from the Al matrix (equilibrium strain level is 22%) into the Pb particle (reference strain level is zero) revealing compressive strain for the Pb side whereas the Al matrix shows tensile strain. The total length of the gradient is 1.5 nm. (d) The strain prole was measured across the model interface along the length and averaged over the width of the box shown in (b). A strain gradient is obtained across the interface region starting from the Al matrix (equilibrium strain level of 22%) into the Pb particle (reference strain level of 0%). Again, compressive strain is found for the Pb side whereas the Al matrix shows tensile strain. Note the dierence in length: here the gradient extends about 0.7 nm whereas in the experimental case it extended about 1.5 nm.

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Fig. 5. (a) Experimental shear component exy using Pb as the reference lattice. Shear strains on a scale from 40% to +40% are displayed. Pre-located shear strain zones (indicated by black arrows) in the Al matrix near the [1 0 0]-interface are noticeable. (b) Shear component exy using the model interfaces shown in Fig. 2b. Strains on a scale from 40% to +40% are displayed. Note the increased shear strain at the intersection of the {1 1 1} and {1 0 0} interfaces originating from the deliberately incorporated step in the model interface (Fig. 2b), which is not observed in the experimental case shown in (a).

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Fig. 6. (a) Experimental rigid-body rotation xxy using Pb as the reference lattice. Rotations ranging from 0.4 to +0.4 (anticlockwise positive) are displayed. Certain areas (indicated by white arrows) along the interfaces appear slightly rotated (6 0.1). (b) Rigid-body rotation xxy using the model interfaces shown in Fig. 2b. Rotations from 0.4 to +0.4 are displayed.

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4. Discussion The detailed strain analysis presented in the last section unambiguously shows considerable strain for the interface regions of PbAl particlematrix hetero-structures with compressive strain for the Pb side and tensile strain for the Al side. The strained zones extend up to 23 lattice spacings on either side of the interface. The interface regions are not sheared or signicantly rotated, which leads to the conclusion that the whole state of the particlematrix interface is elastically strained but not plastically deformed. Thus, based on the comprehensive strain analysis presented here, a new interpretation is derived for particlematrix hetero-interfaces of ball-milled AlPb composites. Below, the strain analysis is critically discussed with respect to its robustness and with respect to the melting behaviour of nanometre-sized Pb inclusions embedded in the Al matrix. 4.1. Robustness The robustness of GPA itself has been demonstrated previously in several case studies by comparison with other strain mapping algorithms [2227] and theoretical considerations [28]. The fact that the complex-valued exit-face wave function retrieved from focus series reconstruction is used here excludes further errors due to image distortions introduced by the projector lens system [19]. Especially, delocalization due to coherent aberrations of the objective lens is minimized [14,15]. However, in order to evaluate correctly the newly derived situation at the interface regions in terms of strains, each experimental strain map was compared with a model interface constructed by two rigidly coupled lattices reecting the mismatch of Al and Pb accurately. Moreover, an unrelaxed atomic step was deliberately integrated around the intersection of the {1 1 1}/{1 0 0} interface. This articially created step was clearly discerned as a bulge in the strain map of the model interface (Fig. 3b). However, bulges were found in the experimental maps at positions where the model did not show any (Fig. 3a). The observation of signicant bulging, i.e. the deviation of the strain eld from planar geometry resembling an edge-on interface indicates that the model based on two unrelaxed lattices meeting at a planar interface is too simplied to resemble the experimental conguration. Thus, the current result indicates that the topology of the real interface between Pb and Al entails corrugations along the direction of the incident electron beam, i.e. mixed atomic columns. The fact that the features produced by the step in the articial interface are not found in the strain maps of the real particle indicates that in-plane defects, such as steps, do not occur on the interface of the experimentally analysed particle. However, the step in the model can be used as a quantitative measure to achieve a proper evaluation of the particlematrix hetero-interface in terms of strain. In addition, the strain prole across the model interface reveals an interface width of 0.7 nm in total, which is mainly determined by the radius of the

mask used in the reciprocal space to generate the geometric phase maps. However, this value would also t with the structural and diusional width of grain boundaries/interfaces of about 2 * a0 % 0.50.8 nm (a0: lattice parameter) [2932]. 4.2. Rough and wavy interfaces The experimental situation of the interface region is depicted in Fig. 3a and in more detail in Fig. 4a, where bulges and dimples are found. It is noted that the {1 1 1}-interface appears to be atter (general curvature of the whole interface) than the {1 0 0}-particlematrix interface. The signicance of this observation is unclear due to the fact that only one interface of each kind was analysed so that any statistical basis is missing. However, based on the specic excess free energy densities of the two interfaces, a atter {1 0 0}-particlematrix interface would be expected since the excess interface free energy density of that interface is higher. Intrinsically, such diuse interfaces need to be involved in any transient state that develops via atomic motion towards a more stable conguration based on faceted interfaces. The lifetime of such transient states depends on temperature and might be extended in time. The observation of partial faceting after annealing severely deformed AlPb composites indicates that such microstructures are certainly transient in nature [13,33]. However, whether the atomic Al and Pb columns are still separated or if atomic mixing is involved here cannot be determined on the basis of the strain mapping as presented in this study. 4.3. Observation of compressive strain at the interface regions of the Pb particle The detailed strain analysis presented in the preceding paragraphs has clearly shown that the interface regions of PbAl particlematrix hetero-structures are elastically distorted with compressive strains for the Pb and tensile strains for the Al side. Thus a pressure or strain relief at the interface accommodated by vacancies or creep cavitation has to be excluded [3436]. However, an earlier onset in melting of {1 0 0} interfaces [37] cannot be explained in terms of the strains observed, since the strain state was found to be similar for both types of interfaces, i.e. {1 0 0} and {1 1 1}. Moreover, the interface regions are not sheared or signicantly rotated, which leads to the conclusion that the whole state of the particlematrix interface is elastically strained but not plastically deformed. Thus, this nding actually shows the validity of early two-phase models that describe nanostructured materials in terms of a core/shell approach [38]. In addition, this observation stresses the importance of the interface contributions with respect to property tuning of nanostructured materials since bulk material could not support such large deviations from equilibrium without rapid relaxation via the generation of localized and highly mobile defects.

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4.4. Link to the melting behaviour of matrix-encased nanoparticles To link the microstructural observation together with the strain analysis to the melting behaviour of this individual Pb particle is both desirable and tempting but it has to remain speculative since the direct melting was not monitored. However, a couple of statements can be made and are discussed below. First of all, to judge the situation of the analysed Pb particle embedded in an Al matrix correctly, it should be emphasized that the AlPb composite used for this study was produced by high-energy ball-milling [13]. The melting behaviour of Pb particles in such a material is usually characterized by a melting point depression to temperatures below the melting point of bulk Pb [3,13,39]. The morphology of the embedded Pb inclusions was recently determined by electron tomography [40] and two dierent species were found. The majority of particles had curved spherical shapes with some degree of faceting in their outline. About 4% of Pb particles were cuboctahedrally shaped, displaying clear {1 0 0} and {1 1 1}-facets and the Pb particle investigated in this study belongs to this latter (minor) species. However, it has been previously shown for such composites that annealing led to faceting of the Pb particles which subsequently showed an increased melting temperature, Tm, above the melting point of bulk Pb [13]. Thus, it is reasonable to expect that the Pb particle analysed here would show a certain increase of the melting point (up to 13 K after [13]). Such increase of Tm can be described by the CouchmanJesser equation [41]:   3clm csm 1 Tm T0 1 rL Tm is the melting point of the embedded particle and T0 is the bulk melting point. clm and csm are the liquid/matrix and solid/particle interfacial energies, L is the latent heat and r the particle radius. Pressure eects or strains due to dierential thermal expansion of the matrix and the embedded phase are not included in this expression. However, the strain analysis of the Pb particle presented here unambiguously reveals considerable strain at the interface which has to be taken into account. An adequate way to describe the melting behaviour (rst-order transition) considering strain/pressure is given by the Clapeyron equation: DV Dp DT M DS 2

superheating) [39] since the mist is accommodated in the same manner for both species of Pb particles [6,8], i.e. spherical or faceted. However, it has been reported that steps/ledges at particlematrix interfaces lead to melting point depression [42]. Thus, two facts could account for an increase of the melting point, namely the faceted shape or the compressive strain according to the Clapeyron Eq. (2), whereas the occurrence of steps could account for a decrease. Currently, it cannot be said how these three contributions add up. More experimental facts in terms of strain mapping of curved particle matrix interfaces as well as a direct observation of the melting of such excavated Pb particles have to be awaited before any further conclusions can be arrived at. 5. Summary The comprehensive strain analysis presented in this study provides new insight into particlematrix heterointerfaces of AlPb composites at which no elastic distortions have been observed before. We found considerable strain for the interface regions with compressive strain for the Pb side and tensile strain for the Al side. The strained zones extend up to 23 lattice spacings on either side of the interface. The interface regions are not sheared or signicantly rotated, which leads to the conclusion that the whole state of the particlematrix interface is elastically strained but not plastically deformed. Since the outer regions of the Pb particle are under compressive strain of large magnitude, a higher melting temperature is expected according to the Clapeyron equation, whereas the occurrence of steps at the interface could account for a decrease. However, further experimental facts are needed before the consequences of the strain analysis can directly be linked to the melting behaviour of matrix-encased Pb particles. Acknowledgment CTK acknowledges nancial support by the European Commission under contract No. NMP3-CT-2005-013862 (INCEMS). References
[1] Birringer R, Zimmer P. Acta Mater 2009;57:1703. [2] Moore KI, Chattopadhyay K, Cantor B. Proc Roy Soc Lond 1987;A414:499. [3] Chattopadhyay K, Goswami R. Prog Mater Sci 1997;42:287. [4] Johnson E, Andersen HH, Dahmen U. Microsc Res Tech 2004;64:356. [5] Mei QS, Lu K. Prog Mater Sci 2007;52:1175. [6] Ro sner H, Weissmu ller J, Wilde G. Philos Mag Lett 2004;84:673. [7] Dahmen U, Xiao SQ, Paciornik S, Johnson E, Johansen A. Phys Rev Lett 1997;78:471. [8] Ro sner H, Weissmu ller J, Wilde G. Philos Mag Lett 2006;86:623. [9] Ro sner H, Freitag B, Wilde G. Philos Mag Lett 2007;87:341. [10] Ro sner H, Lopatin S, Freitag B, Wilde G. In: Richter A, Schwedt A, editors. Proceedings of the 14th european microscopy congress, vol. 2. Aachen Germany: Springer; 2008. p. 359. [11] Hy tch MJ, Snoeck E, Kilaas R. Ultramicroscopy 1998;74:131.

DV, DS, Dp, DT are the changes in volume, entropy, pressure and melting temperature, respectively. Therefore any increase in pressure would shift the melting point to higher temperatures. Since the outer regions of the Pb particle are under compressive strain (negative) of large magnitude, a higher melting temperature is expected according to Eq. (2). The strain peaks (hot spots) in the strain maps originating from the mist dislocation cores at the interfaces do not have an inuence on the melting behaviour (depression or

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