Simultaneous visualization of oxygen vacancies and the accompanying cation shifts in a perovskite oxide by combining annular imaging techniques

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1 Simultaneous visualization of oxygen vacancies and the accompanying cation shifts in a perovskite oxide by combining annular imaging techniques Shunsuke Kobayashi 1, Scott D. Findlay 2, Naoya Shibata 3, Teruyasu Mizoguchi 4, Yukio Sato 3, Eiji Okunishi 5, Yuichi Ikuhara 3, 6 1, 6, 7, a) and Takahisa Yamamoto 1 Department of Advanced Materials Science, University of Tokyo, Kashiwa, , Japan 2 School of Physics, Monash University, Victoria 3800, Australia 3 Institute of Engineering Innovation, University of Tokyo, Tokyo, , Japan 4 Institute of Industrial Science, University of Tokyo, Tokyo, , Japan 5 Electron Optics Division, JEOL Ltd., Tokyo, , Japan 6 Nanostructures Research Laboratory, Japan Fine Ceramics Center, Atsuta, Nagoya , Japan 7 Department of Quantum Engineering, Nagoya University, Chikusa, Nagoya , Japan a)yamataka@k.u-tokyo.ac.jp 1. Methods Polycrystalline SrMnO 2.6 was prepared by solid-state sintering. At first, hexagonal SrMnO 3 powder was prepared by a conventional solid-state reaction method. The powder mixtures with appropriate molar quantities of SrCO 3 and Mn(NO 3 ) 2 6H 2 O were calcined at 1573 K for 5 h in air. The pellets made of the calcined powder were confirmed to have hexagonal SrMnO 3 structure by X-ray diffractometry. SrMnO 2.6 was then obtained by heating these pellets at 1773 K for 12 h in air and quenching them in oil. This sample was observed with crushed polycrystalline particles supported on holey carbon films by an aberration corrected STEM (ARM-200F, JEOL Ltd.) with a cold-type field emission gun operated at 200 kv and a probe-forming aperture semiangle of 22 mrad. The HAADF and ABF images were simultaneously recorded with mrad and mrad detectors, respectively. Image simulations were carried out assuming an aberration-free probe and accounting for a finite effective source size characterized by a Gaussian with a half-width at half-maximum of 0.04 nm. The Debye-Waller factors previously reported for SrMnO 2.6 were used for the image simulations. 1

2 2. Extracting respective information from spectral frequencies Figure S1(a) and (b) show the two dimensional Fourier transforms of a region of the HAADF and ABF images from SrMnO 2.6. The spectral frequencies indicated by the blue circles in Fig. S1(a), which are the group of 100 and 110 spectral frequencies, and the red circles in Fig. S1(b), which are the group of 110 spectral frequencies, encode the periodic structure of the cation shifts around O vacancies and the O vacancies, respectively. The images of Fig. 3(b) and d are synthesized via inverse Fourier transform applied only to the extracted spots indicated in Fig. S1(a) and (b). FIG. S1. Two dimensional Fourier transforms of a region of the (a) HAADF and (b) ABF images of SrMnO 2.6. The spectral frequencies indicated by the blue circles in (a) and the red circles in (b) originate from the periodic structure of cation shifts around O vacancies and the O vacancies, respectively. 2

3 3. Interpretation of the images extracted from the Fourier analysis Although obtained by inverse Fourier transform applied only to the indicated spots of Fig. S1(a) and (b), we claim that Fig. 3(b) and (d) are nearly equal to the difference of intensities between the STEM images of SrMnO 2.6 and the fundamental perovskite ABO 3. We confirm this via simulation as follows. STEM images were simulated for both SrMnO 2.6 and tetragonal-srmno 3. For the tetragonal-srmno 3 structure, Debye-Waller factors were estimated from the average of the Debye-Waller factors for the same species of atom for the SrMnO 2.6 structure. The simulated HAADF images of SrMnO 2.6 and tetragonal-srmno 3 are shown in Fig. S2(a) and (b), respectively, with their difference shown in (c). The simulated ABF images of SrMnO 2.6 and tetragonal-srmno 3 are shown in Fig. S2(d) and (e), respectively, with their difference shown in (f). Bright contrast in the difference image thus indicates more intensity in the SrMnO 2.6 image than in the tetragonal-srmno 3 image. Dark contrast shows the reverse. Thus, the bright intensity peaks in the subtracted images indicate the direction of the cation shifts, most clearly in Fig. S2(c) but also in (f), and, very clearly in (f), the position of the O vacancy. A composite image comprising the HAADF image ((a): gray color) and the subtracted images ((c): blue color and (f): red color) is shown in Fig. S2(g). This composite image is very similar to Fig. 4(b), supporting our assertion about the approximate equivalence between the image difference concept and the images synthesized by the Fourier analysis. However, the ABF subtracted image in (f) is different from the extracted image (Fig. 3(d), an enlarged section of which is reproduced in Fig. S3(a)). This is because the images in Fig. S3(a) is extracted from a group of 110 spectral frequencies only, meaning that the extracted image mainly has a information of the periodic structure of O vacancies and only a slight contribution from the cation shifts. Figure S3(b) shows the image synthesized by inverse Fourier transforming both the 100 and 110 spectral frequencies for the ABF image. This image should now contain information on both the periodic structure of O vacancies and on the cation shifts around them. Figure S3(b) is indeed seen to be very similar to the subtraction image of Fig. S2(f), validating the approach used and the interpretation as a difference in the intensity of the appropriate STEM image between the SrMnO 2.6 and the fundamental perovskite SrMnO 3 structures. 3

4 FIG. S2. (a) HAADF and (d) ABF images are the simulated images of SrMnO 2.6. (b) HAADF and (e) ABF images are the simulated images of tetragonal-srmno 3. (c) The difference between images (a) and (b). (f) The difference between images (d) and (e). (g) A composite image comprising the HAADF image ((a): Gray color) and the subtracted images ((c): blue color and (f): red color). FIG. S3. (a) The magnified image around an O vacancy site in Fig. 3D. (b) An image synthesized by inverse Fourier transform applied only to the group of 100 and 110 spectral frequencies in the Fourier transform of the ABF experimental image of SrMnO

5 4. The line profiles of cation shifts The line profiles from the experimental and simulated images around O vacancies are shown in Fig. S4(a)-(d). The intensity profiles from the experimental HAADF and ABF images are a sum of 50 line scans taken from the raw images. We do not have a pristine experimental reference, i.e. of tetragonal-srmno 3, for the same thickness and imaging conditions, but we can synthesize one by again Fourier filtering the HAADF and ABF images, now selecting only those peaks consistent with the fundamental perovskite ABO 3 unit. This gives pseudo-experimental images with the structure/symmetry of the red dashed circles in Fig. 3(h), which can be used as a reference for measuring the cation shifts present in the true experimental data. The HAADF and ABF intensity profiles clearly show the cation atomic positions around O vacancies are shifted from tetragonal-srmno 3. The line profiles taken from the simulated ABF images, despite showing some variation with thickness due to coherent interference in the contributing electron distribution, indicate that O vacancies can be observed over a wide range of thicknesses. FIG. S4 (a)-(d) The line profiles from the experimental and simulated HAADF and ABF images. The line profiles obtained from the experimental images are a sum of 50 line scans. The intensity of the ABF profiles is shown inversely. Simulated profiles are shown for specimen thicknesses of 5, 10, 20 and 40 nm. 5

6 5. The observation results around the interface The interface of the different phases, both of which are of SrMnO 2.6 but which consist of viewing it along the distinct [001] and [120] zone axes, are shown in Fig. S5 as (a) the HAADF image, (b) the ABF image, and (c) the composite image. The existence of a different phases and the interface location is hardly discernable from the HAADF and ABF images, but is clearly seen in the composited image of the present visualization technique. Moreover, the contrast in the composite image suggests the transition between the different phases is gradual. This is not an artifact of the Fourier analysis: the gradual change is confirmed by line profiles taken from the transition region. Figure S5(d) shows a projected line scan taken from an average over five areas of very similar contrast within the transition region. By contrast to Fig. S4(d), the nominal O vacancy site in Fig. S5(d) does not show the intensity reduction due to a full vacancy column, but nor does it show the peak expected of a fully occupied O column, evidence of a gradual transition in structure between these extremes. Thus, the present visualization technique can be applied to identifying various distributions of defect structure in materials. FIG. S5 (a) HAADF, (b) ABF and (c) composited images show around the interface of two phases, which are viewed along the [001] and [120] zone axes as shown in Fig. 4. Inversion contrast of ABF image is attached in (b). A radial Wiener filter was applied to the images for noise reduction. (d) The line profiles obtained from a region of weak O vacancy contrast of the ABF images. A composited image corresponding to the line profile is inserted in (d). The line profile is a sum of 5 line scans around interface and the intensity of the ABF profiles is shown inversely. The dotted lines in (d) show the difference intensities of the position of O columns and O vacancies. 6

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