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Electron diffractive imaging of oxygen atoms in nanocrystals at sub-ångström resolution

Nature Nanotechnology volume 5, pages 360–365 (2010)Cite this article

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Abstract

High-resolution imaging of low-atomic-number chemical elements using electron microscopy is challenging and may require the use of high doses of electrons. Electron diffractive imaging, which creates real-space images using diffraction intensities and phase retrieval methods, could overcome such issues, although it is also subject to limitations. Here, we show that a combination of electron diffractive imaging and high-resolution transmission electron microscopy can image individual TiO2 nanocrystals with a resolution of 70 pm while exposing the specimen to a low dose of electrons. Our approach, which does not require spherical and chromatic aberration correction, can reveal the location of light atoms (oxygen) in the crystal lattice. We find that the unit cell in nanoscale TiO2 is subtly different to that in the corresponding bulk.

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Figure 1: TEM analysis of an ‘anatase-like’ TiO2 rod-shaped nanocrystal along its 〈1, 0, 0〉 zone axis.
Figure 2: Phase-retrieved diffractive image of a distorted ‘anatase-like’ TiO2 nanocrystal lattice along the 〈1, 0, 0〉 direction.
Figure 3: Effect of finite resolution and thermal displacements on the visibility of oxygen spots in the projected electron potential of the distorted ‘anatase-like’ structure in the 〈100〉 orientation.

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Authors and Affiliations

  1. Istituto di Cristallografia (IC-CNR) via Amendola 122/O, Bari, 70126, Italy

    Liberato De Caro & Cinzia Giannini

  2. IOM CNR Laboratorio TASC, Area Science Park—Basovizza, Building MM SS 14, Km 163.5, Trieste, 34149, Italy

    Elvio Carlino

  3. Scuola Superiore ISUFI, Università del Salento, Distretto Tecnologico, Via per Arnesano Km 5, Lecce, 73100, Italy

    Gianvito Caputo & Pantaleo Davide Cozzoli

  4. National Nanotechnology Laboratory (NNL) of CNR-INFM, Unità di Ricerca IIT, Via per Arnesano Km 5, Lecce, 73100, Italy

    Gianvito Caputo & Pantaleo Davide Cozzoli

Authors
  1. Liberato De Caro
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  2. Elvio Carlino
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  3. Gianvito Caputo
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  4. Pantaleo Davide Cozzoli
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  5. Cinzia Giannini
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Contributions

L.D.C. and C.G. conceived the EDI methodology, which was further developed in collaboration with E.C., who performed HRTEM and n-ED experiments. C.G. performed the X-ray diffraction experiments and L.D.C. developed and applied the algorithm for the phase-retrieval processing. P.D.C. conceived and supervised development of colloidal TiO2 synthesis. G.C. synthesized the TiO2 nanocrystals. L.D.C. wrote the paper in close collaboration with C.G., E.C. and P.D.C. The results were discussed by all the authors.

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Correspondence to Cinzia Giannini.

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The authors declare no competing financial interests.

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De Caro, L., Carlino, E., Caputo, G. et al. Electron diffractive imaging of oxygen atoms in nanocrystals at sub-ångström resolution. Nature Nanotech 5, 360–365 (2010). https://doi.org/10.1038/nnano.2010.55

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