Transmission electron microscopy is a powerful imaging tool that has found broad application in materials science, nanoscience and biology1,2,3. With the introduction of aberration-corrected electron lenses, both the spatial resolution and the image quality in transmission electron microscopy have been significantly improved4,5 and resolution below 0.5 ångströms has been demonstrated6. To reveal the three-dimensional (3D) structure of thin samples, electron tomography is the method of choice7,8,9,10,11, with cubic-nanometre resolution currently achievable10,11. Discrete tomography has recently been used to generate a 3D atomic reconstruction of a silver nanoparticle two to three nanometres in diameter12, but this statistical method assumes prior knowledge of the particle’s lattice structure and requires that the atoms fit rigidly on that lattice. Here we report the experimental demonstration of a general electron tomography method that achieves atomic-scale resolution without initial assumptions about the sample structure. By combining a novel projection alignment and tomographic reconstruction method with scanning transmission electron microscopy, we have determined the 3D structure of an approximately ten-nanometre gold nanoparticle at 2.4-ångström resolution. Although we cannot definitively locate all of the atoms inside the nanoparticle, individual atoms are observed in some regions of the particle and several grains are identified in three dimensions. The 3D surface morphology and internal lattice structure revealed are consistent with a distorted icosahedral multiply twinned particle. We anticipate that this general method can be applied not only to determine the 3D structure of nanomaterials at atomic-scale resolution13,14,15, but also to improve the spatial resolution and image quality in other tomography fields7,9,16,17,18,19,20.
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Williams, D. B. & Carter, C. B. Transmission Electron Microscopy: A Textbook for Materials Science 2nd edn (Springer, 2009)
Spence, J. C. H. Experimental High-Resolution Electron Microscopy 3rd edn (Oxford Univ. Press, 2003)
Frank, J. Three-Dimensional Electron Microscopy of Macromolecular Assemblies (Oxford Univ. Press, 2006)
Batson, P. E., Dellby, N. & Krivanek, O. L. Sub-ångstrom resolution using aberration corrected electron optics. Nature 418, 617–620 (2002)
Haider, M. et al. Electron microscopy image enhanced. Nature 392, 768–769 (1998)
Erni, R., Rossell, M. D., Kisielowski, C. & Dahmen, U. Atomic-resolution imaging with a sub-50-pm electron probe. Phys. Rev. Lett. 102, 096101 (2009)
Frank, J. Electron Tomography (Plenum, 1992)
Midgley, P. A. & Weyland, M. 3D electron microscopy in the physical sciences: the development of Z-contrast and EFTEM tomography. Ultramicroscopy 96, 413–431 (2003)
Lučić, V., Förster, F. & Baumeister, W. Structural studies by electron tomography: from cells to molecules. Annu. Rev. Biochem. 74, 833–865 (2005)
Midgley, P. A. & Dunin-Borkowski, R. E. Electron tomography and holography in materials science. Nature Mater. 8, 271–280 (2009)
Arslan, I., Yates, T. J. V., Browning, N. D. & Midgley, P. A. Embedded nanostructures revealed in three dimensions. Science 309, 2195–2198 (2005)
Van Aert, S., Batenburg, K. J., Rossell, M. D., Erni, R. & Van Tendeloo, G. Three-dimensional atomic imaging of crystalline nanoparticles. Nature 470, 374–377 (2011)
Marks, L. D. Experimental studies of small particle structures. Rep. Prog. Phys. 57, 603–649 (1994)
Billinge, S. J. L. & Levin, I. The problem with determining atomic structure at the nanoscale. Science 316, 561–565 (2007)
Yacamán, M. J., Ascencio, J. A., Liu, H. B. & Gardea-Torresdey, J. Structure shape and stability of nanometric sized particles. J. Vac. Sci. Technol. B 19, 1091–1023 (2001)
Lee, E. et al. Radiation dose reduction and image enhancement in biological imaging through equally sloped tomography. J. Struct. Biol. 164, 221–227 (2008)
Kak, A. C. & Slaney, M. Principles of Computerized Tomographic Imaging (SIAM, Philadelphia, 2001)
Fahimian, B. P., Mao, Y., Cloetens, P. & Miao, J. Low dose X-ray phase-contrast and absorption CT using equally-sloped tomography. Phys. Med. Biol. 55, 5383–5400 (2010)
Mao, Y., Fahimian, B. P., Osher, S. J. & Miao, J. Development and optimization of regularized tomographic reconstruction algorithms utilizing equally-sloped tomography. IEEE Trans. Image Process. 19, 1259–1268 (2010)
Jiang, H. et al. Quantitative 3D imaging of whole, unstained cells by using X-ray diffraction microscopy. Proc. Natl Acad. Sci. USA 107, 11234–11239 (2010)
Bar Sadan, M. et al. Toward atomic-scale bright-field electron tomography for the study of fullerene-like nanostructures. Nano Lett. 8, 891–896 (2008)
Bovin, J.-O., Wallenberg, R. & Smith, D. J. Imaging of atomic clouds outside the surfaces of gold crystals by electron microscopy. Nature 317, 47–49 (1985)
Muller, D. A. Structure and bonding at the atomic scale by scanning transmission electron microscopy. Nature Mater. 8, 263–270 (2009)
Pennycook, S. J. & Nellist, P. D. Scanning Transmission Electron Microscopy: Imaging and Analysis 1st edn (Springer, 2011)
Miao, J., Föster, F. & Levi, O. Equally sloped tomography with oversampling reconstruction. Phys. Rev. B 72, 052103 (2005)
Kirkland, E. J. Advanced Computing in Electron Microscopy 2nd edn (Springer, 2010)
Howie, A. Diffraction channelling of fast electrons and positrons in crystals. Phil. Mag. 14, 223–237 (1966)
Daniel, M. C. & Astruc, D. Gold nanoparticles: assembly, supramolecular chemistry, quantum-size-related properties, and applications toward biology, catalysis, and nanotechnology. Chem. Rev. 104, 293–346 (2004)
Barnard, A. S., Young, N. P., Kirkland, A. I., van Huis, M. A. & Xu, H. Nanogold: a quantitative phase map. ACS Nano 3, 1431–1436 (2009)
Arslan, I., Marquis, E. A., Homer, M., Hekmaty, M. & Bartelt, N. C. Towards better 3-D reconstructions by combining electron tomography and atom-probe tomography. Ultramicroscopy 108, 1579–1585 (2008)
Averbuch, A., Coifman, R. R., Donoho, D. L., Israeli, M. & Shkolnisky, Y. A framework for discrete integral transformations I — the pseudopolar Fourier transform. SIAM J. Sci. Comput. 30, 785–803 (2008)
Saxton, W. O., Baumeister, W. & Hahn, M. Three-dimensional reconstruction of imperfect two-dimensional crystals. Ultramicroscopy 13, 57–70 (1984)
Bailey, D. H. & Swarztrauber, P. N. The fractional Fourier transform and applications. SIAM Rev. 33, 389–404 (1991)
Miao, J., Sayre, D. & Chapman, H. N. Phase retrieval from the magnitude of the Fourier transform of non-periodic objects. J. Opt. Soc. Am. A 15, 1662–1669 (1998)
Miao, J., Charalambous, P., Kirz, J. & Sayre, D. Extending the methodology of X-ray crystallography to allow imaging of micrometre-sized non-crystalline specimens. Nature 400, 342–344 (1999)
Miao, J., Ohsuna, T., Terasaki, O., Hodgson, K. O. & O’Keefe, M. A. Atomic resolution three-dimensional electron diffraction microscopy. Phys. Rev. Lett. 89, 155502 (2002)
Zuo, J. M., Vartanyants, I., Gao, M., Zhang, R. & Nagahara, L. A. Atomic resolution imaging of a carbon nanotube from diffraction intensities. Science 300, 1419–1421 (2003)
We thank E. J. Kirkland for help with multislice STEM calculations, R. F. Egerton, Z. H. Zhou and J. A. Rodríguez for discussions and I. Atanasov for assistance in data acquisition. The tomographic tilt series were acquired at the Electron Imaging Center for NanoMachines of the California NanoSystems Institute. This work was partially supported by UC Discovery/TomoSoft Technologies (IT107-10166).
The authors declare no competing financial interests.
This file contains Supplementary Methods, Supplementary Figures 1-13 and Supplementary Table 1. (PDF 2825 kb)
This movie shows a 3D volume rendering of the reconstructed gold nanoparticle. (MOV 4264 kb)
This movie shows a 3D iso-surface rendering of the reconstructed gold nanoparticle. (MOV 4321 kb)
This movie shows a 3D volume rendering of the four major grains determined from the reconstructed gold nanoparticle. (MOV 4279 kb)
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Scott, M., Chen, CC., Mecklenburg, M. et al. Electron tomography at 2.4-ångström resolution. Nature 483, 444–447 (2012). https://doi.org/10.1038/nature10934
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