Abstract

Conventional three-dimensional (3D) structure determination methods require either multiple measurements at different sample orientations or a collection of serial sections through a sample. Here we report the experimental demonstration of single-shot 3D structure determination of an object; in this case, individual gold nanocrystals at ~5.5 nm resolution using ~10 fs X-ray free-electron laser pulses. Coherent diffraction patterns are collected from high-index-faceted nanocrystals, each struck by an X-ray free-electron laser pulse. Taking advantage of the symmetry of the nanocrystal and the curvature of the Ewald sphere, we reconstruct the 3D structure of each nanocrystal from a single-shot diffraction pattern. By averaging a sufficient number of identical nanocrystals, this method may be used to determine the 3D structure of nanocrystals at atomic resolution. As symmetry exists in many virus particles, this method may also be applied to 3D structure studies of such particles at nanometer resolution on femtosecond time scales.

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Acknowledgements

We thank Haibing Xia for providing monodisperse trisoctahedral gold nanocrystals used for this study, Margaret M. Murnane, Z. Hong Zhou and Xing Zhang for stimulating discussions. This work was supported by the DARPA PULSE program through a grant from AMRDEC and the Institute of Physical and Chemical Research (RIKEN) of Japan. The experiments were performed at SACLA with the approval of JASRI and the programme review committee (No. 2012A8027). H.J. acknowledges the support by the National Natural Science Foundation of China (No.21390414) and J.A.R. is supported by a Giannini Foundation postdoctoral fellowship. M.G.-J. is supported by the RIKEN-Liverpool partnership award shared with T.I. and Samar Hasnain.

Author information

Affiliations

  1. Department of Physics and Astronomy and California NanoSystems Institute, University of California, Los Angeles, California 90095, USA

    • Rui Xu
    • , Zhifeng Huang
    • , Chien-Chun Chen
    • , Yunfei Zou
    •  & Jianwei Miao
  2. State Key Laboratory of Crystal Materials, Shandong University, Jinan 250100, China

    • Huaidong Jiang
    •  & Jiadong Fan
  3. RIKEN SPring-8 Center, Kouto 1-1-1, Sayo, Hyogo 679-5148, Japan

    • Changyong Song
    • , Daewoong Nam
    • , Jaehyun Park
    • , Marcus Gallagher-Jones
    • , Sangsoo Kim
    • , Sunam Kim
    • , Yuki Takayama
    • , Tomotaka Oroguchi
    • , Takaki Hatsui
    • , Yuichi Inubushi
    • , Koji Yonekura
    • , Takahiro Sato
    • , Masaki Yamamoto
    • , Masayoshi Nakasako
    • , Makina Yabashi
    •  & Tetsuya Ishikawa
  4. Department of Biological Chemistry, UCLA-DOE Institute for Genomics and Proteomics, University of California, Los Angeles, California 90095, USA

    • Jose A. Rodriguez
  5. Department of Physics, Pohang University of Science and Technology, Pohang 790-784, Korea

    • Daewoong Nam
  6. Institute of Integrative Biology, University of Liverpool, Liverpool L69 7ZB, UK

    • Marcus Gallagher-Jones
  7. Department of Precision Science and Technology, Graduate School of Engineering, Osaka University, 2-1 Yamada-oka, Suita, Osaka 565-0871, Japan

    • Akihiro Suzuki
    •  & Yukio Takahashi
  8. Department of Physics, Faculty of Science and Technology, Keio University, 3-14-1 Hiyoshi, Kohoku-ku, Yokohama, Kanagawa 223-8522, Japan

    • Yuki Takayama
    • , Tomotaka Oroguchi
    •  & Masayoshi Nakasako
  9. Japan Synchrotron Radiation Research Institute, Kouto 1-1-1, Sayo, Hyogo 679-5198, Japan

    • Takashi Kameshima
    • , Kensuke Tono
    •  & Tadashi Togashi

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Contributions

J.M. directed the research; J.M. and H.J. designed the experiment; R.X., J.M., C.S. Z.H., J.A.R., H.J., D.N., J.P., M.G.-J., Sa. K., Su. K., A.S., Yuki T., T.O., Yukio T., T.H., Y.I., T.K., K.Y., K.T., T.T., T.S., Mas. Y., M.N., Mak. Y. and T.I. conducted the experiments; R.X., J.M., H.J., Z.H., J.A.R., C.-C.C., J.F. and Y.Z. analysed the data, performed reconstructions and interpreted the results, J.M., R.X., H.J., C.S. and J.A.R. wrote the manuscript. All authors commented on the manuscript.

Competing interests

The authors declare no competing financial interests.

Corresponding author

Correspondence to Jianwei Miao.

Supplementary information

PDF files

  1. 1.

    Supplementary Figures and Table

    Supplementary Figures 1-12 and Supplementary Table 1

Videos

  1. 1.

    Supplementary Movie 1

    A real-time movie of a typical single-shot XFEL experiment. XFEL pulses (photon energy: 5.4 keV, pulse duration: ~10 fs and pulse energy at the source: ~300  μJ) was focused to a ~1.5  μm spot by a pair of K-B mirrors and impinged on high-index-faceted gold nanocrystals deposited on a 100-nm-thick Si3N4 membrane. The experiment was performed at 1 Hz.

  2. 2.

    Supplementary Movie 2

    100 good quality single-shot diffraction patterns collected from trisoctahedral gold nanocrystals, each hit by an XFEL pulse based on the diffraction-before-destruction scheme.

  3. 3.

    Supplementary Movie 3

    Iso-surface renderings of the 3D reconstructions from a single-shot diffraction pattern (a) and an assembled 3D diffraction pattern (b).

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DOI

https://doi.org/10.1038/ncomms5061

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