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Three-dimensional imaging of dislocations in a nanoparticle at atomic resolution

Abstract

Dislocations and their interactions strongly influence many material properties, ranging from the strength of metals and alloys to the efficiency of light-emitting diodes and laser diodes1,2,3,4. Several experimental methods can be used to visualize dislocations. Transmission electron microscopy (TEM) has long been used to image dislocations in materials5,6,7,8,9, and high-resolution electron microscopy can reveal dislocation core structures in high detail10, particularly in annular dark-field mode11. A TEM image, however, represents a two-dimensional projection of a three-dimensional (3D) object (although stereo TEM provides limited information about 3D dislocations4). X-ray topography can image dislocations in three dimensions, but with reduced resolution12. Using weak-beam dark-field TEM13 and scanning TEM14, electron tomography has been used to image 3D dislocations at a resolution of about five nanometres (refs 15, 16). Atom probe tomography can offer higher-resolution 3D characterization of dislocations, but requires needle-shaped samples and can detect only about 60 per cent of the atoms in a sample17. Here we report 3D imaging of dislocations in materials at atomic resolution by electron tomography. By applying 3D Fourier filtering together with equal-slope tomographic reconstruction, we observe nearly all the atoms in a multiply twinned platinum nanoparticle. We observed atomic steps at 3D twin boundaries and imaged the 3D core structure of edge and screw dislocations at atomic resolution. These dislocations and the atomic steps at the twin boundaries, which appear to be stress-relief mechanisms, are not visible in conventional two-dimensional projections. The ability to image 3D disordered structures such as dislocations at atomic resolution is expected to find applications in materials science, nanoscience, solid-state physics and chemistry.

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Figure 1: 3D reconstruction of a multiply twinned Pt nanoparticle before and after applying a 3D Fourier filter.
Figure 2: Grain boundary comparisons between a 2D experimental projection and several 2.6-Å-thick internal slices of the reconstructed Pt nanoparticle.
Figure 3: Observation of the 3D core structure of an edge dislocation at atomic resolution.
Figure 4: Observation of the 3D core structure of a screw dislocation at atomic resolution.

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Acknowledgements

We thank B. S. Dunn for commenting on our manuscript and L. Ruan for discussions. The tomographic tilt series were acquired at the Electron Imaging Center for NanoMachines of California NanoSystems Institute. This work was supported by UC Discovery/TomoSoft Technologies (IT107-10166). L.D.M. acknowledges support by the NSF MRSEC (DMR-1121262) at the Materials Research Center of Northwestern University.

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Contributions

J.M. conceived and directed the project; C.-Y.C., C.Z., Y.H. and M.C.S. synthesized and prepared the samples; C.Z., E.R.W., B.C.R. and J.M. designed and conducted the experiments; C.-C.C. and J.M. performed the CM alignment and EST reconstruction; J.M., C.-C.C., C.Z. and L.D.M. analysed and interpreted the results, J.M., C.-C.C. and C.Z. wrote the manuscript. All authors commented on the manuscript.

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Correspondence to Jianwei Miao.

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Chen, CC., Zhu, C., White, E. et al. Three-dimensional imaging of dislocations in a nanoparticle at atomic resolution. Nature 496, 74–77 (2013). https://doi.org/10.1038/nature12009

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