Skip to main content

Thank you for visiting nature.com. You are using a browser version with limited support for CSS. To obtain the best experience, we recommend you use a more up to date browser (or turn off compatibility mode in Internet Explorer). In the meantime, to ensure continued support, we are displaying the site without styles and JavaScript.

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.

Your institute does not have access to this article

Relevant articles

Open Access articles citing this article.

Access options

Buy article

Get time limited or full article access on ReadCube.

$32.00

All prices are NET prices.

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.

References

  1. Hull, D. & Bacon, D. J. Introduction to Dislocations 5th edn (Butterworth-Heinemann, 2011)

    Google Scholar 

  2. Smith, W. F. & Hashemi, J. Foundations of Materials Science and Engineering 4th edn (McGraw-Hill Science, 2005)

    Google Scholar 

  3. Nakamura, S. The roles of structural imperfections in InGaN-based blue light-emitting diodes and laser diodes. Science 281, 956–961 (1998)

    CAS  Article  Google Scholar 

  4. Hua, G. C. et al. Microstructure study of a degraded pseudomorphic separate confinement heterostructure blue-green laser diode. Appl. Phys. Lett. 65, 1331–1333 (1994)

    ADS  CAS  Article  Google Scholar 

  5. Hirsch, P. B., Horne, R. W. & Whelan, M. J. LXVIII. Direct observations of the arrangement and motion of dislocations in aluminium. Phil. Mag. 1, 677–684 (1956)

    ADS  CAS  Article  Google Scholar 

  6. Bollmann, W. Interference effects in the electron microscopy of thin crystal foils. Phys. Rev. 103, 1588–1589 (1956)

    ADS  CAS  Article  Google Scholar 

  7. Menter, J. W. The direct study by electron microscopy of crystal lattices and their imperfections. Proc. R. Soc. Lond. A 236, 119–135 (1956)

    ADS  CAS  Article  Google Scholar 

  8. Howie, A. & Whelan, M. J. Diffraction contrast of electron microscope images of crystal lattice defects. III. Results and experimental confirmation of the dynamical theory of dislocation image contrast. Proc. R. Soc. Lond. A 267, 206–230 (1962)

    ADS  CAS  Article  Google Scholar 

  9. Hirsch, P. B., Cockayne, D. J. H., Spence, J. C. H. & Whelan, M. J. 50 years of TEM of dislocations: past, present and future. Phil. Mag. 86, 4519–4528 (2006)

    ADS  CAS  Article  Google Scholar 

  10. Spence, J. C. H. Experimental High-Resolution Electron Microscopy 3rd edn (Oxford Univ. Press, 2003)

    Google Scholar 

  11. Chisholm, M. F. & Pennycook, S. J. Structural origin of reduced critical currents at YBa2Cu3O7−δ grain boundaries. Nature 351, 47–49 (1991)

    ADS  CAS  Article  Google Scholar 

  12. Ludwig, W. et al. Three-dimensional imaging of crystal defects by ‘topo-tomography’. J. Appl. Crystallogr. 34, 602–607 (2001)

    CAS  Article  Google Scholar 

  13. Cockayne, D. J. H., Ray, I. L. F. & Whelan, M. J. Investigations of dislocation strain fields using weak beams. Phil. Mag. 20, 1265–1270 (1969)

    ADS  CAS  Article  Google Scholar 

  14. Pennycook, S. J. & Nellist, P. D. Scanning Transmission Electron Microscopy: Imaging and Analysis 1st edn (Springer, 2011)

    Book  Google Scholar 

  15. Barnard, J. S., Sharp, J., Tong, J. R. & Midgley, P. A. High-resolution three-dimensional imaging of dislocations. Science 313, 319 (2006)

    CAS  Article  Google Scholar 

  16. Midgley, P. A. & Weyland, M. in Scanning Transmission Electron Microscopy: Imaging and Analysis. (eds Pennycook, S. J. & Nellist, P. D. ) 353–392 (Springer, 2011)

    Book  Google Scholar 

  17. Kelly, T. F. & Miller, M. K. Atom probe tomography. Rev. Sci. Instrum. 78, 031101 (2007)

    ADS  Article  Google Scholar 

  18. Xin, H. L., Ercius, P., Hughes, K. J., Engstrom, J. R. & Muller, D. A. Three-dimensional imaging of pore structures inside low-κ dielectrics. Appl. Phys. Lett. 96, 223108 (2010)

    ADS  Article  Google Scholar 

  19. 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)

    ADS  CAS  Article  Google Scholar 

  20. Scott, M. C. et al. Electron tomography at 2.4 Å resolution. Nature 483, 444–447 (2012)

    ADS  CAS  Article  Google Scholar 

  21. Howie, A. Diffraction channelling of fast electrons and positrons in crystals. Phil. Mag. 14, 223–237 (1966)

    ADS  CAS  Article  Google Scholar 

  22. Chiu, C. Y. et al. Platinum nanocrystals selectively shaped using facet-specific peptide sequences. Nature Chem. 3, 393–399 (2011)

    ADS  CAS  Article  Google Scholar 

  23. Miao, J., Föster, F. & Levi, O. Equally sloped tomography with oversampling reconstruction. Phys. Rev. B 72, 052103 (2005)

    ADS  Article  Google Scholar 

  24. Lee, E. et al. Radiation dose reduction and image enhancement in biological imaging through equally sloped tomography. J. Struct. Biol. 164, 221–227 (2008)

    CAS  Article  Google Scholar 

  25. 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)

    Article  Google Scholar 

  26. Zhao, Y. et al. High resolution, low dose phase contrast x-ray tomography for 3D diagnosis of human breast cancers. Proc. Natl Acad. Sci. USA 109, 18290–18294 (2012)

    ADS  CAS  Article  Google Scholar 

  27. Marks, L. D. Wiener-filter enhancement of noisy HREM images. Ultramicroscopy 62, 43–52 (1996)

    CAS  Article  Google Scholar 

  28. Howie, A. & Marks, L. D. Elastic strains and the energy balance for multiply twinned particles. Phil. Mag. A 49, 95–109 (1984)

    ADS  CAS  Article  Google Scholar 

  29. Balk, T. J. & Hemker, K. J. High resolution transmission electron microscopy of dislocation core dissociations in gold and iridium. Phil. Mag. A 81, 1507–1531 (2001)

    ADS  CAS  Article  Google Scholar 

  30. Johnson, C. L. J. et al. Effects of elastic anisotropy on strain distributions in decahedral gold nanoparticles. Nature Mater. 7, 120–124 (2008)

    ADS  CAS  Article  Google Scholar 

  31. 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)

    ADS  CAS  Article  Google Scholar 

  32. Bailey, D. H. & Swarztrauber, P. N. The fractional Fourier transform and applications. SIAM Rev. 33, 389–404 (1991)

    MathSciNet  Article  Google Scholar 

  33. 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)

    MathSciNet  Article  Google Scholar 

  34. Kirkland, E. J. Advanced Computing in Electron Microscopy 2nd edn (Springer, 2010)

    Book  Google Scholar 

  35. Brown, R. G. & Hwang, P. Y. C. Introduction to Random Signals and Applied Kalman Filtering 3rd edn (Wiley, 1996)

    MATH  Google Scholar 

  36. Saxton, W. O. Computer Techniques for Image Processing in Electron Microscopy (Academic, 1978)

    Google Scholar 

  37. Hawkes, P. W. Computer Processing of Electron Microscope Images (Springer, 1980)

    Book  Google Scholar 

  38. Möbus, G., Necker, G. & Rühle, M. Adaptive Fourier-filtering technique for quantitative evaluation of high-resolution electron micrographs of interfaces. Ultramicroscopy 49, 46–65 (1993)

    Article  Google Scholar 

Download references

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.

Author information

Authors and Affiliations

Authors

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.

Corresponding author

Correspondence to Jianwei Miao.

Ethics declarations

Competing interests

The authors declare no competing financial interests.

Supplementary information

PowerPoint slides

Rights and permissions

Reprints and Permissions

About this article

Cite this article

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

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1038/nature12009

Further reading

Comments

By submitting a comment you agree to abide by our Terms and Community Guidelines. If you find something abusive or that does not comply with our terms or guidelines please flag it as inappropriate.

Search

Quick links

Nature Briefing

Sign up for the Nature Briefing newsletter — what matters in science, free to your inbox daily.

Get the most important science stories of the day, free in your inbox. Sign up for Nature Briefing