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.

  • Letter
  • Published:

Grain rotation and lattice deformation during photoinduced chemical reactions revealed by in situ X-ray nanodiffraction

Abstract

In situ X-ray diffraction (XRD) and transmission electron microscopy (TEM) have been used to investigate many physical science phenomena, ranging from phase transitions, chemical reactions and crystal growth to grain boundary dynamics1,2,3,4,5,6. A major limitation of in situ XRD and TEM is a compromise that has to be made between spatial and temporal resolution1,2,3,4,5,6. Here, we report the development of in situ X-ray nanodiffraction to measure high-resolution diffraction patterns from single grains with up to 5 ms temporal resolution. We observed, for the first time, grain rotation and lattice deformation in chemical reactions induced by X-ray photons: Br + hv → Br + e and e + Ag+ → Ag0. The grain rotation and lattice deformation associated with the chemical reactions were quantified to be as fast as 3.25 rad s−1 and as large as 0.5 Å, respectively. The ability to measure high-resolution diffraction patterns from individual grains with a temporal resolution of several milliseconds is expected to find broad applications in materials science, physics, chemistry and nanoscience.

This is a preview of subscription content, access via your institution

Access options

Buy this article

Prices may be subject to local taxes which are calculated during checkout

Figure 1: Schematic layout of in situ X-ray nanodiffraction with up to 5 ms temporal resolution.
Figure 2: Real-time observation of grain rotation in chemical reactions induced by X-ray photons.
Figure 3: Real-time observation of simultaneous grain rotation and lattice deformation in chemical reactions induced by X-ray photons.

Similar content being viewed by others

References

  1. Reimers, J. N. & Dahn, J. R. Electrochemical and in situ X-ray diffraction studies of lithium intercalation in LixCoO2 . J. Electrochem. Soc. 139, 2091–2097 (1992).

    Article  CAS  Google Scholar 

  2. Grossa, K. J., Guthrie, S., Takara, S. & Thomas, G. In-situ X-ray diffraction study of the decomposition of NaAlH4 . J. Alloys Compd. 297, 270–281 (2000).

    Article  Google Scholar 

  3. Margulies, L., Winther, G. & Poulsen, H. F. In situ measurement of grain rotation during deformation of polycrystals. Science 291, 2392–2394 (2001).

    Article  CAS  Google Scholar 

  4. Schmidt, S. et al. Watching the growth of bulk grains during recrystallization of deformed Metals. Science 305, 229–232 (2004).

    Article  CAS  Google Scholar 

  5. Williamson, M. J., Tromp, R. M., Vereecken, P. M., Hull, R. & Ross, F. M. Dynamic microscopy of nanoscale cluster growth at the solid–liquid interface. Nature Mater. 2, 532–536 (2003).

    Article  CAS  Google Scholar 

  6. Zheng, H. et al. Observation of single colloidal platinum nanocrystal growth trajectories. Science 324, 1309–1312 (2009).

    Article  CAS  Google Scholar 

  7. Gottstein, G. & Shvindlerman, L. S. Grain Boundary Migration in Metals: Thermodynamics, Kinetics, Applications 2nd edn (CRC Press, 2009).

    Book  Google Scholar 

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

    Google Scholar 

  9. Miao, J., Ishikawa, T., Robinson, I. K. & Murnane, M. M. Beyond crystallography: Diffractive imaging using coherent X-ray light source. Science 348, 530–535 (2015).

    Article  CAS  Google Scholar 

  10. Williams, D. B. & Carter, C. B. Transmission Electron Microscopy: A Textbook for Materials Science 2nd edn (Springer, 2009).

    Book  Google Scholar 

  11. Ke, M., Hackney, S. A., Milligan, W. W. & Aifantis, E. C. Observation and measurement of grain rotation and plastic strain in nanostructured metal thin films. Nanostruct. Mater. 5, 689–697 (1995).

    Article  CAS  Google Scholar 

  12. Larson, B. C., Yang, W., Ice, G. E., Budai, J. D. & Tischler, J. Z. Three-dimensional X-ray structural microscopy with submicrometre resolution. Nature 415, 887–890 (2002).

    Article  CAS  Google Scholar 

  13. Offerman, S. E. et al. Grain nucleation and growth during phase transformations. Science 298, 1003–1005 (2002).

    Article  CAS  Google Scholar 

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

    Article  CAS  Google Scholar 

  15. Chen, C-C. et al. Three-dimensional imaging of dislocations in a nanoparticle at atomic resolution. Nature 496, 74–77 (2013).

    Article  CAS  Google Scholar 

  16. Harris, K. E., Singh, V. V. & King, A. H. Grain rotation in thin films of gold. Acta Mater. 46, 2623–2633 (1998).

    Article  CAS  Google Scholar 

  17. Salditt, T. et al. Partially coherent nano-focused x-ray radiation characterized by Talbot interferometry. Opt. Express 19, 9656–9675 (2011).

    Article  CAS  Google Scholar 

  18. Kraft, P. et al. Performance of single-photon-counting PILATUS detector modules. J. Synchrotron Radiat. 16, 368–375 (2009).

    Article  CAS  Google Scholar 

  19. James, T. H. (ed.) in The Theory of the Photographic Process 4th edn (Macmillan Publishing Co., 1977).

    Google Scholar 

  20. Gurney, R. W. & Mott, N. F. The theory of the photolysis of silver bromide and the photographic latent image. Proc. R. Soc. Lond. A 64, 151–167 (1938).

    Article  Google Scholar 

  21. Leite, E. R. et al. Crystal growth in colloidal tin oxide nanocrystals induced by coalescence at room temperature. Appl. Phys. Lett. 83, 1566–1568 (2003).

    Article  CAS  Google Scholar 

  22. Shan, Z. et al. Grain boundary-mediated plasticity in nanocrystalline nickel. Science 305, 654–657 (2004).

    Article  CAS  Google Scholar 

  23. Berry, C. R. & Griffith, R. L. Structure and growth mechanism of photolytic silver in silver bromide. Acta Crystallogr. 3, 219–222 (1950).

    Article  CAS  Google Scholar 

  24. Burley, G. Photolytic behavior of silver iodide. J. Res. Natl Bur. Stand. 67A, 301–307 (1963).

    Article  CAS  Google Scholar 

  25. Pearson, W. B. A Handbook of Lattice Spacings and Structures of Metals and Alloys (Pergamon Press, 1958).

    Google Scholar 

  26. Huberman, M. L. & Grimsditch, M. Lattice expansions and contractions in metallic superlattices. Phys. Rev. Lett. 62, 1403–1406 (1989).

    Article  CAS  Google Scholar 

  27. Diao, J., Gall, K. & Dunn, M. L. Surface-stress-induced phase transformation in metal nanowires. Nature Mater. 2, 656–660 (2003).

    Article  CAS  Google Scholar 

  28. Clark, J. N. et al. Ultrafast three-dimensional imaging of lattice dynamics in individual gold nanocrystals. Science 341, 56–59 (2013).

    Article  CAS  Google Scholar 

  29. Shyjumon, I. et al. Structural deformation, melting point and lattice parameter studies of size selected silver clusters. Eur. Phys. J. D 37, 409–415 (2006).

    Article  CAS  Google Scholar 

  30. Rocha, T. C. R. & Zanchet, D. Structural defects and their role in the growth of Ag triangular nanoplates. J. Phys. Chem. C 111, 6989–6993 (2007).

    Article  CAS  Google Scholar 

  31. Kirkland, A. I. et al. Structural studies of trigonal lamellar particles of gold and silver. Proc. R. Soc. Lond. A 440, 589–609 (1993).

    Article  CAS  Google Scholar 

  32. Ice, G. E., Budai, J. D. & Pang, J. W. L. The race to X-ray microbeam and nanobeam science. Science 334, 1234–1239 (2011).

    Article  CAS  Google Scholar 

  33. Krüger, S. P. et al. Sub-15 nm beam confinement by two crossed X-ray waveguides. Opt. Express 18, 13492–13501 (2010).

    Article  Google Scholar 

  34. Patterson, A. The Scherrer formula for X-ray particle size determination. Phys. Rev. 56, 978–982 (1939).

    Article  CAS  Google Scholar 

Download references

Acknowledgements

We thank I. Vartaniants for stimulating discussions and A. Zozulya for help with the experiments. This work was supported by the DARPA PULSE program through a grant from AMRDEC and Helmholtz Society grants VH-VI-403 and DFG SFB755. This work was also partially funded by the Office of Basic Energy Sciences of the US Department of Energy (Grant No. DE-FG02-13ER46943), ONR MURI (Grant No. N00014-14-1-0675) and NSF (Grant No. DMR-1437263).

Author information

Authors and Affiliations

Authors

Contributions

J.M. directed the project; Z.H., M.B., R.X., T.S., J.M., M.O., S.K., M.S., A.S., Y.T. and T.N.B. conducted the experiments; Z.H., J.M., M.B., T.N.B., T.S. and M.S. performed the data analysis; J.M., Z.H., T.S. and T.N.B. wrote the manuscript.

Corresponding author

Correspondence to Jianwei Miao.

Ethics declarations

Competing interests

The authors declare no competing financial interests.

Supplementary information

Supplementary Information

Supplementary Information (PDF 1890 kb)

Supplementary Information

Supplementary Movie 1 (AVI 13706 kb)

Supplementary Information

Supplementary Movie 2 (AVI 28064 kb)

Supplementary Information

Supplementary Movie 3 (AVI 2613 kb)

Supplementary Information

Supplementary Movie 4 (AVI 10637 kb)

Supplementary Information

Supplementary Movie 5 (AVI 3608 kb)

Supplementary Information

Supplementary Movie 6 (AVI 23436 kb)

Supplementary Information

Supplementary Movie 7 (AVI 3307 kb)

Supplementary Information

Supplementary Movie 8 (AVI 3490 kb)

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Huang, Z., Bartels, M., Xu, R. et al. Grain rotation and lattice deformation during photoinduced chemical reactions revealed by in situ X-ray nanodiffraction. Nature Mater 14, 691–695 (2015). https://doi.org/10.1038/nmat4311

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1038/nmat4311

This article is cited by

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