Skip to main content
SpringerLink
Log in

Quantitative microstructural imaging by scanning Laue x-ray micro- and nanodiffraction

  • Synchrotron Radiation Research in Materials Science
  • Published:
MRS Bulletin Aims and scope Submit manuscript

Abstract

Local crystal structure, crystal orientation, and crystal deformation can all be probed by Laue diffraction using a submicron x-ray beam. This technique, employed at a synchrotron facility, is particularly suitable for fast mapping the mechanical and microstructural properties of inhomogeneous multiphase polycrystalline samples, as well as imperfect epitaxial films or crystals. As synchrotron Laue x-ray microdiffraction enters its 20th year of existence and new synchrotron nanoprobe facilities are being built and commissioned around the world, we take the opportunity to overview current capabilities as well as the latest technical developments. Fast data collection provided by state-of-the-art area detectors and fully automated pattern indexing algorithms optimized for speed make it possible to map large portions of a sample with fine step size and obtain quantitative images of its microstructure in near real time. We extrapolate how the technique is anticipated to evolve in the near future and its potential emerging applications at a free-electron laser facility.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Figure 1
Figure 2
Figure 3
Figure 4
Figure 5
Figure 6

Similar content being viewed by others

References

  1. W. Friedrich, P. Knipping, M.V. Laue, Sitzungsber. Kö niglich-Bayerischen Akad. der Wiss. Math. Phys. Kla. 42, 303 (1912).

    Google Scholar 

  2. W.L. Bragg, Proc. Cambridge Philos. Soc. 17, 43 (1913).

  3. M.M. Woolfson, An Introduction to X-Ray Crystallography (Cambridge University Press, Cambridge, 1997).

  4. R.E. Dinnebier, S.L.J. Billinge, Eds., Powder Diffraction: Theory and Practice (RSC Publishing, Cambridge, 2008).

  5. D.K. Bowen, B.K. Tanner, High Resolution X-Ray Diffractometry and Topography (CRC Press, Boca Raton, FL, 2005).

  6. K. Moffat, D. Szebenyi, D. Bilderback, Science 223 (4643), 1423 (1984).

  7. J.R. Helliwell, J. Habash, D.W.J. Cruikshank, M.M. Harding, T.J. Greenhough, J.W. Campbell, I.J. Clifton, M. Elder, P.A. Machin, M.Z. Papiz, S. Zurek, J. Appl. Crystallogr. 22 (5), 483 (1989).

  8. K. Moffat, J.R. Helliwell, in Synchrotron Radiation in Chemistry and Biology III, E. Mandelkow, Ed. (Springer-Verlag, Berlin, 1989), p. 61.

  9. D. Bourgeois, B. Vallone, F. Schotte, A. Arcovito, A.E. Miele, G. Sciara, M. Wulff, P. Anfinrud, M. Brunori, Proc. Natl. Acad. Sci. U.S.A. 100 (15), 8704 (2003).

  10. H.R. Wenk, F. Heidelbach, D. Chateigner, F. Zontone, J. Synchrotron Radiat. 4 (2), 95 (1997).

  11. J. Chung, G. Ice, J. Appl. Phys. 86 (9), 5249 (1999).

  12. O. Tschauner, P.D. Asimow, N. Kostandova, T.J. Ahrens, C. Ma, S. Sinogeikin, Z. Liu, S. Fakra, N. Tamura, Proc. Natl. Acad. Sci. U.S.A. 106 (33), 13691 (2009).

  13. A. Mehta, X.-Y. Gong, V. Imbeni, A.R. Pelton, R.O. Ritchie, Adv. Mater. 19 (9), 1183 (2007).

  14. B.C. Valek, J.C. Bravman, N. Tamura, A.A. MacDowell, R.S. Celestre, H.A. Padmore, R. Spolenak, W.L. Brown, B.W. Batterman, J.R. Patel, Appl. Phys. Lett. 81 (22), 4168 (2002).

  15. J.J. Bozzola, L.D. Russell, Electron Microscopy: Principles and Techniques for Biologists (Jones & Bartlett Learning, Sudbury, MA, 1999).

  16. O.E. Myers Jr., Am. J. Phys. 19 (6), 359 (1951).

  17. B. Lai, W. Yun, D.G. Legnini, Y. Xiao, J. Chrzas, P.J. Vicario, V. White, S. Bajikar, D. Denton, F. Cerrina, E. Di Fabrizio, M. Gentili, L. Grella, M. Baciocchi, Appl. Phys. Lett. 61 (16), 1877 (1992).

  18. Y.S. Chu, J.M. Yi, F. De Carlo, Q. Shen, W.-K. Lee, H.J. Wu, C.L. Wang, J.Y. Wang, C.J. Liu, C.H. Wang, S.R. Wu, C.C. Chien, Y. Hwu, A. Tkachuck W. Yun, M. Feser, K.S. Liang, C.S. Yang, J.H. Je, G. Margaritondo, Appl. Phys. Lett. 92 (10), 103119 (2008).

  19. W. Chao, J. Kim, S. Rekawa, P. Fischer, E.H. Anderson, Opt. Express 17 (20), 17669 (2009).

  20. A. Snigirev, V. Kohn, I. Snigireva, B. Lengeler, Nature 384 (6604), 49 (1996).

  21. A.A. Snigirev, I. Snigireva, M. Drakopoulos, V. Nazmov, E. Reznikova, S. Kuznetsov, M. Grigoriev, J. Mohr, V. Saile, Proc. SPIE 5195, 21 (2003).

  22. C.G. Schroer, M. Kuhlmann, U.T. Hunger, T.F. Günzler, O. Kurapova, S. Feste, F. Frehse, B. Lengeler, M. Drakopoulos, A. Somogyi, A.S. Simionovici, A. Snigirev I. Snigireva, C. Schug, W.H. Schröder, Appl. Phys. Lett. 82 (9), 1485 (2003).

  23. P. Kirkpatrick, A.V. Baez, J. Opt. Soc. Am. 38 (9), 766 (1948).

  24. H. Mimura, S. Matsuyama, H. Yumoto, H. Hara, K. Yamamura, Y. Sano, M. Shibahara, K. Endo, Y. Mori, Y. Nishino, Jpn. J. Appl. Phys. 44 (18), L 539 (2005).

  25. W. Liu, G.E. Ice, J.Z. Tischler, A. Khounsary, C. Liu, L. Assoufid, A.T. Macrander, Rev. Sci. Instrum. 76 (11), 113701 (2005).

  26. W. Liu, G.E. Ice, L. Assoufid, C. Liu, B. Shi, R. Khachatryan, J. Qian, P. Zschack, J.Z. Tischler, J.-Y. Choi, J. Synchrotron Radiat. 18 (4), 575 (2011).

  27. G.E. Ice, B.C. Larson, Adv. Eng. Mater. 2 (10), 643 (2000).

  28. M. Kunz, N. Tamura, K. Chen, A.A. MacDowell, R.S. Celestre, M.M. Church S. Fakra, E.E. Domning, J.M. Glossinger, J.L. Kirschman, G.Y. Morrison, D.W. Plate, B.V. Smith, T. Warwick, V.V. Yashchuk, H.A. Padmore, E. Ustundag, Rev. Sci. Instrum. 80 (3), 035108 (2009).

  29. N. Tamura, R.S. Celestre, A.A. MacDowell, H.A. Padmore, R. Spolenak, B.C. Valek, N. Meier Chang, A. Manceau, J.R. Patel, Rev. Sci. Instrum. 73 (3), 1369 (2002).

  30. O. Ulrich, X. Biquard, P. Bleuet, O. Geaymond, P. Gergaud, J.S. Micha, O. Robach, F. Rieutord, Rev. Sci. Instrum. 82 (3), 033908 (2011).

  31. J.-H. Park, J. Park, K.-B. Lee, T.-Y. Koo, H.S. Shun, Y.D. Ko, J.-S. Chung, J.Y. Hwang, S.-Y. Jeong, Appl. Phys. Lett. 91 (1), 012906 (2007).

  32. R. Feng, A. Gerson, G. Ice, AIP Conf. Proc. 879, 872 (2007).

  33. R. Maaβ, D. Grolimund, S.V. Petegem, Appl. Phys. Lett. 89 (15), 151905 (2006).

  34. F. Hofmann, X. Song, I. Dolbnya, B. Abbey, A.M. Korsunsky, Procedia Eng. 1 (1), 193 (2009).

  35. http://www.nsrrc.org.tw/english/tps.aspx.

  36. http://ssrf.sinap.ac.cn/english.

  37. http://www.synchrotron.org.au.

  38. N. Tamura, M. Kunz, K. Chen, Mater. Sci. Eng. A 524 (1), 28 (2009).

  39. Y. Sheng, M. Church, V.Y. Valeriy, K. Goldberg, R.S. Celestre, W.R. McKinneyr J. Kirschman, G.Y. Morrison, T. Noll, T. Warwick, H.A. Padmore, X-Ray Opt. Instrum. 2010, 784732 (2010).

  40. K.S. Liang, G.-H. Luo, J.-R. Chen, D.-J. Huang, C.-S. Hwang, C. Wang, C.T. Chen, Synchrotron Radiat. News 22 (5), 13 (2009).

  41. A.B. Greninger, Trans. Am. Inst. Min. Metall. Pet. Eng. 117, 61 (1935).

  42. J.S. Chung, N. Tamura, G.E. Ice, B.C. Larson, J.D. Budai, “X-Ray Microbeam Measurement of Local Texture and Strain in Metals,” Mater. Res. Soc. Symp. Proc. 563, D. Brown, A.H. Verbruggen, C.A. Volkert, Eds. (Materials Research Society, Warrendale, PA, 1999), p. 169.

  43. N.Tamura, B.C. Valek, R. Spolenak, A.A. MacDowell, R.S. Celestre, H.A. Padmore, W.L. Brown, T. Marieb, J.C. Bravman, B.W. Batterman, J.R. Patel, “Materials, Technology, and Reliability for Advanced Interconnects and Low-k Dielectrics,” Mater. Res. Soc. Symp. Proc. 612, K. Maex, Y.-C. Joo, G.S. Oehrlein, S. Ogawa, J.T. Wetzel, Eds. (Materials Research Society, Warrendale, PA, 2000).

  44. R.I. Barabash, G.E. Ice, B.C. Larson, W. Yang, Rev. Sci. Instrum. 73 (3), 1652 (2002).

  45. B.C. Larson, W. Yang, G.E. Ice, J.D. Budai, J.Z. Tischler, Nature 415 (6874), 887 (2002).

  46. W. Liu, G.E. Ice, in Strain and Dislocation Gradients from Diffraction R. Barabash, G.E. Ice, Eds. (World Scientific, Singapore, 2014), p. 53.

  47. J.D. Budai, W. Yang, B.C. Larson, J.Z. Tischler, W. Liu, H. Weiland, G.E. Ice, Mater. Sci. Forum 467–470, 1373 (2004).

  48. N.B. Morgan, Mater. Sci. Eng. A 378 (1), 16 (2004).

  49. H.E. Karaca, I. Karaman, B. Basaran, Y. Ren, Y.I. Chumlyakov, H.J. Maier Adv. Funct. Mater. 19 (7), 983 (2009).

  50. V. Srivastava, X. Chen, R.D. James, Appl. Phys. Lett. 97 (1), 014101 (2010).

  51. V. Srivastava, Y. Song, K. Bhatti, R.D. James, Adv. Energy Mater. 1 (1), 97 (2011).

  52. Y. Song, K.P. Bhatti, V. Srivastava, C. Leighton, R.D. James, Energy Environ. Sci. 6 (4), 1315 (2013).

  53. Y. Song, Phys. Chem. Chem. Phys. 16 (25), 12750 (2014).

  54. X. Chen, S. Cao, T. Ikeda, V. Srivastava, G.J. Snyder, D. Schryvers, R.D. James, Acta Mater. 59 (15), 6124 (2011).

  55. Y. Song, X. Chen, V. Dabada, T.W. Shield, R.D. James, Nature 502 (7469), 85 (2013).

  56. C. Chluba, W. Ge, R.L. de Miranda, J. Strobel, L. Kienle, E. Quandt, M. Wuttig Science 348 (6238), 1004 (2015).

  57. X. Chen, V. Srivastava, V. Dabade, R.D. James, J. Mech. Phys. Solids 6 1 (12), 2566 (2013).

  58. X. Chen, Y. Song, N. Tamura, R.D. James, J. Mech. Phys. Solids (2016), doi:10.1016/j.jmps.2016.02.009.

  59. P.-C. Wang, G.S. Cargill III, I.C. Noyan, C.-K. Hu, Appl. Phys. Lett. 72 (11), 1296 (1998).

  60. P.S. Ho, T. Kwok, Rep. Prog. Phys. 52 (3), 301 (1989).

  61. B.C. Valek, N. Tamura, R. Spolenak, W.A. Caldwell, A.A. MacDowell R.S. Celestre, H.A. Padmore, J.C. Bravman, B.W. Batterman, W.D. Nix, J.R. Patel J. Appl. Phys. 94 (6), 3757 (2003).

  62. R.I. Barabash, G.E. Ice, N. Tamura, B.C. Valek, J.C. Bravman, R. Spolenak, J.R. Patel, J. Appl. Phys. 93 (9), 5701 (2003).

  63. K. Chen, N. Tamura, B.C. Valek, K.-N. Tu, J. Appl. Phys. 104 (1), 013513 (2008).

  64. A.S. Budiman, P.R. Besser, C.S. Hau-Riege, A. Marathe, Y.-C. Joo, N. Tamura, J.R. Patel, W.D. Nix, J. Electron. Mater. 38 (3), 379 (2009).

  65. K. Chen, N. Tamura, K.-N. Tu, “In-Situ Study of Electromigration-Induced Grain Rotation in Pb-Free Solder Joint by Synchrotron Microdiffraction,” Mater. Res. Soc. Symp. Proc. 1116, J.R. Greer, J. Vlassak, J. Daniel, T. Tsui, Eds. (Materials Research Society, Warrendale, PA, 2008), p. 1116–I05–06.

  66. K. Chen, N. Tamura, M. Kunz, K.-N. Tu, Y.-S. Lai, J. Appl. Phys. 106 (2) 023502 (2009).

  67. S.S. Iyer, MRS Bull. 40 (3), 225 (2015).

  68. T. Jiang, J. Im, R. Huang, P.S. Ho, MRS Bull. 40 (3), 248 (2015).

  69. A.S. Budiman, H.-A.-S. Shin, B.-J. Kim, S.-H. Hwang, H.-Y. Son, M.-S. Suh Q.-H. Chung, K.-Y. Byun, N. Tamura, M. Kunz, Y.-C. Choo, Microelectron. Reliab. 52 (3), 530 (2012).

  70. T. Jiang, C. Wu, L. Spinella, J. Im, N. Tamura, M. Kunz, H.-Y. Son, B.G. Kim, R. Huang, P.-S. Ho, Appl. Phys. Lett. 103 (21), 211906 (2013).

  71. T. Jiang, C. Wu, N. Tamura, M. Kunz, B.G. Kim, H.-Y. Son, M.S. Suh, J. Im, R. Huang, P.-S. Ho, IEEE Trans. Device Mater. Reliab. 14 (2), 698 (2014).

  72. X. Liu, P.A. Thadesar, C.L. Taylor, M. Kunz, N. Tamura, M.S. Bakir, S.K. Sitaraman, Appl. Phys. Lett. 103 (2), 022107 (2013).

  73. X. Liu, P.A. Thadesar, C.L. Taylor, M. Kunz, N. Tamura, M.S. Bakir, S.K. Sitaraman, J. Appl. Phys. 114 (6), 064908 (2013).

  74. J. Deslippe, A. Essiari, S.J. Patton, T. Samak, C.E. Tull, A. Hexamer, D. Kumar D. Parkinson, P. Stewart, Proc. 9th Workshop Workflows in Support of Large-Scale Sci. IEEE Press, (2014), p. 31.

  75. Y. Li, D. Qian, J. Xue, J. Wan, A. Zhang, N. Tamura, Z. Song, K. Chen, Appl. Phys. Lett. 107 (18), 181902 (2015).

  76. J. Xue, A. Zhang, Y. Li, D. Qian, J. Wan, B. Qi, N. Tamura, Z. Song, K. Chen Sci. Rep. 5, 14903 (2015).

  77. C. Dejoie, M. Kunz, N. Tamura, C. Bousige, K. Chen, S. Teat, C. Beavers C. Baerlocher, J. Appl. Crystallogr. 44 (1), 177 (2011).

  78. C. Dejoie, P. Martinetto, N. Tamura, M. Kunz, F. Porcher, P. Bordat, R. Brown E. Dooryhée,M.Anne, L.B. McCusker, J. Phys. Chem. C 118 (48), 28032 (2014).

  79. C. Dejoie, L.B. McCusker, C. Baerlocher, R. Abela, B.D. Patterson, M. Kunz, N. Tamura, J. Appl. Crystallogr. 46 (3), 791 (2013).

  80. H.N. Chapman, P. Fromme, A. Barty, T.A. Whitem, R.A. Kirian, A. Aquila, M.S. Hunter, J. Schulz, D.P. DePonte, U. Weierstall, R.B. Doak, F.R.N.C. Maia, A.V. Martin, I. Schlichting, L. Lomb, N. Coppola, R.L. Shoeman, S.W. Epp R. Hartmann, D. Rolles, A. Rudenko, L. Foucar, N. Kimmel, G. Weidenspointner P. Holl, M. Liang, M. Barthelmess, C. Caleman, S. Boutet, M.J. Bogan, J. Krzywinski C. Bostedt, S. Bajt, L. Gumprecht, B. Rudek, B. Erk, C. Schmidt, A. Hömke, C. Reich, D. Pietschner, L. Strüder, G. Hauser, H. Gorke, J. Ullrich, S. Herrmann, G. Schaller F. Schopper, H. Soltau, K.-U. Kühnel, M. Messerschmidt, J.D. Bozek, S.P. Hau-Riege, M. Frank, C.Y. Hampton, R.G. Sierra, D. Starodub, G.J. Williams, J. Hajdu N. Timneanu, M.M. Seibert, J. Andreasson, A. Rocker, O. Jönsson, M. Svenda, S. Stern, K. Nass, R. Andritschke, C.-D. Schröter, F. Krasniqi, M. Bott, K.E. Schmidt, X. Wang, I. Grotjohann, J.M. Holton, T.R.M. Barends, R. Neutze, S. Marchesini R. Fromme, S. Schorb, D. Rupp, M. Adolph, T. Gorkhover, I. Andersson H. Hirsemann, G. Potdevin, H. Graafsma, B. Nilsson, J.C.H. Spence, Nature 470 (7332), 73 (2011).

  81. I. Schlichting, IUCrJ 2 (2), 246 (2015).

  82. B.D. Patterson, P. Beaud, H.H. Braun, C. Dejoie, G. Ingold, C. Milne, L. Pattjey, B. Pedrini, J. Szlachentko, R. Abela, CHIMIA 68 (1), 73 (2014).

  83. C. Dejoie, L.B. McCusker, C. Baerlocher, M. Kunz, N. Tamura, J. Appl. Crystallogr. 46 (6), 1805 (2013).

  84. C. Dejoie, S. Smeets, C. Baerlocher, N. Tamura, P. Pattison, R. Abela L. McCusker, IUCrJ 2 (3), 361 (2015).

  85. K. Chen, M. Kunz, N. Tamura, H.-R. Wenk, Geology 43 (3), 2015 (2015).

  86. C. Dejoie, N. Tamura, M. Kunz, P. Goudeau, P. Sciau, J. Appl. Crystallogr. 48 (5), 1522 (2015).

  87. E.Y. Ma, Y.T. Cui, Y. Ueda, S. Tang, K. Chen, N. Tamura, P.M. Wu, J. Fujioka, Y. Tokura, Z.-X. Shen, Science 350 (6260), 538 (2015).

  88. I.C. Olson, R.A. Metzler, N. Tamura, M. Kunz, C.E. Killian, P.U.P.A. Gilbert, J. Struct. Biol. 183 (2), 180 (2013).

    Google Scholar 

  89. R. Barabash, G. Ice, Eds., Strain and Dislocation Gradients from Diffraction: Spatially-Resolved Local Structure and Defects (World Scientific, Singapore, 2014).

Download references

Acknowledgment

The Advanced Light Source is supported by the Director, Office of Science, Office of Basic Energy Sciences, of the US Department of Energy under Contract No. DE-AC02–05CH11231.

Author information

Authors and Affiliations

  1. Department of Mechanical and Aerospace Engineering, Hong Kong University of Science and Technology, Hong Kong

    Xian Chen

  2. Department of Materials, ETH Zürich, Switzerland

    Catherine Dejoie

  3. Department of Materials Science and Engineering and Advanced Materials Processing and Analysis Center, University of Central Florida, USA

    Tengfei Jiang

  4. Scientific Research Division, National Synchrotron Radiation Research Center, Taiwan

    Ching Shun Ku

  5. Advanced Light Source, Lawrence Berkeley National Laboratory, USA

    Nobumichi Tamura

Authors
  1. Xian Chen
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Catherine Dejoie
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Tengfei Jiang
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Ching Shun Ku
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Nobumichi Tamura
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Xian Chen.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Chen, X., Dejoie, C., Jiang, T. et al. Quantitative microstructural imaging by scanning Laue x-ray micro- and nanodiffraction. MRS Bulletin 41, 445–453 (2016). https://doi.org/10.1557/mrs.2016.97

Download citation

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1557/mrs.2016.97

Search

Navigation