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A Basic Introduction to Grazing Incidence Small-Angle X-Ray Scattering

  • P. Müller-BuschbaumEmail author
Chapter
Part of the Lecture Notes in Physics book series (LNP, volume 776)

Abstract

Within the last years, grazing incidence small-angle X-ray scattering (GISAXS) emerged to a versatile and frequently used analysis technique in the field of microand nano-structured thin films and surfaces. GISAXS is used for the characterization of micro- and nano-scale density correlations and shape analysis of objects at surfaces or at buried interfaces for various classes of materials such as ceramics, metals, semiconductors, polymers, biopolymers, and soft matter. As a result, GISAXS provides an excellent complement to more conventional nano-scale structural probes such as atomic force microscopy (AFM) and transmission electron microscopy (TEM). Whereas both are operated in real space, GISAXS as an advanced scattering technique gives results in reciprocal space. In contrast to standard small-angle X-ray scattering (SAXS), which uses transmission geometry described in Chap. 2, GISAXS is performed in reflection geometry. Thus GISAXS has somewhat similarities with SAXS and can be understood as a SAXS experiment performed in another scattering geometry (replacing transmission by reflection geometry). Alternatively, GISAXS can be envisaged as the extension of grazing incidence diffraction (GID) to small scattering angles or as a sort of diffuse reflectivity. Consequently, three different X-ray communities, SAXS, GID, and diffuse reflectivity are converging through GISAXS [1].

Keywords

Incident Angle Critical Angle Bragg Peak Pair Correlation Function Grazing Incidence 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.

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Reference

  1. 1.
    Müller-Buschbaum P. Structure determination in the thin film geometry using grazing incidence small angle scattering; In Polymer Surfaces and Interfaces: Characterization, Modification and Applications, p.17–46 M. Stamm (Eds.), Springer Berlin, ISBN-13: 978-3-540-73864-0 (2008).Google Scholar
  2. 2.
    Levine J.R., Cohen J.B., Chung Y.W., Georgopoulos P. Grazing-incidence small-angle X-ray scattering: new tool for studying thin film growth; J. Appl. Cryst. 22, 528 (1989).CrossRefGoogle Scholar
  3. 3.
    Levine J.R., Cohen J.B., Chung Y.W. Thin film island growth kinetics: a grazing incidence small angle X-ray scattering study of gold on glass; Surf. Sci. 248, 215 (1991).CrossRefADSGoogle Scholar
  4. 4.
    Salditt T., Metzger T.H., Peisl J., Jiang X. Diffuse X-ray scattering of amorphous multilayers; J. Phys. III 4, 1573 (1994).CrossRefGoogle Scholar
  5. 5.
    Salditt T., Metzger T.H., Peisl J. Kinetic roughness of amorphous multilayers studied by diffuse X-ray scattering; Phys. Rev. Lett. 73, 2228 (1994).CrossRefADSGoogle Scholar
  6. 6.
    Salditt T., Metzger T.H., Brandt Ch., Klemradt U., Peisl J. Determination of the static scaling exponent of self-affine interfaces by nonspecular X-ray scattering; Phys. Rev. B 51, 5617 (1995).CrossRefADSGoogle Scholar
  7. 7.
    Salditt T., Metzger T.H., Peisl J., Reinker B., Moske M., Samwer K. Determination of the height-height correlation function of rough surfaces from diffuse X-ray scattering; Europhys. Lett 32, 331 (1995).CrossRefADSGoogle Scholar
  8. 8.
    Salditt T., Metzger T.H., Peisl J., Goerigk G. Non-specular X-ray scattering from thin films and multilayers with small-angle scattering equipment; J. Phys. D Appl. Phys. 28, A236 (1995).CrossRefADSGoogle Scholar
  9. 9.
    Naudon A., Thiaudiere D. Grazing-incidence small-angle scattering. Morphology of deposited clusters and nanostructure of thin films; J. Appl. Cryst. 30, 822 (1997).CrossRefGoogle Scholar
  10. 10.
    Naudon A., Babonneau D., Thiaudiere D., Lequien S. Grazing-incidence small-angle X-ray scattering applied to the characterization of aggregates in surface regions; Physica B 283, 69 (2000).CrossRefADSGoogle Scholar
  11. 11.
    Hazara S., Gibaud A., Desert A., Sella C., Naudon A. Morphology of nanocermet in thin films: X-ray scattering study; Physica B 283, 97 (2000).CrossRefADSGoogle Scholar
  12. 12.
    Müller-Buschbaum P., Vanhoorne P., Scheumann V., Stamm M. Observation of nano-dewetting structures; Europhys. Lett. 40, 655 (1997).CrossRefADSGoogle Scholar
  13. 13.
    Müller-Buschbaum P., Casagrande M., Gutmann J., Kuhlmann T., Stamm M., Cunis S., von Krosigk G., Lode U., Gehrke R. Determination of micrometer length scales with an X-ray reflection ultra small-angle scattering set-up; Europhys. Lett. 42, 517 (1998).CrossRefADSGoogle Scholar
  14. 14.
    Zhang W., Robinson I.K. Grazing exit small angle X-ray scattering on grain formation in polycrystalline metal films; Z. Kristallogr. 222, 601 (2007).CrossRefGoogle Scholar
  15. 15.
    Rueda D.R., Nogales A., Hernandez J.J., Garcia-Gutierrez M.C., Ezquerra T.A., Roth S.V., Zolotukhin M.G., Serna R. Stacking of main chain-crown ether polymers in nanofilms: A grazing incident medium-small angle X-ray scattering (GIMAXS-GISAXS) study; Langmuir 23, 12677 (2007).CrossRefGoogle Scholar
  16. 16.
    Müller-Buschbaum P., Bauer E., Maurer E., Roth S. V., Gehrke R., Burghammer M., Riekel C. Large scale and local scale structures in polymer blend films: A GIUSAXS and sub-microbeam GISAXS investigation; Appl. Cryst. 40, s341 (2007).CrossRefGoogle Scholar
  17. 17.
    Doshi D.A., Gibaud A., Liu N., Sturmayr D., Malanoski A.P., Dunphy D.R., Chen H., Narayanan S., MacPhee A., Wang J., Reed S.T., Hurd A.J., van Swol F., Brinker C.J. In-situ scattering study of continuous silica-surfactant self-assembly during steady-state dip coating; J. Phys. Chem. B 107, 7683 (2003).CrossRefGoogle Scholar
  18. 18.
    Lee B., Yoon J., Oh W., Hwang Y., Heo K., Jin K.S., Kim J., Kim K.W., Ree M. In-situ grazing incidence small-angle X-ray scattering studies on nanopore evolution in low-k organosilicate dielectric thin films; Macromolecules 38, 3395 (2005).CrossRefADSGoogle Scholar
  19. 19.
    Roth S.V., Burghammer M., Riekel C., Müller-Buschbaum P., Diethert A., Panagiotou P., Walter H. Self-assembled gradient nanoparticle-polymer multilayers investigated by an advanced characterisation method: Microbeam grazing incidence x-ray scattering; Appl. Phys. Lett. 82, 1935 (2003).CrossRefADSGoogle Scholar
  20. 20.
    Roth S.V., Müller-Buschbaum P., Burghammer M., Walter H., Panagiotou P., Diethert A., Riekel C. Microbeam grazing incidence small angle X-ray scattering – a new method to investigate nanostructured heterogeneous thin films and multilayers; Spectrochim. Acta Part B At. Spectrosc. 59, 1765 (2004).Google Scholar
  21. 21.
    Roth S.V., Rankl M., Artus G.R.J., Seeger S., Burghammer M., Riekel C., Müller-Buschbaum P. Domain nano-structure of thin cellulose layers investigated by microbeam grazing incidence small-angle X-ray scattering; Physica B 357, 190 (2005).CrossRefADSGoogle Scholar
  22. 22.
    Müller-Buschbaum P., Roth S.V., Burghammer M., Diethert A., Panagiotou P., Riekel C. Multiple-scaled polymer surfaces investigated with micro-focus grazing incidence small-angle X-ray scattering; Europhys.Lett. 61, 639 (2003).CrossRefADSGoogle Scholar
  23. 23.
    Müller-Buschbaum P., Roth S.V., Burghammer M., Bauer E., Pfister S., David C., Riekel C. Local defects in thin polymer films: A scanning sub-microbeam grazing incidence small angle scattering investigation; Physica B 357, 148 (2005).CrossRefADSGoogle Scholar
  24. 24.
    Müller-Buschbaum P., Perlich J., Abul Kashem M.M., Schulz L., Roth S.V., Cheng Y.J., Gutmann J.S. Combinatorial investigation of nanostructures formed in a titanium dioxide based nanocomposite film on top of fluor-doped tin oxide layers; Phys. Stat. Sol. (RRL) 1, R119 (2007).CrossRefGoogle Scholar
  25. 25.
    Vartanyants I.A., Grigoriev D., Zozulya A.V. Coherent X-ray imaging of individual islands in GISAXS geometry; Thin Solid Films 515, 5546 (2007).CrossRefADSGoogle Scholar
  26. 26.
    Vartanyants I.A., Zozulya A.V., Mundboth K., Yefanov O.M., Richard M.-I., Wintersberger E., Stangl J., Diaz A., Mocuta C., Metzger T.H., Bauer G., Boeck T., Schmidbauer M. Crystal truncation planes revealed by three-dimensional reconstruction of reciprocal space; Phys. Rev. B 77, 115317 (2008).CrossRefADSGoogle Scholar
  27. 27.
    Lee B., Seifert S., Riley S.J., Tikhonov G., Tomczyk N.A., Vajda S., Winans R.E. Anomalous grazing incidence small-angle X-ray scattering studies of platinum nanoparticles formed by cluster deposition; J. Chem. Phys. 123, 074701 (2005).CrossRefADSGoogle Scholar
  28. 28.
    Vajda S., Winans R.E., Elam J.W., Lee B., Pellin M.J., Seifert S., Tikhonov G.Y., Tomczyk N.A. Supported gold clusters and cluster-based nanomaterials: characterization, stability and growth studies by in situ GISAXS under vacuum conditions and in the presence of hydrogen; Top. Catal. 39, 161 (2006).CrossRefGoogle Scholar
  29. 29.
    James R.W. The Optical Principles of the Diffraction of X-Rays. OxBow Press, Woodbridge Connecticut (1962).Google Scholar
  30. 30.
    Born M., Wolf E. Principles of Optics; 2nd ed., Pergamon Press, Oxford (1964).Google Scholar
  31. 31.
    Müller-Buschbaum P. Grazing incidence small-angle X-ray scattering – an advanced scattering technique for the investigation of nanostructured polymer films; Anal. Bioanal. Chem. 376, 3 (2003).Google Scholar
  32. 32.
    Lazzari R. IsGISAXS: a program for grazing incidence small-angle X-ray scattering analysis for supported islands; J. Appl. Cryst. 35, 406 (2002).CrossRefGoogle Scholar
  33. 33.
    The program IsGISAXS with instructions is available on simple request to the author R. Lazzari (http://www.insp.jussieu.fr/axe2/Oxydes/IsGISAXS/isgisaxs.htm) or at http://www.esrf.fr
  34. 34.
    Wang W., Troll K., Kaune G., Metwalli E., Ruderer M., Skrabania K., Laschewsky A., Roth S.V., Papadakis C.M., Müller-Buschbaum P. Thin films of poly(N-isopropylacrylamide) end-capped with n-butyltrithiocarbonate; Macromolecules 41, 3209 (2008).CrossRefADSGoogle Scholar
  35. 35.
    Guinier A., Fournet G. Small-Angle Scattering of X-Rays. John Wiley & Sons, New York (1955).Google Scholar
  36. 36.
    Guinier A. X-Ray Diffraction in Crystals, Imperfect Crystals and Amorphous Bodies. Dover Publications, Inc, New York (1963).Google Scholar
  37. 37.
    Glatter G., Kratky O. Small Angle X-Ray Scattering. Academic Press (1982).Google Scholar
  38. 38.
    Kotlarchyk M., Chen S.-H. Analysis of small-angle scattering spectra from polydisperse interacting colloids; J. Chem. Phys. 79, 2461 (1983).CrossRefADSGoogle Scholar
  39. 39.
    Revenant C., Leroy F., Lazzari R., Renaud G., Henry C.R. Quantitative analysis of grazing incidence small-angle X-ray scattering: Pd/MgO(001) growth; Phys. Rev. B 69, 035411 (2004).Google Scholar
  40. 40.
    Pedersen J. S. Determination of size distributions from small-angle scattering data for systems with effective hard-sphere potential; J. Appl. Crystallogr. 27, 595 (1994).CrossRefGoogle Scholar
  41. 41.
    Revenant C., Leroy F., Renaud G., Lazzari R., Letoublon A., Madey T. Structural and morphological evolution of Co on faceted Pt/W(1 1 1) surface upon thermal annealing; Surf. Sci. 601, 3431 (2007).CrossRefADSGoogle Scholar
  42. 42.
    Lazzari R., Leroy F., Renaud G. Grazing-incidence small-angle X-ray scattering from dense packing of islands on surfaces: Development of distorted wave Born approximation and correlation between particle sizes and spacing; Phys. Rev. B 76, 125411 (2007).CrossRefADSGoogle Scholar
  43. 43.
    Lazzari R., Renaud G., Jupille J., Leroy F. Self-similarity during growth of the Au/TiO2(110) model catalyst as seen by the scattering of X-rays at grazing-angle incidence; Phys. Rev. B 76, 125412 (2007).CrossRefADSGoogle Scholar
  44. 44.
    Hosemann R., Vogel W., Weick D. Novel aspects of the real paracrystal; Acta. Cryst. A 37, 85 (1981).CrossRefGoogle Scholar
  45. 45.
    Müller-Buschbaum P., Hermsdorf N., Roth S.V., Wiedersich J., Cunis S., Gehrke R. Comparative analysis of nanostructured diblock copolymer films; Spectroch. Acta Part B At. Spectrosc. 59, 1789 (2004).CrossRefADSGoogle Scholar
  46. 46.
    Müller-Buschbaum P., Bauer E., Wunnicke O., Stamm M. Control of thin film morphology by an interplay of dewetting, phase separation and micro-phase separation; J. Phys. Condens. Matter 17, S363 (2005).CrossRefGoogle Scholar
  47. 47.
    Lee B., Park I., Yoon J., Park S., Kim J., Kim K.W., Chang T., Ree M. Structural analysis of block copolymer thin films with grazing incidence small-angle X-ray scattering; Macromolecules 38, 4311 (2005).CrossRefADSGoogle Scholar
  48. 48.
    Tang C., Tracz A., Kruk M., Zhang R., Smilgies D.M., Matyjaszewski K., Kowalewski T. Long-range ordered thin films of block copolymers prepared by zone-casting and their thermal conversion into ordered nanostructured carbon; J. Am. Chem. Soc. 127, 6918 (2005).CrossRefGoogle Scholar
  49. 49.
    Busch P., Rauscher M., Smilgies D.-M., Posselt D., Papadakis C.M. Grazing-incidence small-angle X-ray scattering (GISAXS) from thin, nanostructured block copolymer films – The scattering cross-section in the distorted-wave Born approximation; J. Appl. Cryst. 39, 433 (2006).CrossRefGoogle Scholar
  50. 50.
    Busch P., Posselt D., Smilgies D.-M., Rauscher M., Papadakis C.M. Inner structure of thin films of lamellar poly(styrene-b-butadiene) diblock copolymers as revealed by grazing-incidence small-angle scattering; Macromolecules 40, 630 (2007).CrossRefADSGoogle Scholar
  51. 51.
    Jin S., Yoon J., Heo K., Park H.-W., Kim J., Kim K.-W., Shin T.J., Chang T., Ree M. Detailed analysis of gyroid structures in diblock copolymer thin films with synchrotron grazing-incidence X-ray scattering; J. Appl. Cryst. 40, 950 (2007).CrossRefGoogle Scholar
  52. 52.
    Heo K., Yoon J., Jin S., Kim J., Kim K.-W., Shin T.J., Chung B., Chang T., Ree M. Polystyrene-b-polyisoprene thin films with hexagonally perforated layer structure: quantitative grazing-incidence X-ray scattering analysis; J. Appl. Cryst. 41, 281 (2008).CrossRefGoogle Scholar
  53. 53.
    Yoon J., Jin K.S., Kim H.C., Kim G., Heo K., Jin S., Kim J., Kim K.-W., Ree M. Quantitative analysis of lamellar structures in brush polymer thin films by synchrotron grazing-incidence X-ray scattering; J. Appl. Cryst. 40, 476 (2007).CrossRefGoogle Scholar
  54. 54.
    Smarsly B., Gibaud A., Ruland W., Sturmayr D., Brinker C.J. Quantitative SAXS analysis of oriented 2D hexagonal cylindrical silica mesostructures in thin films obtained from nonionic surfactants; Langmuir 21, 3858 (2005).CrossRefGoogle Scholar
  55. 55.
    Ruland W., Smarsly B. 2D SAXS of self-assembled nanocomposite films with oriented arrays of spheres: Determination of lattice type, preferred orientation, deformation and imperfection; J. Appl. Cryst. 59, 435 (2006).Google Scholar
  56. 56.
    Lindner P., Zemb T. Neutrons, X-Rays and Light: Scattering Methods Applied to Soft Condensed matter. Elsevier, Amsterdam (2002).Google Scholar
  57. 57.
    Roth S.V., Walter H., Burghammer M., Riekel C., Lengeler B., Schroer C., Kuhlmann M., Walther T., Domnick R., Müller-Buschbaum P. Combinatorial investigation of the isolated nanoparticle to coalescent layer transition in a gradient sputtered gold nanoparticle multilayer; Appl. Phys. Lett. 88, 021910 (2006).CrossRefADSGoogle Scholar
  58. 58.
    Metwalli E., Couet S., Schlag K., Röhlsberger R., Körstgens V., Ruderer M., Wang W., Kaune G., Roth S.V., Müller-Buschbaum P. In situ GISAXS investigation of gold sputtering onto a polymer template; Langmuir 24, 4265 (2008).CrossRefGoogle Scholar
  59. 59.
    Sinha S.K., Sirota E.B., Garoff S., Stanley H.B. X-ray an neutron scattering from rough surfaces; Phys. Rev. B 38, 2297 (1988).CrossRefADSGoogle Scholar
  60. 60.
    Holy V., Kubuena J., Ohlidal I., Lischka K., Plotz W. X-ray reflection from rough layered systems; Phys. Rev. B 47, 15896 (1993).CrossRefADSGoogle Scholar
  61. 61.
    Holy V., Baumbach T. Non specular X-ray reflection from rough multilayers; Phys. Rev. B 49, 10668 (1994).CrossRefADSGoogle Scholar
  62. 62.
    Baumbach G.T., Holy V., Pietsch U., Gailhanou M. The influence of specular interface reflection on grazing-incidence X-ray diffraction and diffuse-scattering from superlattices; Physica B 198, 249 (1994).CrossRefADSGoogle Scholar
  63. 63.
    Sanyal M.K., Sinha S.K., Gibaud A., Satija S.K., Majkrzak C.F., Homa H. Springer Proc. Phys. 61, 91 (1992).Google Scholar
  64. 64.
    Lekner J., In Theory of Reflection. Martinus Nijhoff Publishers, Dodrecht (1987).Google Scholar
  65. 65.
    Yoneda Y. Anomalous surface reflection of X-rays; Phys. Rev. 131, 2010 (1963).CrossRefADSGoogle Scholar
  66. 66.
    Aleksandrovic V., Greshnykh D., Randjelovic I., Frömsdorf A., Kornowski A., Roth S.V., Klinke C., Weller H. Preparation and Electrical Properties of Cobalt-Platinum Nanoparticle Monolayers Deposited by the Langmuir-Blodgett Technique; ACS Nano 2, 1123 (2008).CrossRefGoogle Scholar
  67. 67.
    Frömsdorf A., Capek R., Roth S.V. \(\mu\)-GISAXS experiment and simulation of a highly ordered model monolayer of PMMA-beads; J. Phys. Chem. B 110, 15166 (2006).Google Scholar
  68. 68.
    Müller-Buschbaum P., Gebhardt R., Maurer E., Bauer E., Gehrke R., Doster W. Thin casein films as prepared by spin-coating: Influence of film thickness and of pH; Biomacromolecules 7, 1773 (2006).CrossRefGoogle Scholar
  69. 69.
    Müller-Buschbaum P., Gebhardt R., Roth S.V., Metwalli E., Doster W. Effect of calcium concentration on the structure of casein micelles in thin films; Biophys. J. 93, 960 (2007).CrossRefGoogle Scholar
  70. 70.
    Perlich J., Schulz L., Abul Kashem M.M., Cheng Y.-J., Memesa M., Gutmann J.S., Roth S.V., Müller-Buschbaum P. Modification of the morphology of P(S-b-EO) templated thin TiO2 films by swelling with PS homopolymer; Langmuir 23, 10299 (2007).CrossRefGoogle Scholar
  71. 71.
    Lee B., Park I., Park H., Lo C.-T., Chang T., Winansa R.E. Electron density map using multiple scattering in grazing-incidence small-angle X-ray scattering; J. Appl. Cryst. 40, 496 (2007).CrossRefGoogle Scholar
  72. 72.
    Busch P., Krishnan S., Paik M., Toombes G.E.S., Smilgies D.-M., Gruner S.M., Ober C.K., Surface induced tilt propagation in thin films of semifluorinated liquid crystalline side chain block copolymers; Macromolecules 40, 81 (2007).CrossRefADSGoogle Scholar
  73. 73.
    Roth S.V., Döhrmann R., Dommach M., Kuhlmann M., Kröger I., Gehrke R., Walter H., Schroer C., Lengeler B., Müller-Buschbaum P. The small-angle options of the upgraded USAXS beamline BW4 at HASYLAB; Rev. Sci. Instr. 77, 085106 (2006).CrossRefADSGoogle Scholar
  74. 74.
    Kaune G., Ruderer M., Metwalli E., Wang W., Couet S., Schlage K., Röhlsberger R., Roth S.V., Müller-Buschbaum P. In-situ GISAXS study of gold film growth on conducting polymer films; ACS Applied Materials and Interfaces.(Submitted)Google Scholar

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© Springer-Verlag Berlin Heidelberg 2009

Authors and Affiliations

  1. 1.Physik-Department, LS E13Technische Universitüt München85748 GarchingGermany

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