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

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Applications of Synchrotron Light to Scattering and Diffraction in Materials and Life Sciences

Part of the book series: Lecture Notes in Physics ((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].

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Reference

  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. 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).

    Article  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  4. Salditt T., Metzger T.H., Peisl J., Jiang X. Diffuse X-ray scattering of amorphous multilayers; J. Phys. III 4, 1573 (1994).

    Article  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  12. Müller-Buschbaum P., Vanhoorne P., Scheumann V., Stamm M. Observation of nano-dewetting structures; Europhys. Lett. 40, 655 (1997).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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. 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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  Google Scholar 

  29. James R.W. The Optical Principles of the Diffraction of X-Rays. OxBow Press, Woodbridge Connecticut (1962).

    Google Scholar 

  30. Born M., Wolf E. Principles of Optics; 2nd ed., Pergamon Press, Oxford (1964).

    Google Scholar 

  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. Lazzari R. IsGISAXS: a program for grazing incidence small-angle X-ray scattering analysis for supported islands; J. Appl. Cryst. 35, 406 (2002).

    Article  Google Scholar 

  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. 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).

    Article  ADS  Google Scholar 

  35. Guinier A., Fournet G. Small-Angle Scattering of X-Rays. John Wiley & Sons, New York (1955).

    Google Scholar 

  36. Guinier A. X-Ray Diffraction in Crystals, Imperfect Crystals and Amorphous Bodies. Dover Publications, Inc, New York (1963).

    Google Scholar 

  37. Glatter G., Kratky O. Small Angle X-Ray Scattering. Academic Press (1982).

    Google Scholar 

  38. Kotlarchyk M., Chen S.-H. Analysis of small-angle scattering spectra from polydisperse interacting colloids; J. Chem. Phys. 79, 2461 (1983).

    Article  ADS  Google Scholar 

  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. 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).

    Article  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  44. Hosemann R., Vogel W., Weick D. Novel aspects of the real paracrystal; Acta. Cryst. A 37, 85 (1981).

    Article  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  Google Scholar 

  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. Lindner P., Zemb T. Neutrons, X-Rays and Light: Scattering Methods Applied to Soft Condensed matter. Elsevier, Amsterdam (2002).

    Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  60. Holy V., Kubuena J., Ohlidal I., Lischka K., Plotz W. X-ray reflection from rough layered systems; Phys. Rev. B 47, 15896 (1993).

    Article  ADS  Google Scholar 

  61. Holy V., Baumbach T. Non specular X-ray reflection from rough multilayers; Phys. Rev. B 49, 10668 (1994).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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. Lekner J., In Theory of Reflection. Martinus Nijhoff Publishers, Dodrecht (1987).

    Google Scholar 

  65. Yoneda Y. Anomalous surface reflection of X-rays; Phys. Rev. 131, 2010 (1963).

    Article  ADS  Google Scholar 

  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).

    Article  Google Scholar 

  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. 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).

    Article  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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).

    Article  ADS  Google Scholar 

  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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  1. Physik-Department, LS E13, Technische Universitüt München, James-Franck-Str.1, 85748 Garching, Germany

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    Müller-Buschbaum, P. (2009). A Basic Introduction to Grazing Incidence Small-Angle X-Ray Scattering. In: Gomez, M., Nogales, A., Garcia-Gutierrez, M., Ezquerra, T. (eds) Applications of Synchrotron Light to Scattering and Diffraction in Materials and Life Sciences. Lecture Notes in Physics, vol 776. Springer, Berlin, Heidelberg. https://doi.org/10.1007/978-3-540-95968-7_3

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