Grazing‐incidence transmission X‐ray scattering: surface scattering in the Born approximation

Determination of the three-dimensional order in thin nanostructured films remains challenging. Real-space imaging methods, including electron microscopies and scanning-probe methods, have difficulty reconstructing the depth of a film and suffer from limited statistical sampling. X-ray and neutron scattering have emerged as powerful complementary techniques but have substantial data collection and analysis challenges. This article describes a new method, grazing-incidence transmission small-angle X-ray scattering, which allows for fast scattering measurements that are not burdened by the refraction and reflection effects that have to date plagued grazing-incidence X-ray scattering. In particular, by arranging a sample/beam geometry wherein the scattering exits through the edge of the substrate, it is possible to record scattering images that are well described by straightforward (Born approximation) scattering models.

[1]  Wen-li Wu,et al.  Small Angle X-Ray Scattering for Sub-100 nm Pattern Characterization , 2003 .

[2]  Mean-field theory of light scattering by one-dimensional rough surfaces , 1998 .

[3]  Detlef-M. Smilgies,et al.  Grazing‐incidence small‐angle X‐ray scattering from thin polymer films with lamellar structures – the scattering cross section in the distorted‐wave Born approximation , 2006 .

[4]  D.K.G. De Boer X-RAY SCATTERING AND X-RAY FLUORESCENCE FROM MATERIALS WITH ROUGH INTERFACES , 1996 .

[5]  Spohn,et al.  Small-angle x-ray scattering under grazing incidence: The cross section in the distorted-wave Born approximation. , 1995, Physical review. B, Condensed matter.

[6]  M. Burghammer,et al.  In situ observation of nanoparticle ordering at the air-water-substrate boundary in colloidal solutions using x-ray nanobeams , 2007 .

[7]  S. Darling,et al.  Nanoscopic Patterned Materials with Tunable Dimensions via Atomic Layer Deposition on Block Copolymers , 2010, Advanced materials.

[8]  Zhiping Luo,et al.  Reversible Kirkwood-Alder transition observed in Pt3Cu2 nanoctahedron assemblies under controlled solvent annealing/drying conditions. , 2012, Journal of the American Chemical Society.

[9]  Charles T. Black,et al.  Plasma etch transfer of self-assembled polymer patterns , 2012, Advanced Lithography.

[10]  Sirota,et al.  X-ray and neutron scattering from rough surfaces. , 1988, Physical review. B, Condensed matter.

[11]  B. Ocko,et al.  Grazing incident small angle x-ray scattering: A metrology to probe nanopatterned surfaces , 2009 .

[12]  Paulette Clancy,et al.  Shape-anisotropy driven symmetry transformations in nanocrystal superlattice polymorphs. , 2011, ACS nano.

[13]  M. A. Kashem,et al.  In situ observation of cluster formation during nanoparticle solution casting on a colloidal film , 2011, Journal of physics. Condensed matter : an Institute of Physics journal.

[14]  K. Yager,et al.  Nanoimprint-induced molecular orientation in semiconducting polymer nanostructures. , 2011, ACS nano.

[15]  G. Renaud,et al.  Probing surface and interface morphology with Grazing Incidence Small Angle X-Ray Scattering , 2009 .

[16]  Jerome B. Cohen,et al.  Grazing-incidence small-angle X-ray scattering: new tool for studying thin film growth , 1989 .

[17]  T. Emrick,et al.  Nanoparticle assembly at fluid interfaces: structure and dynamics. , 2005, Langmuir : the ACS journal of surfaces and colloids.

[18]  Chieh-Tsung Lo,et al.  Electron density map using multiple scattering in grazing-incidence small-angle X-ray scattering , 2007 .

[19]  W. L. Wu,et al.  Small Angle X-Ray Scattering Metrology for Sidewall Angle and Cross Section of Nanometer Scale Line Gratings , 2004 .

[20]  Dmitri V Talapin,et al.  Self-assembly of PbTe quantum dots into nanocrystal superlattices and glassy films. , 2006, Journal of the American Chemical Society.

[21]  Y. Yoneda,et al.  Anomalous Surface Reflection of X Rays , 1963 .

[22]  C Jeffrey Brinker,et al.  Peering into the self-assembly of surfactant templated thin-film silica mesophases. , 2003, Journal of the American Chemical Society.

[23]  G. G. Stokes "J." , 1890, The New Yale Book of Quotations.

[24]  B. Korgel,et al.  Stacking of hexagonal nanocrystal layers during Langmuir-Blodgett deposition. , 2012, The journal of physical chemistry. B.

[25]  B. Ocko,et al.  Water-vapor-assisted nanoimprinting of PEDOT:PSS thin films. , 2012, Small.

[26]  Manfred Burghammer,et al.  Self-assembled gradient nanoparticle-polymer multilayers investigated by an advanced characterization method: microbeam grazing incidence x-ray scattering , 2003 .

[27]  Ignaz Eisele,et al.  Grazing incidence small angle x-ray scattering from free-standing nanostructures , 1999 .

[28]  S. Narayanan,et al.  Waveguide-enhanced grazing-incidence small-angle x-ray scattering of buried nanostructures in thin films , 2011 .

[29]  Benjamin D. Hamilton,et al.  Simulation and interpretation of 2D diffraction patterns from self-assembled nanostructured films at arbitrary angles of incidence: from grazing incidence (above the critical angle) to transmission perpendicular to the substrate. , 2006, The journal of physical chemistry. B.

[30]  G. Renaud,et al.  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 , 2007 .

[31]  B. Korgel,et al.  GISAXS Characterization of Order in Hexagonal Monolayers of FePt Nanocrystals , 2010 .

[32]  Minhao Yan,et al.  On the intersection of grating truncation rods with the Ewald sphere studied by grazing‐incidence small‐angle X‐ray scattering , 2007 .

[33]  C. Hawker,et al.  Controlling Polymer-Surface Interactions with Random Copolymer Brushes , 1997, Science.

[34]  P. Müller‐Buschbaum,et al.  Debye–Scherrer rings from block copolymer films with powder-like order , 2011 .

[35]  B. Borie X-Ray Diffraction in Crystals, Imperfect Crystals, and Amorphous Bodies. , 1965 .

[36]  Soojin Park,et al.  Macroscopic 10-Terabit–per–Square-Inch Arrays from Block Copolymers with Lateral Order , 2009, Science.

[37]  G. Vineyard,et al.  Grazing-incidence diffraction and the distorted-wave approximation for the study of surfaces , 1982 .

[38]  M. Burghammer,et al.  Colloidal silver nanoparticle gradient layer prepared by drying between two walls of different wettability , 2009, Journal of physics. Condensed matter : an Institute of Physics journal.

[39]  Kathryn W. Guarini,et al.  Optimization of diblock copolymer thin film self assembly , 2002 .

[40]  Francesc Pérez-Murano,et al.  Grazing-incidence small-angle X-ray scattering of soft and hard nanofabricated gratings , 2012 .

[41]  C. Stafford,et al.  Nanoscopic Templates from Oriented Block Copolymer Films , 2000 .

[42]  Kwang-Woo Kim,et al.  Structural Analysis of Block Copolymer Thin Films with Grazing Incidence Small-Angle X-ray Scattering , 2005 .

[43]  Dorthe Posselt,et al.  Structural instabilities in lamellar diblock copolymer thin films during solvent vapor uptake. , 2008, Langmuir : the ACS journal of surfaces and colloids.