Exploiting GISAXS for the Study of a 3D Ordered Superlattice of Self-Assembled Colloidal Iron Oxide Nanocrystals

Altamura, Davide; Holý, V.; Siliqi, Dritan; Lekshmi, I.C.; Nobile, Concetta; Maruccio, Giuseppe; Cozzoli, P. Davide; Fan, Lixin; Gozzo, F.; Giannini, Cinzia

doi:10.1021/cg3010739

Cited by 22 publications

(29 citation statements)

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“…Remarkably, both substrate surface chemistry and size monodispersity of the nanostructures were revealed to be decisive in controlling the extent of the superlattice. [70,71]. Figure 9d shows a cone-shaped island made of iron oxide nanocrystals self-assembled by a magnetic field onto a silicon substrate [71].…”

Section: Nano-structured Surfacesmentioning

confidence: 99%

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X-ray Diffraction: A Powerful Technique for the Multiple-Length-Scale Structural Analysis of Nanomaterials

et al. 2016

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During recent decades innovative nanomaterials have been extensively studied, aiming at both investigating the structure-property relationship and discovering new properties, in order to achieve relevant improvements in current state-of-the art materials. Lately, controlled growth and/or assembly of nanostructures into hierarchical and complex architectures have played a key role in engineering novel functionalized materials. Since the structural characterization of such materials is a fundamental step, here we discuss X-ray scattering/diffraction techniques to analyze inorganic nanomaterials under different conditions: dispersed in solutions, dried in powders, embedded in matrix, and deposited onto surfaces or underneath them.

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Section: Nano-structured Surfacesmentioning

confidence: 99%

“…[70,71]. Figure 9d shows a cone-shaped island made of iron oxide nanocrystals self-assembled by a magnetic field onto a silicon substrate [71]. A section of the island, imaged by SEM, revealed a three-dimensional (3D) ordered superlattice, whose lattice symmetry cannot be retrieved from the SEM data in Figure 9d.…”

Section: Nano-structured Surfacesmentioning

confidence: 99%

X-ray Diffraction: A Powerful Technique for the Multiple-Length-Scale Structural Analysis of Nanomaterials

et al. 2016

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“…The data were analysed against a new theoretical model 59 (see the calculated map in Figure 12b), as the applicability of software available for the fitting of the whole GISAXS intensity, up to recently, has been either restricted to 2D in-plane assemblies of particles (IsGISAXS), 61 limited to the calculation and indexing of the expected diffraction spot positions (NANOCELL) 62 or devoted to particular types of samples -e.g., with thin film morphology and flat interfaces (NANODIFT). For this study, a new program has been implemented for simulating and fitting GISAXS data collected from compact 3D assemblies.…”

Section: Gisaxs -3d Self-assembly Of Iron Oxide Ncs 59mentioning

confidence: 99%

Assembled Nanostructured Architectures Studied by Grazing Incidence X-Ray Scattering

Altamura

Sibillano

Siliqi

et al. 2012

Nanomaterials and Nanotechnology

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In this chapter, we will focus on a specific X-raybased technique among those employed in surface science and which is especially suitable for the study of self-assembled nanocrystals: Grazing Incidence Small Angle X-ray Scattering (GISAXS). We will first introduce the main field of investigation considered herein, with basic notions of X-ray scattering from surfaces, and then address basic concepts about GISAXS. Finally, we will describe a few relevant examples of studies, of nanostructured architectures, through ex situ and in situ experiments of grazing incidence X-ray scattering. This manuscript is focused on the former, showing that they can be performed by using laboratory instruments. In situ investigations still need synchrotron radiation sources in most cases; therefore, only a few examples selected from the literature are reported here, for the sake of completeness. The experiments described are mainly performed in the small angle range, providing information on the size and shape of nanocrystals, together with their spatial arrangement. Both 2D and 3D architectures are considered. In particular, GISAXS measurements of 2D superlattices of nano-octapods, performed both at a third generation synchrotron beamline and with a table-top set-up, are compared; the employed table-top set-up is described in a dedicated paragraph. Further examples of grazing incidence studies as performed by the authors with a table-top set-up are reported: a GISAXS study of 3D iron oxide nanocrystal superlattices, showing the importance of modelling in order to obtain structural information from data; a combined small/wide angle scattering (GISAXS/GIWAXS) study of 3D PbS nanocrystal superlattices; and a GIWAXS study of P3HT nanofibres, showing how the ordering at the molecular and atomic length scales can be obtained by exploring different angular ranges in the same grazing incidence geometry. Finally, selected examples of in situ GISAXS studies, performed with synchrotron radiation sources, are described.

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“…In the former, position of a nanoparticle is derived from the ideal site in a perfectly ordered crystal lattice while in the latter, it is derived from the positions of the neighboring nanoparticles . It has been well‐evidenced that spontaneous nanoparticle self‐assembly is characterized by cumulative disorder resulting in the short‐range order . The short‐range order was also extensively demonstrated in polymers, glasses and alloys .…”

Section: Introductionmentioning

confidence: 99%

“…Other possibilities of the nanoparticle ordering including stacking faults, twin planes or transition to a fully disordered state would require another approach. In particular, the models allowing simulation of the disordered state were published recently and were successfully applied to quantum dots and iron oxide nanoparticles . Here, the GISAXS patterns are simulated by Monte Carlo method while our model based on 3D ideal paracrystal is semi‐analytical by nature.…”

Section: Introductionmentioning

confidence: 99%

Application of the paracrystal model to GISAXS analysis of the 3D self-assembled nanoparticle crystals

Végsö

Šiffalovič

Jergel

et al. 2014

Phys. Status Solidi B

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An original diffraction model for the evaluation of the grazing‐incidence small‐angle X‐ray scattering (GISAXS) of the three‐dimensional (3D) supported self‐assembled nanoparticle crystals is presented. The model utilizes the formalism of traditional crystallography that is applied to nanoparticles as scattering entities. The infinite paracrystal concept was adopted in order to include cumulative disorder that is typical for the self‐assembled nanoparticle structures. Azimuthal averaging around a chosen crystallographic direction allows incorporation of texture effects. A transformation of the SAXS paracrystal equations to comply with the GISAXS geometry was employed to describe the scattering process in the limit of the kinematical approximation which facilitates calculations. The model was developed for the face‐centered cubic (FCC) symmetry, however, its extension to any other cubic symmetry is straightforward. The model was tested on a 3D nanoparticle assembly formed on silicon from a dried drop‐cast colloidal solution of monodisperse silver nanoparticles of 5.8 ± 0.6 nm diameter. Presence of the FCC nanoparticle crystal with the [111] texture along the substrate normal was evidenced from evaluation of the synchrotron GISAXS data. The degree of paracrystal disorder is 2.5% and 3.6% parallel and perpendicular to the substrate, respectively, suggesting the anisotropic character of the self‐assembling process. A SAXS measurement of the nanoparticle crystal formed from the same solution in a capillary revealed a randomly oriented FCC structure with a slightly larger paracrystal disorder of 4%. Obviously, different conditions of the nanoparticle crystal formation affect its azimuthal and translational disorder.

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Exploiting GISAXS for the Study of a 3D Ordered Superlattice of Self-Assembled Colloidal Iron Oxide Nanocrystals

Cited by 22 publications

References 29 publications

X-ray Diffraction: A Powerful Technique for the Multiple-Length-Scale Structural Analysis of Nanomaterials

X-ray Diffraction: A Powerful Technique for the Multiple-Length-Scale Structural Analysis of Nanomaterials

Assembled Nanostructured Architectures Studied by Grazing Incidence X-Ray Scattering

Application of the paracrystal model to GISAXS analysis of the 3D self-assembled nanoparticle crystals

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