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Nanomaterials
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Total Scattering Based Characterization Techniques for Nanostructures
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Total Scattering Based Characterization Techniques for Nanostructures

A special issue of Nanomaterials (ISSN 2079-4991). This special issue belongs to the section "Synthesis, Interfaces and Nanostructures".

Deadline for manuscript submissions: closed (31 December 2022) | Viewed by 10562

Special Issue Editors

Dr. Antonietta Guagliardi

E-Mail Website
Guest Editor
Consiglio Nazionale delle Ricerche, Istituto di Cristallografia, via Valleggio 11, 22100 Como, Italy
Interests: Nanocrystallography, Structure, Defects, Strain, Size, Morphological and Surface characterization of nanocrystals (NCs), nanostructures, nanocomposites, multi-scale systems and disordered materials; X-ray Total scattering methods (WAXTS, SAXS); Debye Scattering Equation; Structure-property correlations at the nanoscale; WAXTS experiments at Large Scale Facilities; development of protocols for WAXTS data collection, reduction and analysis; classes of nano/defective materials investigated through suitably developed atomistic models: metals, oxides, semiconductors, quantum dots, bioceramics, nanocomposites, coordination polymers, pharmaceuticals
Dr. Federica Bertolotti

E-Mail Website
Guest Editor
Dipartimento di Scienza e Alta Tecnologia, Università dell’Insubria, via Valleggio 11, 22100 Como, Italy
Interests: total scattering methods; debye-scattering equation; synchrotron techniques; structural disorder and defectiveness; solid state chemistry; nanomaterials; colloidal quantum dots

Special Issue Information

Dear Colleagues,

Recent advances in Nanoscience and Nanotechnology have pushed the frontier of next-generation nanostructures towards a high level of structural complexity. Engineering and controlling such complexity with atomic and nanometer precision are crucial in order to enhance the material properties and improve the fabrication methods. Nonetheless, characterizing these complex nanostructures remains a challenging task. 

Scattering techniques based on X-ray, neutron, visible light sources, and experiments in reciprocal space are powerful and highly versatile tools to the scope. The different techniques span the small and wide-angle scattering regions and, depending on the different length scales being probed, provide different and complementary information encompassing the atomic, nanometer and micrometer scales. Experiments can be performed by irradiating dry powders and colloidal suspension of nanoparticles (enabling statistically robust analysis of the distribution properties of the ensemble), in grazing incidence mode (to investigate thin films prepared by cheap solution-based processes) and in scanning mode (providing spatially resolved properties of laterally extended systems). Brilliant sources and efficient detectors allow fast scattering data acquisition enabling time-dependent changes to be monitored within in-situ/in-operando experiments.

Within this reach scenario, this special issue welcomes, but not limits to, contributions that focus on the different scattering techniques and investigate technologically appealing nanostructures in terms of their crystal structure and atomic-scale defectiveness, local short-range vs long-range order, lattice strain and compositional inhomogeneity/gradients in core-shell and core-crown systems; determination of nanocrystals/nanoparticle size, shape, surface and faceting; investigation of supramolecular order, 3D/2D self-assembled superlattices and thin films nanostructures.

This special issue is open to research papers and review articles covering the latest trends related to nanostructures characterization through scattering techniques, and wants to provide the readers with a clear overview of the recent advances in scattering methodologies.

Dr. Antonietta Guagliardi
Dr. Federica Bertolotti
Guest Editors

Manuscript Submission Information

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Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Nanomaterials is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2900 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • wide angle scattering
  • small angle scattering
  • X-ray scattering
  • neutron scattering
  • dynamic light scattering
  • static light scattering
  • grazing incidence
  • scanning techniques
  • pair distribution function
  • debye scattering equation
  • short range order
  • particle sizing/shaping
  • nanocrystals structure
  • surface relaxation
  • nanocrystals faceting
  • structural defects
  • static disorder
  • dynamic disorder
  • superlattices
  • thin films
  • in situ scattering experiments
  • in operando scattering experiments
  • time-resolved scattering experiments
  • spatial-resolved scattering experiments

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Published Papers (6 papers)

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Research

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25 pages, 3702 KiB  
Article
Structure and Surface Relaxation of CeO2 Nanoparticles Unveiled by Combining Real and Reciprocal Space Total Scattering Analysis
by Marco Scavini, Federica Bertolotti, Jonadri Mlloja, Filippo Umbri, Anna Bosc, Serena Cappelli, Stefano Checchia, Cesare Oliva, Patrizia Fumagalli, Davide Ceresoli, Mariangela Longhi, Antonietta Guagliardi and Mauro Coduri
Nanomaterials 2022, 12(19), 3385; https://doi.org/10.3390/nano12193385 - 27 Sep 2022
Cited by 3 | Viewed by 2461
Abstract
We present a combined real and reciprocal space structural and microstructural characterization of CeO2 nanoparticles (NPs) exhibiting different crystallite sizes; ~3 nm CeO2 NPs were produced by an inverse micellae wet synthetic path and then annealed at different temperatures. X-ray total [...] Read more.
We present a combined real and reciprocal space structural and microstructural characterization of CeO2 nanoparticles (NPs) exhibiting different crystallite sizes; ~3 nm CeO2 NPs were produced by an inverse micellae wet synthetic path and then annealed at different temperatures. X-ray total scattering data were analyzed by combining real-space-based Pair Distribution Function analysis and the reciprocal-space-based Debye Scattering Equation method with atomistic models. Subtle atomic-scale relaxations occur at the nanocrystal surface. The structural analysis was corroborated by ab initio DFT and force field calculations; micro-Raman and electron spin resonance added important insights to the NPs’ defective structure. The combination of the above techniques suggests a core-shell like structure of ultrasmall NPs. These exhibit an expanded outer shell having a defective fluorite structure, while the inner shell is similar to the bulk structure. The presence of partially reduced O2−δ species testifies to the high surface activity of the NPs. On increasing the annealing temperature, the particle dimensions increase, limiting disorder as a consequence of the progressive surface-to-volume ratio reduction. Full article
(This article belongs to the Special Issue Total Scattering Based Characterization Techniques for Nanostructures)
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17 pages, 1369 KiB  
Article
Diffraction from Nanocrystal Superlattices
by Antonio Cervellino and Ruggero Frison
Nanomaterials 2022, 12(10), 1781; https://doi.org/10.3390/nano12101781 - 23 May 2022
Viewed by 1822
Abstract
Diffraction from a lattice of periodically spaced crystals is a topic of current interest because of the great development of self-organised superlattices (SL) of nanocrystals (NC). The self-organisation of NC into SL has theoretical interest, but especially a rich application prospect, as the [...] Read more.
Diffraction from a lattice of periodically spaced crystals is a topic of current interest because of the great development of self-organised superlattices (SL) of nanocrystals (NC). The self-organisation of NC into SL has theoretical interest, but especially a rich application prospect, as the coherent organisation has large effects on a wide range of material properties. Diffraction is a key method to understand the type and quality of SL ordering. Hereby, the characteristic diffraction signature of an SL of NC—together with the characteristic types of disorder—are theoretically explored. Full article
(This article belongs to the Special Issue Total Scattering Based Characterization Techniques for Nanostructures)
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17 pages, 4001 KiB  
Article
Effects of Structural and Microstructural Features on the Total Scattering Pattern of Nanocrystalline Materials
by Nicola Dengo, Norberto Masciocchi, Antonio Cervellino, Antonietta Guagliardi and Federica Bertolotti
Nanomaterials 2022, 12(8), 1252; https://doi.org/10.3390/nano12081252 - 7 Apr 2022
Cited by 3 | Viewed by 2024
Abstract
Atomic- and nanometer-scale features of nanomaterials have a strong influence on their chemical and physical properties and a detailed description of these elements is a crucial step in their characterization. Total scattering methods, in real and reciprocal spaces, have been established as fundamental [...] Read more.
Atomic- and nanometer-scale features of nanomaterials have a strong influence on their chemical and physical properties and a detailed description of these elements is a crucial step in their characterization. Total scattering methods, in real and reciprocal spaces, have been established as fundamental techniques to retrieve this information. Although the impact of microstructural features, such as defectiveness of different kinds, has been extensively studied in reciprocal space, disentangling these effects from size- and morphology-induced properties, upon downsizing, is not a trivial task. Additionally, once the experimental pattern is Fourier transformed to calculate the pair distribution function, the direct fingerprint of structural and microstructural features is severely lost and no modification of the histogram of interatomic distances derived therefrom is clearly discussed nor considered in the currently available protocols. Hereby, starting from atomistic models of a prototypical system (cadmium selenide), we simulate multiple effects on the atomic pair distribution function, obtained from reciprocal space patterns computed through the Debye scattering equation. Size and size dispersion effects, as well as different structures, morphologies, and their interplay with several kinds of planar defects, are explored, aiming at identifying the main (measurable and informative) fingerprints of these features on the total scattering pattern in real and reciprocal spaces, highlighting how, and how much, they become evident when comparing different cases. The results shown herein have general validity and, as such, can be further extended to other classes of nanomaterials. Full article
(This article belongs to the Special Issue Total Scattering Based Characterization Techniques for Nanostructures)
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21 pages, 2616 KiB  
Article
An Atomistic Model Describing the Structure and Morphology of Cu-Doped C-S-H Hardening Accelerator Nanoparticles
by Gregorio Dal Sasso, Maria Chiara Dalconi, Giorgio Ferrari, Jan Skov Pedersen, Sergio Tamburini, Federica Bertolotti, Antonietta Guagliardi, Marco Bruno, Luca Valentini and Gilberto Artioli
Nanomaterials 2022, 12(3), 342; https://doi.org/10.3390/nano12030342 - 21 Jan 2022
Cited by 14 | Viewed by 3769
Abstract
Calcium silicate hydrate (C-S-H) is the main binding phase in Portland cement. The addition of C-S-H nanoparticles as nucleation seeds has successfully been used to accelerate the hydration process and the precipitation of binding phases either in conventional Portland cement or in alternative [...] Read more.
Calcium silicate hydrate (C-S-H) is the main binding phase in Portland cement. The addition of C-S-H nanoparticles as nucleation seeds has successfully been used to accelerate the hydration process and the precipitation of binding phases either in conventional Portland cement or in alternative binders. Indeed, the modulation of the hydration kinetics during the early-stage dissolution-precipitation reactions, by acting on the nucleation and growth of binding phases, improves the early strength development. The fine-tuning of concrete properties in terms of compressive strength and durability by designed structural modifications can be achieved through the detailed description of the reaction products at the atomic scale. The nano-sized, chemically complex and structurally disordered nature of these phases hamper their thorough structural characterization. To this aim, we implement a novel multi-scale approach by combining forefront small-angle X-ray scattering (SAXS) and synchrotron wide-angle X-ray total scattering (WAXTS) analyses for the characterization of Cu-doped C-S-H nanoparticles dispersed in a colloidal suspension, used as hardening accelerator. SAXS and WAXTS data were analyzed under a unified modeling approach by developing suitable atomistic models for C-S-H nanoparticles to be used to simulate the experimental X-ray scattering pattern through the Debye scattering equation. The optimization of atomistic models against the experimental pattern, together with complementary information on the structural local order from 29Si solid-state nuclear magnetic resonance and X-ray absorption spectroscopy, provided a comprehensive description of the structure, size and morphology of C-S-H nanoparticles from the atomic to the nanometer scale. C-S-H nanoparticles were modeled as an assembly of layers composed of 7-fold coordinated Ca atoms and decorated by silicate dimers and chains. The structural layers are a few tens of nanometers in length and width, with a crystal structure resembling that of a defective tobermorite, but lacking any ordering between stacking layers. Full article
(This article belongs to the Special Issue Total Scattering Based Characterization Techniques for Nanostructures)
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20 pages, 7611 KiB  
Article
Highly Stable Thin Films Based on Novel Hybrid 1D (PRSH)PbX3 Pseudo-Perovskites
by Gabriele Calabrese, Candida Pipitone, Diego Marini, Francesco Giannici, Antonino Martorana, Luisa Barba, Caterina Summonte, Norberto Masciocchi and Silvia Milita
Nanomaterials 2021, 11(10), 2765; https://doi.org/10.3390/nano11102765 - 19 Oct 2021
Cited by 1 | Viewed by 2245
Abstract
In this study, the structure and morphology, as well as time, ultraviolet radiation, and humidity stability of thin films based on newly developed 1D (PRSH)PbX3 (X = Br, I) pseudo-perovskite materials, containing 1D chains of face-sharing haloplumbate octahedra, are investigated. All films [...] Read more.
In this study, the structure and morphology, as well as time, ultraviolet radiation, and humidity stability of thin films based on newly developed 1D (PRSH)PbX3 (X = Br, I) pseudo-perovskite materials, containing 1D chains of face-sharing haloplumbate octahedra, are investigated. All films are strongly crystalline already at room temperature, and annealing does not promote further crystallization or film reorganization. The film microstructure is found to be strongly influenced by the anion type and, to a lesser extent, by the DMF/DMSO solvent volume ratio used during film deposition by spin-coating. Comparison of specular X-ray diffraction and complementary grazing incidence X-ray diffraction analysis indicates that the use of DMF/DMSO mixed solvents promotes the strengthening of a dominant 100 or 210 texturing, as compared the case of pure DMF, and that the haloplumbate chains always lie in a plane parallel to the substrate. Under specific DMF/DMSO solvent volume ratios, the prepared films are found to be highly stable in time (up to seven months under fluxing N2 and in the dark) and to highly moist conditions (up to 25 days at 78% relative humidity). Furthermore, for representative (PRSH)PbX3 films, resistance against ultraviolet exposure (λ = 380 nm) is investigated, showing complete stability after irradiation for up to 15 h at a power density of 600 mW/cm2. These results make such thin films interesting for highly stable perovskite-based (opto)electronic devices. Full article
(This article belongs to the Special Issue Total Scattering Based Characterization Techniques for Nanostructures)
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Review

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23 pages, 4497 KiB  
Review
Light Scattering and Turbidimetry Techniques for the Characterization of Nanoparticles and Nanostructured Networks
by Pietro Anzini, Daniele Redoglio, Mattia Rocco, Norberto Masciocchi and Fabio Ferri
Nanomaterials 2022, 12(13), 2214; https://doi.org/10.3390/nano12132214 - 28 Jun 2022
Cited by 6 | Viewed by 2780
Abstract
Light scattering and turbidimetry techniques are classical tools for characterizing the dynamics and structure of single nanoparticles or nanostructured networks. They work by analyzing, as a function of time (Dynamic Light Scattering, DLS) or angles (Static Light Scattering, SLS), the light scattered by [...] Read more.
Light scattering and turbidimetry techniques are classical tools for characterizing the dynamics and structure of single nanoparticles or nanostructured networks. They work by analyzing, as a function of time (Dynamic Light Scattering, DLS) or angles (Static Light Scattering, SLS), the light scattered by a sample, or measuring, as a function of the wavelength, the intensity scattered over the entire solid angle when the sample is illuminated with white light (Multi Wavelength Turbidimetry, MWT). Light scattering methods probe different length scales, in the ranges of ~5–500 nm (DLS), or ~0.1–5 μm (Wide Angle SLS), or ~1–100 μm (Low Angle SLS), and some of them can be operated in a time-resolved mode, with the possibility of characterizing not only stationary, but also aggregating, polymerizing, or self-assembling samples. Thus, the combined use of these techniques represents a powerful approach for studying systems characterized by very different length scales. In this work, we will review some typical applications of these methods, ranging from the field of colloidal fractal aggregation to the polymerization of biologic networks made of randomly entangled nanosized fibers. We will also discuss the opportunity of combining together different scattering techniques, emphasizing the advantages of a global analysis with respect to single-methods data processing. Full article
(This article belongs to the Special Issue Total Scattering Based Characterization Techniques for Nanostructures)
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