A simple formula for determining nanoparticle size distribution by combining small-angle X-ray scattering and diffraction results

Morelhão, Sérgio L.; Kycia, S.

doi:10.1107/s2053273322007215

Cited by 4 publications

(1 citation statement)

References 26 publications

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“…Specifically, through modeling of the G ( r ), accurate mean spherical nanoparticle diameters can be determined for each sample. Methods such as TEM images and Bragg diffraction can often under-represent smaller-sized particles [ 42 ]. For accurate size determination, the instrument broadening factors are first determined through G ( r ) modeling of a Sigma-Aldrich powdered diamond sample.…”

Section: Resultsmentioning

confidence: 99%

Mechanical Exfoliation of Expanded Graphite to Graphene-Based Materials and Modification with Palladium Nanoparticles for Hydrogen Storage

Chow,

Burns,

Boateng

et al. 2023

Nanomaterials

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Hydrogen is a promising green fuel carrier that can replace fossil fuels; however, its storage is still a challenge. Carbon-based materials with metal catalysts have recently been the focus of research for solid-state hydrogen storage due to their efficacy and low cost. Here, we report on the exfoliation of expanded graphite (EG) through high shear mixing and probe tip sonication methods to form graphene-based nanomaterial ShEG and sEG, respectively. The exfoliation processes were optimized based on electrochemical capacitance measurements. The exfoliated EG was further functionalized with palladium nanoparticles (Pd-NP) for solid-state hydrogen storage. The prepared graphene-based nanomaterials (ShEG and sEG) and the nanocomposites (Pd-ShEG and Pd-sEG) were characterized with various traditional techniques (e.g., SEM, TEM, EDX, XPS, Raman, XRD) and the advanced high-resolution pair distribution function (HRPDF) analysis. Electrochemical hydrogen uptake and release (QH) were measured, showing that the sEG decorated with Pd-NP (Pd-sEG, 31.05 mC cm−2) and ShEG with Pd-NP (Pd-ShEG, 24.54 mC cm−2) had a notable improvement over Pd-NP (9.87 mC cm−2) and the composite of Pd-EG (14.7 mC cm−2). QH showed a strong linear relationship with an effective surface area to volume ratio, indicating nanoparticle size as a determining factor for hydrogen uptake and release. This work is a promising step toward the design of the high-performance solid-state hydrogen storage devices through mechanical exfoliation of the substrate EG to control nanoparticle size and dispersion.

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Section: Resultsmentioning

confidence: 99%

Mechanical Exfoliation of Expanded Graphite to Graphene-Based Materials and Modification with Palladium Nanoparticles for Hydrogen Storage

Chow,

Burns,

Boateng

et al. 2023

Nanomaterials

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Synthesis of Novel [CdO(75%)/VO2(20%)/SiC(4%):p-Si] Heterojunction Composite Thin Films Decorated with Chlorophyll using Solvothermal-Laser Dual Technique for Solar Cell Applications

Najm,

Alshrefi,

Hadi

et al. 2024

Silicon

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Implications of size dispersion on X-ray scattering of crystalline nanoparticles: CeO₂ as a case study

Valério,

Trindade,

Penacchio

et al. 2024

J Appl Cryst

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Controlling the shape and size dispersivity and crystallinity of nanoparticles (NPs) has been a challenge in identifying these parameters' role in the physical and chemical properties of NPs. The need for reliable quantitative tools for analyzing the dispersivity and crystallinity of NPs is a considerable problem in optimizing scalable synthesis routes capable of controlling NP properties. The most common tools are electron microscopy (EM) and X-ray scattering techniques. However, each technique has different susceptibility to these parameters, implying that more than one technique is necessary to characterize NP systems with maximum reliability. Wide-angle X-ray scattering (WAXS) is mandatory to access information on crystallinity. In contrast, EM or small-angle X-ray scattering (SAXS) is required to access information on whole NP sizes. EM provides average values on relatively small ensembles in contrast to the bulk values accessed by X-ray techniques. Besides the fact that the SAXS and WAXS techniques have different susceptibilities to size distributions, SAXS is easily affected by NP–NP interaction distances. Because of all the variables involved, there have yet to be proposed methodologies for cross-analyzing data from two techniques that can provide reliable quantitative results of dispersivity and crystallinity. In this work, a SAXS/WAXS-based methodology is proposed for simultaneously quantifying size distribution and degree of crystallinity of NPs. The most reliable easy-to-access size result for each technique is demonstrated by computer simulation. Strategies on how to compare these results and how to identify NP–NP interaction effects underneath the SAXS intensity curve are presented. Experimental results are shown for cubic-like CeO2 NPs. WAXS size results from two analytical procedures are compared, line-profile fitting of individual diffraction peaks in opposition to whole pattern fitting. The impact of shape dispersivity is also evaluated. Extension of the proposed methodology for cross-analyzing EM and WAXS data is possible.

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A simple formula for determining nanoparticle size distribution by combining small-angle X-ray scattering and diffraction results

Cited by 4 publications

References 26 publications

Mechanical Exfoliation of Expanded Graphite to Graphene-Based Materials and Modification with Palladium Nanoparticles for Hydrogen Storage

Mechanical Exfoliation of Expanded Graphite to Graphene-Based Materials and Modification with Palladium Nanoparticles for Hydrogen Storage

Synthesis of Novel [CdO(75%)/VO2(20%)/SiC(4%):p-Si] Heterojunction Composite Thin Films Decorated with Chlorophyll using Solvothermal-Laser Dual Technique for Solar Cell Applications

Implications of size dispersion on X-ray scattering of crystalline nanoparticles: CeO₂ as a case study

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A simple formula for determining nanoparticle size distribution by combining small-angle X-ray scattering and diffraction results

Cited by 4 publications

References 26 publications

Mechanical Exfoliation of Expanded Graphite to Graphene-Based Materials and Modification with Palladium Nanoparticles for Hydrogen Storage

Mechanical Exfoliation of Expanded Graphite to Graphene-Based Materials and Modification with Palladium Nanoparticles for Hydrogen Storage

Synthesis of Novel [CdO(75%)/VO2(20%)/SiC(4%):p-Si] Heterojunction Composite Thin Films Decorated with Chlorophyll using Solvothermal-Laser Dual Technique for Solar Cell Applications

Implications of size dispersion on X-ray scattering of crystalline nanoparticles: CeO2 as a case study

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Implications of size dispersion on X-ray scattering of crystalline nanoparticles: CeO₂ as a case study