Small-Angle Neutron Scattering for Cultural Heritage Studies

Len, Adél; Bajnok, Katalin; Füzi, János

doi:10.1007/978-3-030-60016-7_8

Cited by 6 publications

(3 citation statements)

References 17 publications

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“…Small-angle neutron scattering measurements were performed on the Yellow Submarine instrument located at BNC in Budapest (Hungary) [61,62]. A collimation distance of 5 m and circular beam apertures of 25 and 7 mm in diameter defined the incoming beam divergence, while sample to detector distances of 1.2 and 5.5 m and neutron wavelengths of 0.63 nm defined the range of momentum transfer q = (4π/λ)sin(θ/2) = 0.06-3.1 nm −1 .…”

Section: Small-angle Neutron Scatteringmentioning

confidence: 99%

Design of Nickel-Containing Nanocomposites Based on Ordered Mesoporous Silica: Synthesis, Structure, and Methylene Blue Adsorption

Kouznetsova,

Ivanets,

Prozorovich

et al. 2024

Gels

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Mesoporous materials containing heteroelements have a huge potential for use as catalysts, exchangers, and adsorbents due to their tunable nanometer-sized pores and exceptionally large internal surfaces accessible to bulky organic molecules. In the present work, ordered mesoporous silica containing Ni atoms as active sites was synthesized by a new low-temperature method of condensation of silica precursors on a micellar template from aqueous solutions in the presence of nickel salt. The homogeneity of the resulting product was achieved by introducing ammonia and ammonium salt as a buffer to maintain a constant pH value. The obtained materials were characterized by nitrogen sorption, X-ray and neutron diffraction, scanning electron microscopy, infrared spectroscopy, and thermal analysis. Their morphology consists of polydisperse spherical particles 50–300 nm in size, with a hexagonally ordered channel structure, high specific surface area (ABET = 900–1200 m2/g), large pore volume (Vp = 0.70–0.90 cm3/g), average mesopore diameter of about 3 nm, and narrow pore size distribution. Adsorption tests for methylene blue show sorption capacities reaching 39–42 mg/g at alkaline pH. The advantages of producing nickel silicates by this method, in contrast to precipitation from silicon alkoxides, are the low cost of reagents, fire safety, room-temperature processing, and the absence of specific problems associated with the use of ethanol as a solvent, as well as the absence of the inevitable capture of organic matter in the precipitation process.

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Section: Small-angle Neutron Scatteringmentioning

confidence: 99%

Design of Nickel-Containing Nanocomposites Based on Ordered Mesoporous Silica: Synthesis, Structure, and Methylene Blue Adsorption

Kouznetsova,

Ivanets,

Prozorovich

et al. 2024

Gels

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“…Small angle neutron scattering measurements on the VM and VT series were performed using the Yellow Submarine SANS instrument at the Budapest Neutron Centre [56,57]. The samples were poured into 2 mm thick quartz cuvettes and measured at ambient temperature in the Q range of 0.005-0.36 Å −1 , where Q is de ned as the scattering vector: , θ is half of the scattering angle, and λ is the neutron wavelength used.…”

Section: Characterizationsmentioning

confidence: 99%

Vinyl-Methyl Substituted Silica Aerogel-Like Hybrids as Effective Oil/Organic Solvent Sorbents

Çok

Koç

Len

et al. 2023

Preprint

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This work aimed to develop vinyl/methyl-decorated silica-based aerogel-like hybrids and evaluate their performance as novel oil/organic solvent adsorbents. Silica hybrids were prepared in two series by co-condensation of vinyltrimethoxysilane (VTMS) either with methyltrimethoxysilane (MTMS) (VM-series) or tetraethylorthosilicate (TEOS) (VT-series) followed by surface methylation with TMCS at ambient pressure. By gradual vinyl substitution, the changes in the physicochemical and morphological properties of the hybrids were monitored using complementary characterization techniques, such as FTIR, 29Si-NMR, SEM, N2 porosimetry, small angle neutron/X-ray scattering and contact angle measurements. The results confirmed the significant structural changes in VT-series with increasing VTMS content, whereas it had only a limited effect on the network formation in VM-series. In VT-series, the samples were predominantly mesoporous in nature, even up to a high VTMS content (75 mol%), resulting in large specific surface area values (792–1021 m2/g). However, in VM-series, the samples were mostly macroporous and emerged in sponge-like monolithic form after drying with very low densities (0.087–0.182 g/cm3) and high porosities (87.2–93.9%). The successful vinyl/methyl substitution also resulted in good hydrophobicity (up to 147°) in each series. Owing to its lightweight structure and hydrophobicity, the samples VT-100 and VM-50 had the highest sorption capacities (up to 11.63 g/g for VM-50 and 10.92 g/g for VT-100) for most organic pollutants and stable performance up to 10 cycles. The free-standing monolithic structure, well-developed porous network, enhanced hydrophobic behavior and superior adsorption performance make these materials excellent sorbents for oil spill remediation applications.

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“…Unlike local methods, such as electron microscopy, SANS is thus insensitive to local artefacts and random inhomogeneities. SANS is a powerful tool for studying the microstructure of nanosized porosity in ceramic samples (Allen, 2005;Ryukhtin et al, 2003), particularly in samples for cultural heritage analysis (Len et al, 2022;S ˇevc ˇı ´k et al, 2020). SANS data characterize the bulk structure of the studied sample with excellent statistics and are not biased by surface-bound effects or sample treatments, in contrast to the well known direct imaging methods such as scanning electron microscopy (SEM) or transmission electron microscopy.…”

Section: Introductionmentioning

confidence: 99%

Microstructural changes in building materials after various consolidation treatments studied by small-angle neutron scattering, mercury intrusion porosimetry and scanning electron microscopy

Ryukhtin,

Slížková,

Strunz

et al. 2023

J Appl Cryst

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Stone or rendered facades of historical buildings often encounter loss of cohesion after long-term weathering. Specialist consolidating agents containing nanoparticles which can penetrate the degraded layer are used to extend the lifetime of such facades. Clay mortar prepared in the laboratory was used in the present study as a material for testing the effectiveness of several consolidating agents. Changes in porosity after treatment of the sample layers were assessed using small-angle neutron scattering, mercury intrusion porosimetry and scanning electron microscopy techniques. The scattering differed for the various samples, mainly in the medium range of scattering vector magnitudes. The cause of the scattering was ascribed to three populations of pores: large (micrometres), medium-sized (thousands of ångströms) and small (hundreds of ångströms). While the non-treated sample and the sample treated with a silicic acid ester-based product do not exhibit significant differences, the sample treated with a nano-lime suspension shows a decrease of 16% in the volume fraction of medium-sized pores. A difference was also observed in the sample treated with a dihydrogen ammonium phosphate solution: the size of the medium pores increased while their volume fraction decreased, and a change in the large pores was observed. The modelled small pores remained unaffected by the consolidating treatment.

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Small-Angle Neutron Scattering for Cultural Heritage Studies

Cited by 6 publications

References 17 publications

Design of Nickel-Containing Nanocomposites Based on Ordered Mesoporous Silica: Synthesis, Structure, and Methylene Blue Adsorption

Design of Nickel-Containing Nanocomposites Based on Ordered Mesoporous Silica: Synthesis, Structure, and Methylene Blue Adsorption

Vinyl-Methyl Substituted Silica Aerogel-Like Hybrids as Effective Oil/Organic Solvent Sorbents

Microstructural changes in building materials after various consolidation treatments studied by small-angle neutron scattering, mercury intrusion porosimetry and scanning electron microscopy

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