Neutron Reflectometry

Torikai, Naoya

doi:10.1002/9780470933886.ch5

Cited by 9 publications

(5 citation statements)

References 41 publications

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“…Figure a presents the SCV-NR curves of the integral blend film. A remarkable drop in the reflectivity was consistently observed for the UNR, PNR, and NNR curves not at the critical Q -value for total reflection, Q c , of the Si substrate ( ) but close to the Q c value of dPB ( ) . Here, ρ Si , ρ He , and ρ dPB denote the SLDs for the Si substrate, liquid He, and dPB, respectively.…”

Section: Resultsmentioning

confidence: 80%

“…). 5 Here, ρ Si , ρ He , and ρ dPB denote the SLDs for the Si substrate, liquid He, and dPB, respectively. As shown in the inset, the PNR curve had the highest reflectivity near Q c among the three curves, while the NNR curve had the highest reflectivity at Q ≥ 1 nm −1 .…”

Section: ■ Experimentsmentioning

confidence: 99%

“…Neutron reflectivity (NR) can measure the nanostructures of the buried interfaces of multilayer films because of the high transmission of neutron beams. In addition, because the coherent neutron scattering length differs markedly between deuterium and hydrogen, NR can be used to distinguish organic layers by deuterating either layer. − Thus, SCA layers generated in polymer films have been studied by NR in conjunction with the partial deuteration technique . However, it was difficult for the conventional NR to distinguish the neutrons reflected at multiple surfaces and interfaces of the multilayer films.…”

Section: Introductionmentioning

confidence: 99%

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Interpenetration of Rubber and Silane Coupling Agent on an Inorganic Substrate Revealed by Spin-Contrast-Variation Neutron Reflectivity

Kumada,

Iwahara,

Nishitsuji

et al. 2024

J. Phys. Chem. C

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We elucidated the interpenetration of silane coupling agent (SCA) molecules bound to Si substrates and overcoated rubber using spin-contrastvariation (SCV) neutron reflectivity (NR), which determines the nanostructure of multilayer films from polarized NR curves that change with polarization of hydrogen nuclei in the film samples. In an integral blend film of 15 wt % SCA of trimethoxy(octadecyl)silane and deuterated polybutadiene (dPB) annealed at 120 °C, the (1.7 ± 0.2) nm thick SCA layer was generated between the Si substrate and dPB layer. The SCA layer was composed of 70 vol % SCA molecules extended perpendicularly from the silicon substrate and 30 vol % of dPB molecules. The diffuseness of the interface between the SCA and dPB layers of (1.0 ± 0.2) nm was comparable to the thickness of the SCA layer. These results indicate that SCA and dPB molecules interpenetrate into each other. By contrast, in an SCA-precoated polybutadiene film sample, the layer thickness, diffuseness of interface, and composition of the SCA layer strongly suggest that the densely coated SCA molecules formed a crystal-like structure, and thus, the postcoated polybutadiene molecules could not penetrate into the precoated SCA layer. This poor penetration resulted in peeling off of the polybutadiene layer upon cooling to the cryogenic temperature.

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Section: Resultsmentioning

confidence: 80%

Section: ■ Experimentsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Interpenetration of Rubber and Silane Coupling Agent on an Inorganic Substrate Revealed by Spin-Contrast-Variation Neutron Reflectivity

Kumada,

Iwahara,

Nishitsuji

et al. 2024

J. Phys. Chem. C

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“…With XRR, the X-ray beam probes differences in electron density to determine surface roughness and thickness. Similar analysis can be done using NR, which monitors reflectivity variations arising from different nuclei; NR is more sensitive than XRR for lighter elements or isotopes (Torikai, 2011;Zhou & Chen, 1995). Another commonly used technique for the analysis of polymer (#11, 14, 16), 1 (#9, 12, 15), or 2 (#8, 10,13) G units; bands 17-24 are tri-esterified oligomers with 1 (#18, 20, 22, 24) or 2 (#17, 19, 21, 23 surfaces is XPS, which employs an X-ray beam to measure the differences in the kinetic energy of the electrons radiated from the surface.…”

Section: Nr and Xrrmentioning

confidence: 99%

“…Collectively, these surface techniques have been able to identify phase segregation in block copolymers, interfacial segregation of polymer mixtures, and surface composition changes as a result of time and environment (Rymuszka et al, 2016; Thomas & Penfold, 1996; Torikai, 2011). While XRR, NR, and XPS can provide valuable information about surface composition, they have limited resolution, require isotopic labeling, and are unable to detect intact large molecules such as oligomers.…”

Section: Analysis and Imaging Of Solid Polymer Surfacesmentioning

confidence: 99%

Mass spectrometry of polymers: A tutorial review

Wesdemiotis

Williams-Pavlantos

Keating

et al. 2023

Mass Spectrometry Reviews

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Ever since the inception of synthetic polymeric materials in the late 19th century, the number of studies on polymers as well as the complexity of their structures have only increased. The development and commercialization of new polymers with properties fine‐tuned for specific technological, environmental, consumer, or biomedical applications requires powerful analytical techniques that permit the in‐depth characterization of these materials. One such method with the ability to provide chemical composition and structure information with high sensitivity, selectivity, specificity, and speed is mass spectrometry (MS). This tutorial review presents and exemplifies the various MS techniques available for the elucidation of specific structural features in a synthetic polymer, including compositional complexity, primary structure, architecture, topology, and surface properties. Key to every MS analysis is sample conversion to gas‐phase ions. This review describes the fundamentals of the most suitable ionization methods for synthetic materials and provides relevant sample preparation protocols. Most importantly, structural characterizations via one‐step as well as hyphenated or multidimensional approaches are introduced and demonstrated with specific applications, including surface sensitive and imaging techniques. The aim of this tutorial review is to illustrate the capabilities of MS for the characterization of large, complex polymers and emphasize its potential as a powerful compositional and structural elucidation tool in polymer chemistry.

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Novel neutron reflectometer SOFIA at J-PARC/MLF for in-situ soft-interface characterization

Mitamura

Yamada

Sagehashi

et al. 2012

Polym J

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150

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Structural characterization of interfaces composed of soft materials (soft interfaces) helps in understanding their physical behavior. Neutron reflectometry is one of the most powerful tools to characterize interfacial structures with spatial resolution in nanometers. We have installed a novel horizontal-type time-of-flight neutron reflectometer SOFIA (SOFt Interface Analyzer) at the Japan Proton Accelerator Research Complex. The instrument is capable of accepting two downward neutron beams, at 2.21 and 5.71 to horizontal, which dedicate neutron reflectivity (NR) measurements over a wide range of neutron momentum transfer q (q ¼ (4p/k)sinh, where k and h are wavelength and incident angle, respectively). The accuracy of NR up to q ¼ 6 nm À1 was confirmed by measuring deuterated polystyrene (d-PS) thin films on a silicon (Si) wafer and multilayers of cadmium stearate prepared by the Langmuir-Blodgett method. NR at the deuterium oxide (D 2 O)/Si disk showed specular reflection down to 10 À6-10 À7 and q up to 2.0 nm À1 along the perpendicular to the sample surface, which improved the precise analysis of swollen polyelectrolyte brush structure at the D 2 O interface. Then, time-resolved in-situ NR measurements were carried out at 1-min intervals to observe interfacial mixing of d-PS on the PS brush surface during 398 K annealing, demonstrating that nonequilibrium behavior at the interfaces can be analyzed on the order of minutes.

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Neutron Reflectometry

Cited by 9 publications

References 41 publications

Interpenetration of Rubber and Silane Coupling Agent on an Inorganic Substrate Revealed by Spin-Contrast-Variation Neutron Reflectivity

Interpenetration of Rubber and Silane Coupling Agent on an Inorganic Substrate Revealed by Spin-Contrast-Variation Neutron Reflectivity

Mass spectrometry of polymers: A tutorial review

Novel neutron reflectometer SOFIA at J-PARC/MLF for in-situ soft-interface characterization

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