Article
Polymer Science
Mariapaola Staropoli, Dominik Gerstner, Benoit Duez, Michael Sztucki, Guido Vehres, Aurel Radulescu, Stephan Westermann, Wim Pyckhout-Hintzen, Jean-Sebestien Thomann
Summary: This study investigates the structural and dynamic characteristics of a silica filler network in an industrial elastomeric composite using time-resolved Ultra Small-Angle-X-ray Scattering (USAXS) technique. The in-situ observation under periodic uniaxial deformation reveals a correlation between the filler network evolution and the dynamic-mechanical stress-strain response of the composite. By analyzing the sector-averaged scattering intensities, the researchers identify the jamming/de-jamming transition between clusters during the deformation process.
Article
Polymer Science
Nabil Hayeemasae, Kamaruddin Waesateh, Sitisaiyidah Saiwari, Hanafi Ismail, Nadras Othman
Summary: This study utilized epoxidized natural rubber and halloysite nanotubes to prepare composites, finding that controlling the epoxide level can optimize the formulation, reduce filler-filler interactions, and enhance the performance of the composites.
Article
Polymer Science
Fei Xiang, Konrad Schneider, Matthias Schwartzkopf, Gert Heinrich
Summary: This study investigated the structural changes at the crack tip of unfilled and carbon black-filled natural rubber under static deformation using synchrotron-based small-and wide-angle X-ray scattering. The distributions of cavities and crystallites at the crack tip were determined at different external strain levels. The addition of carbon black was found to enhance strain-induced crystallization and prevent the formation of cavities.
Article
Polymer Science
Feixiang Sha, Guojun Cheng, Xiuhong Li, Feng Tian, Zhongfeng Tang
Summary: This study used synchrotron ultra-small angle X-ray scattering techniques combined with in-situ uniaxial stretching to investigate the degradation mechanism of cross-linked polytetrafluoroethylene (XPTFE) in real time. The results showed that the scatterers for XPTFE became more unequal with increasing cross-linking degree. After stretching or irradiation, the mechanical properties of XPTFE were lost, resulting in the dominance of broken crystals and the formation of voids during stretching. However, XPTFE under constant stress uniaxial stretching exhibited a degree of thermal stability.
POLYMER DEGRADATION AND STABILITY
(2022)
Article
Multidisciplinary Sciences
J. S. Park, J. D. Almer, K. C. James, L. J. Natanson, S. R. Stock
Summary: Members of subclass Elasmobranchii possess bioapatite mineralization in their cartilage skeletons, which has similar crystallography to bone but exhibits some differences. The mineral phase in shark centra has larger nanocrystallite sizes and is associated with less microstrain compared to bone.
JOURNAL OF THE ROYAL SOCIETY INTERFACE
(2022)
Article
Polymer Science
Nabil Hayeemasae, Abdulhakim Masa, Nadras Othman, Indra Surya
Summary: Natural rubber (NR) is incompatible with hydrophilic additives, but the addition of silane coupling agents greatly improves the properties of NR/HNT composites, including modulus, tensile strength, and tear strength. Among the four different silanes tested, AEAPTMS is found to be the most viable choice. The strain-induced crystallization (SIC) of the composites is substantially aided by the corresponding silanes.
Article
Chemistry, Multidisciplinary
Theyencheri Narayanan, Michael Sztucki, Thomas Zinn, Jerome Kieffer, Alejandro Homs-Puron, Jacques Gorini, Pierre Van Vaerenbergh, Peter Boesecke
Summary: This article describes the new technical features and enhanced performance of the ID02 beamline with the Extremely Brilliant Source (EBS) at the ESRF. The beamline enables static and kinetic investigations of a broad range of systems in different size scales and time ranges. Additionally, it allows for multispeckle X-ray photon correlation spectroscopy measurements and relaxation of collimation conditions, resulting in higher flux throughput and lower background. The article highlights the importance of these developments in enabling structural, dynamic, and kinetic investigations of out-of-equilibrium soft matter and biophysical systems.
JOURNAL OF APPLIED CRYSTALLOGRAPHY
(2022)
Article
Polymer Science
Apisit Banpean, Hideaki Takagi, Nobutaka Shimizu, Noriyuki Igarashi, Shinichi Sakurai
Summary: The study focused on the confined crystallization of PEG in PLLA spherulite in a PLLA/PEG blend specimen using SAXS/WAXS measurements. The results showed suppression of PEG lamellae growth in the thickness direction due to space confinement by preformed PLLA lamellae, while also observing more regular stacking in the blend specimen.
Review
Chemistry, Analytical
Seema Thakral, Kyungtae Kim
Summary: Small-angle scattering (SAS) is a versatile analytical technique that provides detailed structural information at the nanometer scale. It has diverse applications in pharmaceutical material characterization, including identification of liquid-crystalline mesophase of drugs, study of excipient microstructure influence, and optimization of solid dispersions and protein-based therapeutics formulations.
TRAC-TRENDS IN ANALYTICAL CHEMISTRY
(2021)
Review
Chemistry, Physical
Kun Qian, Randall E. Winans, Tao Li
Summary: Understanding the nanostructures of liquid electrolytes is crucial for enhancing electrochemical energy storage capacities, but the solvation structures and molecular dynamics in electrolytes are difficult to probe. Small-angle X-ray scattering (SAXS) offers unique insights into molecular clusters and ion pairs in electrolytes, with excellent time-resolution for studying molecular dynamics. This review focuses on the microscopic understanding of liquid electrolytes by SAXS and highlights the unique capabilities of X-ray scattering for nanostructure characterization.
ADVANCED ENERGY MATERIALS
(2021)
Article
Materials Science, Multidisciplinary
H. Takeno, Y. Aoki, K. Kimura
Summary: The addition of SiO2 nanospheres to clay/PAAS hydrogels significantly enhances mechanical performance such as tensile strength and extensibility, without adhering to other constituents. SAXS analysis reveals that clay platelets disperse comparatively in the hydrogels.
MATERIALS TODAY COMMUNICATIONS
(2021)
Article
Materials Science, Characterization & Testing
Aksel S. Obdrup, D. C. Florian Wieland, Mathias K. Huss-Hansen, Matthias M. L. Arras, Matti Knaapila
Summary: In this study, wide-angle X-ray scattering combined with linear discriminant analysis was used to distinguish between healthy and damaged UHMWPE ropes, providing a new method for nondestructive testing.
Article
Polymer Science
Katsumi Hagita, Tetsuo Tominaga, Ryota Yamamoto, Takuo Sone
Summary: In this study, a particle-mesh-based two-dimensional reverse Monte Carlo method was used to investigate the three-dimensional structure of nanoparticle aggregates in rubber tire treads. It was found that the characteristic cluster sizes of silica nanoparticles in end-modified styrene-butadiene rubber treads were smaller than those in nonmodified SBR treads. The deformation of the nanoparticles during stretching was modeled using a series of two-dimensional scattering patterns, and a high-connectivity cluster analysis was used to characterize the morphologies of the nanoparticles.
Article
Biochemistry & Molecular Biology
Hiroshi Imamura, Shinya Honda
Summary: Antibody aggregation and acid denaturation followed by neutralization of pH contribute to the high cost of therapeutic monoclonal antibody production. Understanding the structural details of acid-denatured antibodies is crucial for antibody engineering. Research has shown that acid-denatured monoclonal antibodies become smaller globules at pH 2 compared to their native structure at pH 7. Small-angle X-ray scattering data indicate conformational changes that can lead to aggregation. The distortion of the Fc region and longer inter-domain correlations are found to initiate acid denaturation and aggregation.
INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
(2023)
Article
Polymer Science
Chao-Wen Yang, Ting-Ting Yang, Li-Zhao Huang, Jing-Jing Han, Guang-Ai Sun, Jia-Zhuang Xu, Zhong-Ming Li, Dong Liu
Summary: In this study, deuterated chain labeling and in situ small-angle neutron scattering (SANS) were used to investigate the correlation between structure evolution and Mullins effect of filled silicone rubber under variable amplitude loading. The mechanical properties and macrostructure parameters showed consistent patterns in both conditions. The extracted parameters from the constitutive model further confirmed these patterns. The system exhibited stable equilibrium with minimal variation in mechanical properties and microstructural evolution.
Article
Polymer Science
Hio Sakai, Daisuke Aoki, Kota Seshimo, Koichi Mayumi, Shotaro Nishitsuji, Takashi Kurose, Hiroshi Ito, Hideyuki Otsuka
Article
Chemistry, Multidisciplinary
Kota Seshimo, Hio Sakai, Takuma Watabe, Daisuke Aoki, Hajime Sugita, Koichiro Mikami, Yuchen Mao, Akira Ishigami, Shotaro Nishitsuji, Takashi Kurose, Hiroshi Ito, Hideyuki Otsuka
Summary: Mechanochromic elastomers with force-induced cross-linking reactions and fluorescence properties have been successfully synthesized, demonstrating for the first time damage detection and changes in the mechanical properties of bulk elastomers induced by simple compression or extension.
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION
(2021)
Article
Polymer Science
Hiroki Ogawa, Mikihito Takenaka, Tsukasa Miyazaki
Summary: The study investigated the morphological transition behaviors of symmetric PS-b-P2VP with different molecular weights during spin-coating from a toluene solution using GISAXS. It was found that lower molecular weights led to disordered structures, while higher molecular weights resulted in hexagonally packed cylindrical structures and lamellar structures. The effects of selective solvent evaporation on the transition process were significant for higher molecular weights.
Article
Polymer Science
Yoshihiko Kimura, Sahori Imai, Mikihito Takenaka, Takaya Terashima
Summary: Building cyclic units into amphiphilic copolymers leads to the creation of versatile self-assembled systems in different media, producing nanoaggregates and microphase separation materials with unique properties. The introduction of in-chain ring units enhances the functionality and solubility of the copolymers, resulting in crystallization-driven microphase separation and the formation of sub-5 nm lamellar structure materials.
Article
Nanoscience & Nanotechnology
Yu-Hong Cheng, Reine Moriyama, Hinako Ebe, Kei Mizuguchi, Ryohei Yamakado, Shotaro Nishitsuji, Takayuki Chiba, Junji Kido
Summary: Metal halide perovskites have excellent optoelectronic and semiconducting properties but are often associated with environmental concerns due to the toxicity of lead. This study introduces a two-step crystallization method to improve the performance of lead-free PEA(2)SnI(4) perovskite. The resulting film exhibits narrowed emission and reduced Sn4+ content, leading to a higher external quantum efficiency in the resulting LED.
ACS APPLIED MATERIALS & INTERFACES
(2022)
Article
Engineering, Chemical
Shotaro Nishitsuji, Toshiki Sato, Masaru Ishikawa, Takashi Inoue, Hiroshi Ito
Summary: The effects of annealing conditions and molecular weight on the energies required for cracking and plastic deformation were investigated. It was found that annealing reduced the energy required for plastic deformation, while the energy required for cracking remained the same. Additionally, increasing the molecular weight increased both the energy required for plastic deformation and cracking.
POLYMER ENGINEERING AND SCIENCE
(2022)
Article
Chemistry, Multidisciplinary
Hiroki Ogawa, Mika Aoki, Shunsuke Ono, Yuki Watanabe, Satoru Yamamoto, Keiji Tanaka, Mikihito Takenaka
Summary: We have successfully visualized the spatial heterogeneity of the reaction ratio in epoxy resins by combining medium-angle X-ray scattering (MAXS) and computed tomography (CT). The scattering peak in MAXS reflects the cross-linking structures and can be used to measure the reaction ratio. By reconstructing CT images from the peak intensity, we were able to visualize the spatial heterogeneity of the reaction ratio. This method can be applied to study the heterogeneity of cross-linked structures in other materials.
Article
Polymer Science
Mizuki Kishimoto, Mikihito Takenaka, Hitoshi Iwabuki
Summary: Many studies have shown that crystallization in semicrystalline polymers leads to the existence of an amorphous region with reduced mobility. However, the spatial distribution of this rigid amorphous region has not been fully understood. In this study, contrast variation small-angle X-ray scattering (CV-SAXS) was used to investigate the swollen ethyleneoctene copolymer with granular crystallites, revealing that the rigid amorphous region exists around and between the crystallites. The weight fraction of the rigid amorphous region estimated by CV-SAXS was consistent with measurements obtained by pulsed proton nuclear magnetic resonance.
Article
Polymer Science
Yuki Watanabe, Hiroki Ogawa, Takashi Konishi, Shotaro Nishitsuji, Shunsuke Ono, Nobutaka Shimizu, Mikihito Takenaka
Summary: The study used the SAXS-CT method to investigate the orientation distribution of the lamellar structure of injection-molded HDPE. CT images in the X-Y and X-Z planes showed the different distribution patterns and thickness variations of the skin layer, subskin layer, and core layer.
Article
Polymer Science
Yohei Nakanishi, Ryohei Ishige, Hiroki Ogawa, Yun Huang, Keita Sakakibara, Kohji Ohno, Toshiji Kanaya, Mikihito Takenaka, Yoshinobu Tsujii
Summary: The higher-order structures of polymer-brush-modified nanoparticles in ionic liquids were analyzed using ultrasmall-angle X-ray scattering. The self-assembly of the nanoparticles was found to be entropy-driven and influenced by the concentrations and lengths of the polymer brushes.
Article
Chemistry, Physical
Keisuke Shimokita, Katsuhiro Yamamoto, Noboru Miyata, Yohei Nakanishi, Motoki Shibata, Mikihito Takenaka, Norifumi L. Yamada, Hideki Seto, Hiroyuki Aoki, Tsukasa Miyazaki
Summary: In the case of PMMA thin films on a Si substrate, thermal annealing leads to the formation of a tightly adsorbed layer of PMMA chains near the substrate interface. This layer remains on the substrate even after washing and exhibits a three-layer structure. The presence of a buffer layer between the solid adsorption layer and the bulk-like swollen layer was observed, indicating higher toluene sorption capacity.
Article
Chemistry, Multidisciplinary
Hiroaki Asai, Motoki Shibata, Mikihito Takenaka, Shinichi Takata, Kosuke Hiroi, Makoto Ouchi, Takaya Terashima
Summary: This paper demonstrates a versatile synthetic system of crosslinked hydrogels with highly stretchable, self-healing, and selectively adhesive properties. The hydrogels are obtained by the self-assembly of amphiphilic random copolymers carrying hydrophilic PEG, hydrophobic butyl or dodecyl groups, and methacrylate-terminal PEG in water. The size, aggregation number, and pendant methacrylate number of the micelles are controlled by the composition and degree of polymerization. Hydrogels obtained show self-healing and selectively adhesive properties, with self-healing promoted upon heating and adhesive properties dependent on the alkyl group composition.
Article
Chemistry, Multidisciplinary
Ali Pournaghshband Isfahani, Mahdi Shahrooz, Takuma Yamamoto, Ansori Muchtar, Masateru M. Ito, Daisuke Yamaguchi, Mikihito Takenaka, Easan Sivaniah, Behnam Ghalei
Summary: Polybutadiene-based polyurethanes with different cis/trans/1,2-vinyl microstructure contents were synthesized and investigated for their phase morphology, physical properties, and gas transport properties. Higher vinyl-content PUs exhibited increased phase mixing and smaller microdomains, leading to more tortuous pathways for gas molecules and decreased gas permeability of the membranes.
Article
Polymer Science
Sahori Imai, Yasuyuki Ommura, Yuki Watanabe, Hiroki Ogawa, Mikihito Takenaka, Makoto Ouchi, Takaya Terashima
Summary: Controlled crystallization and microphase separation are possible methods to construct precise nanostructures in functional polymer materials. This paper reports on the crystallization and sub-10 nm microphase separation of amphiphilic random and random block terpolymers, showing that random block terpolymers efficiently induced crystallization and may control microphase separation.
Article
Polymer Science
Takaya Ikami, Yoshihiko Kimura, Mikihito Takenaka, Makoto Ouchi, Takaya Terashima
Summary: Through the synthesis of amphiphilic crystalline random copolymers with different hydrophilic pendants, main chains, composition, monomer sequence, and molecular weight distribution, it was found that a copolyacrylate with hydroxyl terminal PEG chains and octadecyl groups induced crystallization of the octadecyl groups, forming well-ordered lamellar structures with about 5 nm domain spacing, despite broad molecular weight distribution. This system of sub-10 nm microphase separation has the potential to innovate the creation of functional polymer materials with precise nanostructures.
