Three-Dimensional Nanoscale Imaging of SiO2 Nanofiller in Styrene-Butadiene Rubber with High-Resolution and High-Sensitivity Ptychographic X-ray Computed Tomography

Naru Okawa; Nozomu Ishiguro; Shuntaro Takazawa; Hideshi Uematsu; Yuhei Sasaki; Masaki Abe; Kyosuke Ozaki; Yoshiaki Honjo; Haruki Nishino; Yasumasa Joti; Takaki Hatsui; Yukio Takahashi

doi:10.1093/mam/ozae094

Three-Dimensional Nanoscale Imaging of SiO2 Nanofiller in Styrene-Butadiene Rubber with High-Resolution and High-Sensitivity Ptychographic X-ray Computed Tomography

Microsc Microanal. 2024 Nov 4;30(5):836-843. doi: 10.1093/mam/ozae094.

Authors

Naru Okawa^{1

2

3}, Nozomu Ishiguro^{1

3}, Shuntaro Takazawa^{1

2

3}, Hideshi Uematsu^{1

2

3}, Yuhei Sasaki^{1

2

3}, Masaki Abe^{1

3}, Kyosuke Ozaki³, Yoshiaki Honjo³, Haruki Nishino^{3

4}, Yasumasa Joti^{3

4}, Takaki Hatsui³, Yukio Takahashi^{1

3

5

6}

Affiliations

¹ International Center for Synchrotron Radiation Innovation Smart (SRIS), Tohoku University, 468-1 Aramaki-Aza-Aoba, Aoba-ku, Sendai 980-8572, Japan.
² Department of Metallurgy, Graduate School of Engineering, Tohoku University, Aoba-yama 02, Aoba-ku, Sendai 980-8579, Japan.
³ RIKEN SPring-8 Center, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5148, Japan.
⁴ Japan Synchrotron Radiation Research Institute, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5198, Japan.
⁵ Institute of Multidisciplinary Research for Advanced Materials (IMRAM), Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577, Japan.
⁶ Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai 980-8577, Japan.

PMID: 39298155
DOI: 10.1093/mam/ozae094

Abstract

SiO2 aggregates in styrene-butadiene rubber (SBR) were observed using ptychographic X-ray computed tomography (PXCT). The rubber composites were illuminated with X-rays focused by total reflection focusing mirrors, and the ptychographic diffraction patterns were collected using a CITIUS detector in the range of -75° to +75° angle of incidence. The projection images of the rubber composites were reconstructed with a two-dimensional resolution of 76 nm, and no significant structural changes were observed during the PXCT measurements. A three-dimensional image of the rubber composite was reconstructed with an isotropic resolution of 98 nm. Segmentation of SiO2 from the SBR, based on a histogram analysis of the phase shift, revealed a fragmented network structure of interconnected SiO2 aggregates.

Keywords: CITIUS detector; computed tomography; ptychography; rubber materials; weak-phase objects.