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Polymers
Volume 13
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10.3390/polym13172879
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Article

Novel Approaches to In-Situ ATR-FTIR Spectroscopy and Spectroscopic Imaging for Real-Time Simultaneous Monitoring Curing Reaction and Diffusion of the Curing Agent at Rubber Nanocomposite Surface

by
Shun Muroga
1,*,
Yu Takahashi
2,
Yuta Hikima
2,*,
Seisuke Ata
1,
Sergei G. Kazarian
3,*,
Masahiro Ohshima
2,
Toshiya Okazaki
1 and
Kenji Hata
1
1
CNT-Application Research Center, National Institute of Advanced Industrial Science and Technology, Tsukuba Central 5, 1-1-1, Higashi, Tsukuba 305-8565, Japan
2
Department of Chemical Engineering, Graduate School of Engineering, Kyoto University, Kyoto 615-8510, Japan
3
Department of Chemical Engineering, Imperial College London, South Kensington Campus, London SW7 2AZ, UK
*
Authors to whom correspondence should be addressed.
Polymers 2021, 13(17), 2879; https://doi.org/10.3390/polym13172879
Submission received: 10 August 2021 / Revised: 23 August 2021 / Accepted: 24 August 2021 / Published: 27 August 2021
(This article belongs to the Special Issue Advances in Nanofillers Reinforced Polymer Nanocomposites)
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Abstract

Here, we propose a novel attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy method for simultaneously monitoring the curing reaction and the diffusion behavior of curing agents at the surface of rubber in real-time. The proposed scheme was demonstrated by fluorine rubber (FKM) and FKM/carbon nanotube (CNT) nanocomposites with a target curing agent of triallyl-isocyanurate (TAIC). The broadening and the evolution of the C=O stretching of TAIC were quantitatively analyzed to characterize the reaction and the diffusion. Changes in the width of the C=O stretching indicated the reaction rate at the surface was even faster than that of the bulk as measured by a curemeter. The diffusion coefficient of the curing agent in the course of heating was newly calculated by the initial increase in the absorbance and our model based on Fickian diffusion. The diffusion coefficients of TAIC during curing were evaluated, and its temperature and filler dependency were identified. Cross-sectional ATR-FTIR imaging and in situ ATR-FTIR imaging measurements supported the hypothesis of the unidirectional diffusion of the curing agent towards the heated surface. It was shown that our method of in situ ATR-FTIR can monitor the degrees of cure and the diffusion coefficients of curing agents simultaneously, which cannot be achieved by conventional methods, e.g., rheological measurements.
Keywords: in situ attenuated total reflection infrared spectroscopy; curing reaction; diffusion; triallyl isocyanurate; polymer nanocomposite; fluorine rubber; carbon nanotube; Fourier transform infrared spectroscopic imaging in situ attenuated total reflection infrared spectroscopy; curing reaction; diffusion; triallyl isocyanurate; polymer nanocomposite; fluorine rubber; carbon nanotube; Fourier transform infrared spectroscopic imaging

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MDPI and ACS Style

Muroga, S.; Takahashi, Y.; Hikima, Y.; Ata, S.; Kazarian, S.G.; Ohshima, M.; Okazaki, T.; Hata, K. Novel Approaches to In-Situ ATR-FTIR Spectroscopy and Spectroscopic Imaging for Real-Time Simultaneous Monitoring Curing Reaction and Diffusion of the Curing Agent at Rubber Nanocomposite Surface. Polymers 2021, 13, 2879. https://doi.org/10.3390/polym13172879

AMA Style

Muroga S, Takahashi Y, Hikima Y, Ata S, Kazarian SG, Ohshima M, Okazaki T, Hata K. Novel Approaches to In-Situ ATR-FTIR Spectroscopy and Spectroscopic Imaging for Real-Time Simultaneous Monitoring Curing Reaction and Diffusion of the Curing Agent at Rubber Nanocomposite Surface. Polymers. 2021; 13(17):2879. https://doi.org/10.3390/polym13172879

Chicago/Turabian Style

Muroga, Shun, Yu Takahashi, Yuta Hikima, Seisuke Ata, Sergei G. Kazarian, Masahiro Ohshima, Toshiya Okazaki, and Kenji Hata. 2021. "Novel Approaches to In-Situ ATR-FTIR Spectroscopy and Spectroscopic Imaging for Real-Time Simultaneous Monitoring Curing Reaction and Diffusion of the Curing Agent at Rubber Nanocomposite Surface" Polymers 13, no. 17: 2879. https://doi.org/10.3390/polym13172879

APA Style

Muroga, S., Takahashi, Y., Hikima, Y., Ata, S., Kazarian, S. G., Ohshima, M., Okazaki, T., & Hata, K. (2021). Novel Approaches to In-Situ ATR-FTIR Spectroscopy and Spectroscopic Imaging for Real-Time Simultaneous Monitoring Curing Reaction and Diffusion of the Curing Agent at Rubber Nanocomposite Surface. Polymers, 13(17), 2879. https://doi.org/10.3390/polym13172879

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