Abstract
Given that terahertz (THz) radiation responds to intermolecular forces such as hydrogen bonds, THz time-domain spectroscopy (THz-TDS) has expanded possibilities in cellulose research. In this study, THz-TDS was used to investigate the crystallinity of three types of cellulose-based materials. Microcrystalline cellulose (MCC) and wood were ball milled at different times, and pseudo-wood was a mixture of MCC and lignin of different mass fractions. All the samples showed peaks at 3.04 THz in the THz mass absorption coefficient spectra. Further, the spectra from 2.79 THz to 3.32 THz were cut out and detrended by subtraction from a baseline. The integrated intensity of the detrended spectra showed a correlation with the mass fraction of lignin of the pseudo-wood samples, and ball milling time of the MCC and wood samples. The correlation was similar with the crystallinity index calculated from X-ray powder diffraction. Moreover, the original wood sample without ball milling had an integrated intensity that was about 30% that of the original MCC sample, matching with the cellulose concentration of the wood (about 30% to 40%). We normalized the integrated intensity of 2.79 THz to 3.32 THz into 1 to 0 by a min–max algorithm and proposed a new “index” for evaluating crystallinity.
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Acknowledgments
The authors would like to express our grateful appreciation to Dr. Liu and Dr. Wang for the supplement of the organic-solvent lignin samples. This work was supported by JSPS KAKENHI Grant Number 16H02559. The XRD measurement was supported by Radioisotope Research Center, Nagoya University. And the first author also thanks for the Mitsutani scholarship for living support.
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JSPS KAKENHI Grant Number 16H02559.
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Han Wang and Tetsuya Inagaki conceived and designed the experiments. Han Wang performed the experiments, analyzed the data and wrote the paper, Tetsuya Inagaki and Satoru Tsuchikawa gave final approval of the manuscript.
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Wang, H., Tsuchikawa, S. & Inagaki, T. Terahertz time-domain spectroscopy as a novel tool for crystallographic analysis in cellulose: the potentiality of being a new standard for evaluating crystallinity. Cellulose 28, 5293–5304 (2021). https://doi.org/10.1007/s10570-021-03902-x
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DOI: https://doi.org/10.1007/s10570-021-03902-x