Determination of crystallinity of Chinese handmade papers by means of X-ray diffraction
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Peng Liu
Dr. Peng Liu is assistant professor and works at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. He received his Ph.D. from Donghua University in 2017. His research background is in pulping and paper making and polymer materials science. His research interests are traditional handmade papers and preservation of ancient books.
,
Hongbin Zhang
Dr. Hongbin Zhang is associate professor and works at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. He received his Ph.D. from Fudan University in 2014. His research interests are paper ink and protection of ancient books by deacidification.Dr. Sinong Wang is associate professor and works at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. She received her Ph.D. from Fudan University in 2014. Her research interests are deacidification by nano-materials and related deacidification methods.Dr. Hui Yu is associate professor and works at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. He received his Ph.D. from Fudan University in 2014. His research interests are the restoration of traditional Chinese handmade paper technology and the deacidification of ancient books.Bingjie Lu ,Xinran Li andBing Wang are freshmen in the natural science experimental class of Xide College in Fudan University. They participated in the Rising-star Research Program of Xide College to study the characterization technology and structure-activity relationship of traditional Chinese handmade paper.Dr. Yueer Yan is associate professor and works at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. She received her Ph.D. from Fudan University in 2016. Her research interests are traditional handmade papers and preservation of ancient books.
and
Yi Tang
Prof. Dr. Yi Tang is professor at the Department of Chemistry and at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. He is the recipient of the National Science Fund for Distinguished Young Scholars of China. His research interests include conservation of ancient books, molecular sieve catalysis and electrochemical catalysts.
Abstract
The crystallinity indices (CrI) of Chinese handmade papers were investigated using the X-ray diffraction (XRD) method. Four Chinese handmade papers, Yingchun, Zhuma, Yuanshu and Longxucao papers were used as model substrates of mulberry bark, ramie, bamboo and Eulaliopsis binata papers, respectively. Two forms of the paper samples, paper sheets and their comminuted powders, were used in this study. The results showed that their XRD patterns belong to the cellulose-I type and Iβ dominates the cellulose microstructure of these paper samples. Moreover, it was found that the microstructures and CrIs of cellulose of these papers were changed by the grinding treatment. This work suggested that the sheet form of the handmade papers is suitable to determine CrI by XRD, despite the contribution of non-cellulosic components in the papers. The order of CrIs for these paper sheet samples was Yingchun, Zhuma, Longxucao and Yuanshu papers. Besides CrIs, differences in cross-sectional areas of the crystalline zone of cellulose can be used for comparing different types of handmade papers. It was also found that the CrIs and crystallite size of paper cellulose varied between the sheet samples and the powder samples, illustrating that the pulverisation has a negative influence on the microstructure of the handmade papers.
Zusammenfassung
Bestimmung der Kristallinität von handgeschöpften chinesischen Papieren mittels Röntgenbeugung
In der vorliegenden Studie wurde der Kristallinitätsindex (CrI) handgeschöpfter chinesischer Papiere mittels Röntgenbeugung (XRD) untersucht. Vier Papiere – Yingchun, Zhuma, Yuanshu und Longxucao – wurden exemplarisch als Maulbeerbaum-Rindenpapier, Ramie-Papier, Bambuspapier und Eulaliopsis binata-Papier getestet. Proben wurden sowohl aus den Papierbögen als auch aus pulverisierten Papieren hergestellt. XRD Analysen ergaben, dass die Proben zum Cellulose-I-Typ gehören und die Cellulosemikrostrukturen Iβ-dominant sind. Darüber hinaus wurde festgestellt, dass die Mikrostrukturen und der CrI von Cellulose durch die Pulverisierung der Proben verändert wurden. Sowohl der CrI als auch die Kristallitgröße variieren zwischen den Proben von Papierbögen und pulverisierten Proben, was zeigt, dass die Zerkleinerung einen negativen Einfluss auf die Mikrostruktur der handgefertigten Papiere hat. Aufgrund der vorliegenden Studie kann angenommen werden, dass der CrI mittels XRD an handgeschöpfte Papiere trotz der nicht-cellulotischen Komponenten bestimmt werden kann. Der CrI ist am höchsten bei Yingchun-Papier, danach in absteigender Reihenfolge Zhuma, Longxucao und Yuanshu. Neben CrI können Unterschiede in den Querschnittsflächen der kristallinen Zone von Cellulose zum Vergleich verschiedener Arten von handgeschöpften Papieren verwendet werden.
Résumé
La détermination de la cristallinité de papiers chinois faits main et la taille de la cellulose au moyen de la diffraction de rayons X.
L’index de cristallinité (CrI) de papier chinois faits main a été étudié en utilisant la méthode de diffraction aux rayons X (XRD). Quatre papiers chinois faits main Yingchun, Zhuma, Yuanshu et Longxucao ont été respectivement utilisés comme substrats modèles de papier de fibres d’écorce de mûrier, de papier ramie, de bambou et d’Eulaliopsis binata. Deux sortes d’échantillons papier sous forme de feuille et de poudre ont été utilisés dans cette étude. Les résultats montrent que les motifs de XRD sont ceux de la cellulose de type I et les microstructures de ces échantillons de papier de type Iβ dominent. De plus, nous avons constaté que les microstructures et le CrL de la cellulose de ces papiers est changée par le traitement de broyage. Ce travail suggère que l’emploi de feuille de papier fait main est adapté pour déterminer le Crl au moyen de la XRD et on obtient des résultats évidents, en dépit de la présence d’éléments non cellulosiques dans les papiers. L’ordre de Crl de ces feuilles de papier est le suivant: papier Yingchun > papier Zhuma > papier Longxucao > papier Yuanshu. En plus des Crls, des différences dans les zones cristallines de la cellulose des coupes transversales peuvent servir à comparer différents types de papiers faits main. On a aussi constaté que les Crl et la taille des cristaux de cellulose varie entre les feuilles de papier et les échantillons en poudre, ce qui illustre le fait que le broyage a une influence négative sur la microstructure des papiers faits main.
Funding statement: This research was supported by the Foundation of Key Laboratory of Pulp and Paper Science and Technology of Ministry of Education/Shandong Province of China (KF201715); the National Natural Science Foundation of China (21703041; 21805042); the Shanghai Sailing Program (17YF1401100; 18YF1401400).
About the authors
Dr. Peng Liu is assistant professor and works at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. He received his Ph.D. from Donghua University in 2017. His research background is in pulping and paper making and polymer materials science. His research interests are traditional handmade papers and preservation of ancient books.
Dr. Hongbin Zhang is associate professor and works at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. He received his Ph.D. from Fudan University in 2014. His research interests are paper ink and protection of ancient books by deacidification.
Dr. Sinong Wang is associate professor and works at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. She received her Ph.D. from Fudan University in 2014. Her research interests are deacidification by nano-materials and related deacidification methods.
Dr. Hui Yu is associate professor and works at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. He received his Ph.D. from Fudan University in 2014. His research interests are the restoration of traditional Chinese handmade paper technology and the deacidification of ancient books.
Bingjie Lu, Xinran Li and Bing Wang are freshmen in the natural science experimental class of Xide College in Fudan University. They participated in the Rising-star Research Program of Xide College to study the characterization technology and structure-activity relationship of traditional Chinese handmade paper.
Dr. Yueer Yan is associate professor and works at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. She received her Ph.D. from Fudan University in 2016. Her research interests are traditional handmade papers and preservation of ancient books.
Prof. Dr. Yi Tang is professor at the Department of Chemistry and at the Institute for Preservation and Conservation of Chinese Ancient Books in Fudan University. He is the recipient of the National Science Fund for Distinguished Young Scholars of China. His research interests include conservation of ancient books, molecular sieve catalysis and electrochemical catalysts.
References
Agarwal, U. P., Ralph, S. A., Reiner, R. S., Baez, C.: New cellulose crystallinity estimation method that differentiates between organized and crystalline phases. Carbohydrate Polymers 190 (2018): 262–270.10.1016/j.carbpol.2018.03.003Search in Google Scholar
Agarwal, U. P., Reiner, R. R., Ralph, S. A.: Estimation of cellulose crystallinity of lignocelluloses using Near-IR FT-Raman spectroscopy and comparison of the Raman and Segal-WAXS methods. Journal of Agricultural and Food Chemistry 61 (2013): 103–113.10.1021/jf304465kSearch in Google Scholar
Agarwal, U. P., Reiner, R. S., Ralph, S. A.: Cellulose I crystallinity determination using FT–Raman spectroscopy: univariate and multivariate methods. Cellulose 17 (2010): 721–733.10.1007/s10570-010-9420-zSearch in Google Scholar
Baty, J. W., Maitland, C. L., Minter, W., Hubbe, M. A., Jordan-Mowery, S. K.: Deacidification for the conservation and preservation of paper-based works: a review. Bioresources 5 (2010): 1955–2023.10.15376/biores.5.3.1955-2023Search in Google Scholar
Bledzki, A. K., Gassan, J.: Composites reinforced with cellulose based fibres. Progress in Polymer Science 24 (1999): 221–274.10.1016/S0079-6700(98)00018-5Search in Google Scholar
El-Esseily, A.-S., Inaba, M.: Gamma irradiation of Washi. Part 2 changes in degree of polymerization and crystallinity of cellulose. Restaurator. International Journal for the Preservation of Library and Archival Material 25 (2004): 40–46.10.1515/REST.2004.40Search in Google Scholar
Garside, P., Wyeth, P.: Polarised ATR-FTIR characterisation of cellulosic fibres in relation to historic artefacts. Restaurator. International Journal for the Preservation of Library and Archival Material 25 (2004): 249–259.10.1515/REST.2004.249Search in Google Scholar
Garvey, C. J., Parker, I. H., Simon, G. P.: On the interpretation of X-ray diffraction powder patterns in terms of the nanostructure of cellulose I fibres. Macromolecular Chemistry and Physics 206 (2005): 1568–1575.10.1002/macp.200500008Search in Google Scholar
Hassan, R.: Thermal degradation of paper: the structural changes of fibers. Egyptian Journal of Archaeological and Restroration Studies 6 (2016): 71–84.10.21608/ejars.2016.23543Search in Google Scholar
He, J., Cui, S., Wang, S.-Y.: Preparation and crystalline analysis of high-grade bamboo dissolving pulp for cellulose acetate. Journal of Applied Polymer Science 107 (2008): 1029–1038.10.1002/app.27061Search in Google Scholar
Hult, E.-L., Iversen, T., Sugiyama, J.: Characterization of the supermolecular structure of cellulose in wood pulp fibres. Cellulose 10 (2003): 103–110.10.1023/A:1024080700873Search in Google Scholar
Ju, X., Bowden, M., Brown, E. E., Zhang, X.: An improved X-ray diffraction method for cellulose crystallinity measurement. Carbohydrate Polymers 123 (2015): 476–481.10.1016/j.carbpol.2014.12.071Search in Google Scholar
Łojewski, T., Zięba, K., Kołodziej, A., Łojewska, J.: Following cellulose depolymerization in paper: comparison of size exclusion chromatography techniques. Cellulose 18 (2011): 1349–1363.10.1007/s10570-011-9562-7Search in Google Scholar
Nisizawa, K.: Mode of action of cellulases. Journal of Fermentation Technology 51 (1973): 267–304.Search in Google Scholar
Park, S., Baker, J. O., Himmel, M. E., Parilla, P. A., Johnson, D. K.: Cellulose crystallinity index: measurement techniques and their impact on interpreting cellulase performance. Biotechnology for Biofuels 3 (2010): 10.10.1186/1754-6834-3-10Search in Google Scholar
Pedersoli Jr., J.L.: Effect of cellulose crystallinity on the progress of thermal oxidative degradation of paper. Journal of Applied Polymer Science 78 (2000): 61–66.10.1002/1097-4628(20001003)78:1<61::AID-APP90>3.0.CO;2-KSearch in Google Scholar
Sandy, M., Manning, A., Bollet, F.: Changes in the crystallinity of cellulose in response to changes in relative humidity and acid treatment. Restaurator. International Journal for the Preservation of Library and Archival Material 31 (2010): 1–18.10.1515/rest.2010.001Search in Google Scholar
Sawpan, M. A., Pickering, K. L., Fernyhough, A.: Effect of various chemical treatments on the fibre structure and tensile properties of industrial hemp fibres. Composites Part A: Applied Science and Manufacturing 42 (2011): 888–895.10.1016/j.compositesa.2011.03.008Search in Google Scholar
Schenzel, K., Fischer, S., Brendler, E.: New method for determining the degree of cellulose I crystallinity by means of FT Raman spectroscopy. Cellulose 12 (2005): 223–231.10.1007/s10570-004-3885-6Search in Google Scholar
Segal, L., Creely, J. J., Martin, A. E., Conrad, C. M.: An empirical method for estimating the degree of crystallinity of native cellulose using the X-ray diffractometer. Textile Research Journal 29 (1959): 786–794.10.1177/004051755902901003Search in Google Scholar
Wada, M., Okano, T.: Localization of Iα and Iβ phases in algal cellulose revealed by acid treatments. Cellulose 8 (2001): 183–188.10.1023/A:1013196220602Search in Google Scholar
Wang, Y., Zhao, Y., Deng, Y.: Effect of enzymatic treatment on cotton fiber dissolution in NaOH/urea solution at cold temperature. Carbohydrate Polymers 72 (2008): 178–184.10.1016/j.carbpol.2007.08.003Search in Google Scholar
Wilkie, J. S.: Carl Nägeli and the fine structure of living matter. Nature 190 (1961): 1145–1150.10.1038/1901145a0Search in Google Scholar
Yuan, L., Wan, J., Ma, Y., Wang, Y., Huang, M., Chen, Y.: The content of different hydrogen bond models and crystal structure of eucalyptus fibers during beating. Bioresources 8 (2013): 717–734.10.15376/biores.8.1.717-734Search in Google Scholar
Zervos, S., Alexopoulou, I.: Paper conservation methods: a literature review. Cellulose 22 (2015): 2859–2897.10.1007/s10570-015-0699-7Search in Google Scholar
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Articles in the same Issue
- Frontmatter
- Editorial
- Editorial
- Original Works
- Determination of crystallinity of Chinese handmade papers by means of X-ray diffraction
- Identification tags for archival documents based on oxides of transition and inner transition metals – influence on paper supports
- Technical Note
- Eliminating Hydrogen Peroxide Volatiles after Lead White Conversion Treatment Via Sorption Agents
Articles in the same Issue
- Frontmatter
- Editorial
- Editorial
- Original Works
- Determination of crystallinity of Chinese handmade papers by means of X-ray diffraction
- Identification tags for archival documents based on oxides of transition and inner transition metals – influence on paper supports
- Technical Note
- Eliminating Hydrogen Peroxide Volatiles after Lead White Conversion Treatment Via Sorption Agents
