Abstract
A short-length cellulose nanofiber (CNF) aqueous sol, prepared by a high-pressure homogenizer, showed a rapid longer relaxation time (T2) in the low-field 1H-nuclear magnetic resonance (NMR) when diluted from 20 wt% to 1 wt%. Magnetic stirring for 30 min disentangled the fiber networks and the fragmented fibers appeared in the 1 wt% CNF sol. A decrease in the specific viscosity of the diluted sols changed the rheological behavior from exponential to linear below 1 wt%, suggesting a significant decrease in the inter-fibril interaction. The small angle x-ray scattering (SAXS) with the generalized indirect Fourier transformation (GIFT) also indicated similar changes in the fiber flocculation structure without a change in the fiber size. The increasing viscosity upon severe fiber fragmentation by a high-pressure homogenizer may be ascribed to tighter holding of the interfibril water molecules. The time-domain (TD)-NMR fully supported the estimation that the transverse relaxation time (T2) showed consistently short for the 2 wt%, became shorter with the stirring time when diluted from 5 wt% to 2 wt%, and showed long upon dilution from 20 wt% to 2 wt%. Understanding the complex behavior of the highly viscous CNF sols during a simple dilution process may pave the way for developing CNF-related technology.
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References
Ali S, Khan SA, Eastoe J, Hussaini SR, Morsy MA, Yamani ZH (2018) Synthesis, characterization, and relaxometry studies of hydrophilic and hydrophobic superparamagnetic Fe3O4 nanoparticles for oil reservoir applications. Colloids Surf Physicochem Eng Aspects 543:133–143. https://doi.org/10.1016/j.colsurfa.2018.02.002
Bagheri V, Ghanbarzadeha B, Ayaseha A, Ostadrahimi A, Ehsanid A, Alizadeh-Sanie M, Adun PA (2019) The optimization of physico mechanical properties of bionanocomposite films based on gluten/carboxymethyl cellulose/cellulose nanofiber using response surface methodology. Polym Testing 78:105989. https://doi.org/10.1016/j.polymertesting.2019.105989
Baghel RS, Reddy CRK, Singh RP (2021) Seaweed-based cellulose: Applications, and future perspectives. Carbohydrate Polym 267:118241. https://doi.org/10.1016/j.carbpol.2021.118241
Brunner-Popela J, Glatter O (1997) Small-angle scattering of interacting particles. I. Basic principles of a global evaluation technique. J Appl Crystallogr 30:431–442. https://doi.org/10.1107/S0021889896015749
Chen W, Li Q, Cao J, Liu Y, Li J, Zhang J, Luo S, Yu H (2015) Revealing the structures of cellulose nanofiber bundles obtained by mechanical nanofibrillation via TEM observation. Carbohydrate Polym 117:950–956. https://doi.org/10.1016/j.carbpol.2014.10.024
Fairhurst D, Sharma R, Takeda S, Cosgrove T, Prescott SW (2021) Fast NMR relaxation, powder wettability and Hansen solubility parameter analyses applied to particle dispersibility. Powder Technol 377:545–552. https://doi.org/10.1016/j.powtec.2020.09.002
Ehmann, HMA (2012) Structuring of sol gel functionalized cellulose materials and their characterization. Thesis for PhD
El-Hosseiny F, Page DH (1975) The mechanical properties of single wood pulp fibres: theories of strength. Fibre Sci Technol 8(1):21–31. https://doi.org/10.1016/0015-0568(75)90012-3
Ezquerro CS, Minana CC, Izquierdo S, Laspalas M (2019) A molecular dynamics model to measure forces between cellulose fibril surfaces: on the effect of non-covalent polyelectrolyte adsorption. Cellulose 26:1449–1466. https://doi.org/10.1007/s10570-018-2166-8
Fairhurst D, Cosgrove T, Prescott SW (2016) Relaxation NMR as a tool to study the dispersion and formulation behavior of nanostructured carbon materials. Magn Reson Chem 54:521–526. https://doi.org/10.1002/mrc.4218
Fatehi P, MacMillan B, Ziaee Z, Xiao H (2009) Qualitative characterization of the diffusion of cationic-modified PVA into the cellulose fiber pores. Colloids Surf a: Physicochem Eng Asp 348:59–63. https://doi.org/10.1016/j.colsurfa.2009.06.032
Felby C, Thygesen LG, Kristensen JB, Jørgensen H, Elder T (2008) Cellulose–water interactions during enzymatic hydrolysis as studied by time domain NMR. Cellulose 15:703–710. https://doi.org/10.1007/s10570-008-9222-8
Fukuzumi H, Saito T, Iwata T, Kumamoto Y, Isogai A (2009) Transparent and high gas barrier films of cellulose nanofibers prepared by TEMPO-mediated oxidation. Biomacromol 10(1):162–165. https://doi.org/10.1021/bm801065u
Geng L, Peng X, Zhan C, Naderi A, Sharma PR, Mao Y, Hsiao BS (2017) Structure characterization of cellulose nanofiber hydrogel as functions of concentration and ionic strength. Cellulose 24:5417–5429. https://doi.org/10.1007/s10570-017-1496-2
Glatter O (1980a) Evaluation of small-angle scattering data from lamellar and cylindrical particles by the indirect transformation method. J Appl Crystallogr 13:577–584. https://doi.org/10.1107/S0021889880012794
Glatter O (1980b) Determination of particle-size distribution functions from small-angle scattering data by means of the indirect transformation method. J Appl Crystallogr 13:7–11. https://doi.org/10.1107/S0021889880011429
Guan QF, Yang HB, Han ZM, Zhou LC, Zhu YB, Ling ZC, Jiang HB, Wang PF, Ma T, Wu HA, Yu SH (2020) Lightweight, tough, and sustainable cellulose nanofiber-derived bulk structural materials with low thermal expansion coefficient. Sci Adv 6(18):1114. https://doi.org/10.1126/sciadv.aaz1114
Iwamoto S, Lee SH, Endo T (2014) Relationship between aspect ratio and suspension viscosity of wood cellulose nanofibers. Polym J 46:73–76. https://doi.org/10.1038/pj.2013
Iwatake A, Nogi M, Yano H (2008) Cellulose nanofiber-reinforced polylactic acid. Compos Sci Technol 68:2103–2106. https://doi.org/10.1016/j.compscitech.2008.03.006
Jia X, Chen Y, Shi C, Ye Y, Abid M, Jabbar S, Wang P, Zeng X, Wu T (2014) Rheological properties of an amorphous cellulose suspension. Food Hydrocoll 39:27–33. https://doi.org/10.1016/j.foodhyd.2013.12.026
Kamtsikakis A, McBride S, Zoppe JO, Weder C (2021) Cellulose nanofiber nanocomposite pervaporation membranes for ethanol recovery. ACS Appl Nano Mater 4(1):568–579. https://doi.org/10.1021/acsanm.0c02881
Karpovich A, Vlasova M, Sapronova N, Sukharev V, Ivanov V (2016) Exfoliation dynamics of laponite clay in aqueous suspensions studied by NMR relaxometry. Orient J Chem 32:1679–1683. https://doi.org/10.13005/ojc/320346
Kasuga T, Isobe N, Yagyu H, Koga H, Nogi M (2018) Clearly transparent nanopaper from highly concentrated cellulose nanofiber dispersion using dilution and sonication. Nanomater 8:104. https://doi.org/10.3390/nano8020104
Kumagai A, Tajima N, Iwamoto S, Morimoto T, Nagatani A, Okazaki T, Endo T (2019) Properties of natural rubber reinforced with cellulose nanofibers based on fiber diameter distribution as estimated by differential centrifugal sedimentation. Int J Biol Macromol 121:989–995. https://doi.org/10.1016/j.ijbiomac.2018.10.090
Kumagai A, Endo T (2021) Effects of hemicellulose composition and content on the interaction between cellulose nanofibers. Cellulose 28:259–271. https://doi.org/10.1007/s10570-020-03530-x
Li MC, Wu Q, Song K, Lee S, Qing Y, Wu Y (2015) Cellulose nanoparticles: structure–morphology–rheology. ACS Sustain Chem Eng 3:821–832. https://doi.org/10.1021/acssuschemeng.5b00144
Lohrasbi S, Mirzaei E, Karimizade A, Takallu S, Rezaei A (2020) Collagen/cellulose nanofiber hydrogel scaffold: physical, mechanical and cell biocompatibility properties. Cellulose 27:927–940. https://doi.org/10.1007/s10570-019-02841-y
Murase R, Kondo S, Kitamura T, Goi Y, Hashimoto M, Teramoto Y (2018) Cellulose nanofibers as a module for paper-based microfluidic analytical devices: Labile substance storage, processability, and reaction field provision and control. ACS Appl Bio Mater 1(2):480–486. https://doi.org/10.1021/acsabm.8b00206
Nakagaito AN, Yano H (2005) Novel high-strength biocomposites based on microfibrillated cellulose having nano-order-unit web-like network structure. Appl Phys A 80:155–159. https://doi.org/10.1007/s00339-003-2225-2
Paruthi A, Misra SK (2017) Relaxation time: a proton NMR-based approach as a metric to measure reactivity of engineered nanomaterials. J Nanopart Res 19:292. https://doi.org/10.1007/s11051-017-3962-z
Segal L, Creely JJ, Martin AE Jr, Conrad CM (1959) An emprical method for estimating the degree of crystallinity of native cellulose using the X-ray diffractometer. Text Res J 29:786–794. https://doi.org/10.1177/004051755902901003
Silva CEP, Tam KC, Bernardes JS, Loh W (2020) Double stabilization mechanism of O/W Pickering emulsions using cationic nanofibrillated cellulose. J Colloid Interface Sci 574:207–216. https://doi.org/10.1016/j.jcis.2020.04.001
Silva TCF, Habibi Y, Colodette JL (2012) A fundamental investigation of the microarchitecture and mechanical properties of tempo-oxidized nanofibrillated cellulose (NFC)-based aerogels. Cellulose 19:1945–1956. https://doi.org/10.1007/s10570-012-9761-x
Suekuni MT, D’Souza N, Allgeier AM (2022) NMR relaxometry studies on the drying kinetics of cellulose nanofibers. Ind Eng Chem Res 61:5475–5483. https://doi.org/10.1021/acs.iecr.1c04878
Sugino Machine Limited (2021) https://www.sugino.com/site/biomass-nanofiber-e/lineup.html. Accessed 30 Jul 2021
Takai-Yamashita C, Mabuchi Y, Senna M, Fuji M, Ohya Y, Yamagata Y (2021a) Microstructure and surface aactivity of mechanically-dispersed nanofiber aqueous sol. Cellulose 28:775–785. https://doi.org/10.1007/s10570-020-03570-3
Takai-Yamashita C, Mabuchi Y, Ikeda J, Fuji M, Senna M, Ohya Y (2021b) Physicochemical effects and surface activity of cellulose nanofiber sols induced by a planetary ball milling treatment. J Soc Powder Technol Japan 58:164–169. https://doi.org/10.4164/sptj.58.164(inJapanese)
Takai-Yamashita C, Sato E, Fuji M (2020) NMR as a tool to characterize the aggregation structure of silica nanoparticles in a liquid. KONA Powder Particle J 37:233–243. https://doi.org/10.14356/kona.2020012
Takeno H, Inoguchi H, Hsieh WC (2020) Mechanical and structural properties of cellulose nanofiber/poly(vinyl alcohol) hydrogels cross-linked by a freezing/thawing method and borax. Cellulose 27:4373–4387. https://doi.org/10.1007/s10570-020-03083-z
Teixeira J (1988) Small-angle scattering by fractal systems. J Appl Crystallograph 21:781–785. https://doi.org/10.1107/S0021889888000263
Tominaga Y, Sato K, Hotta Y, Shibuya H, Sugie M, Saruyama T (2019) Effect of the addition of Al2O3 and h-BN fillers on the thermal conductivity of a cellulose nanofiber/nanodiamond composite film. Cellulose 26:5281–5289. https://doi.org/10.1007/s10570-019-02488-9
Zuluaga R, Putaux JL, Restrepo A, Mondragon I, Gañán P (2007) Cellulose microfibrils from banana farming residues: isolation and characterization. Cellulose 14:585–592. https://doi.org/10.1007/s10570-007-9118-
Acknowledgements
The authors are particularly grateful for the assistance given by Mr. Takashi Kikkawa and Ms. Kazumi Tanikawa from Sanyo Trading Co., Ltd., for the technical support (Turbiscan and DCS) and Mr. Ryohei Nojiri from Nagoya Institute of Tehnology, Japan. The authors also like to express our gratitude to a part of this study supported by Leading Initiative for Excellent Young Researchers (LEADER) of MEXT, and Hosokawa Powder Foundation, Information Center of Powder Technology, Project to Enhance Innovation Creation Environment for National Universities, Foundation of Public Interest of Tatematsu, Knowledge Hub Aichi, and Future Fiber Factory (FFF) in Gifu University.
Funding
That research was supported Leading Initiative for Excellent Young Researchers (LEADER) of Ministry of Education, Culture, Sports, Science and Technology (MEXT). Hosokawa Powder Foundation, Japan. The Information Center of Particle Technology, Japan. Project to Enhance Innovation Creation Environment for National Universities. Foundation of Public Interest of Tatematsu. Knowledge Hub Aichi.
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Conceptualization: CTY, JI, Data curation: CT-Y, JI, YY, YT, YW, Funding acquisition: CT-Y and MF, Investigation: CT-Y, JI, YW, YY and YT, Project administration: CT-Y, Resources: CT-Y, MF, YY, YT and YO, Supervision: CT-Y, Validation: CT-Y, Visualization: CT-Y, Writing—original draft: CT-Y, Writing—review and editing: CT-Y, JI, MS, MF, YO, YY and YT. The paper has been carefully revised by a professional language editing service (International Technology Exchange Society (ITE)) to improve the grammar and readability.
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Takai-Yamashita, C., Ikeda, J., Wada, Y. et al. Change in the dispersion states of short-length-cellulose nanofibers upon dilution investigated by a time-domain nuclear magnetic resonance (TD-NMR). Cellulose 29, 7049–7062 (2022). https://doi.org/10.1007/s10570-022-04714-3
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DOI: https://doi.org/10.1007/s10570-022-04714-3