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Effects of ball milling on the structure of cotton cellulose

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Abstract

Cellulose is often described as a mixture of crystalline and amorphous material. A large part of the general understanding of the chemical, biochemical and physical properties of cellulosic materials is thought to depend on the consequences of the ratio of these components. For example, amorphous materials are said to be more reactive and have less tensile strength but comprehensive understanding and definitive analysis remain elusive. Ball milling has been used for decades to increase the ratio of amorphous material. The present work used 13 techniques to follow the changes in cotton fibers (nearly pure cellulose) after ball milling for 15, 45 and 120 min. X-ray diffraction results were analyzed with the Rietveld method; DNP (dynamic nuclear polarization) natural abundance 2D NMR studies in the next paper in this issue assisted with the interpretation of the 1D analyses in the present work. A conventional NMR model’s paracrystalline and inaccessible crystallite surfaces were not needed in the model used for the DNP studies. Sum frequency generation (SFG) spectroscopy also showed profound changes as the cellulose was decrystallized. Optical microscopy and field emission-scanning electron microscopy results showed the changes in particle size; molecular weight and carbonyl group analyses by gel permeation chromatography confirmed chemical changes. Specific surface areas and pore sizes increased. Fourier transform infrared (FTIR) and Raman spectroscopy also indicated progressive changes; some proposed indicators of crystallinity for FTIR were not in good agreement with our results. Thermogravimetric analysis results indicated progressive increase in initial moisture content and some loss in stability. Although understanding of structural changes as cellulose is amorphized by ball milling is increased by this work, continued effort is needed to improve agreement between the synchrotron and laboratory X-ray methods used herein and to provide physical interpretation of the SFG results.

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Notes

  1. Even though cotton has a high microfibril angle (French and Kim 2018) or range of deviations of alignment of microfibrils to the fiber axis, for this discussion the alignment of adjacent microfibrils can be considered to be antiparallel.

  2. Despite its simplicity, the Segal method is sometimes used incorrectly. The Segal CrI depends on the intensity minimum between the (110) and (200) peaks, as well as the peak intensity of the (200) reflection. However, authors have too-often chosen the (110) or combined (1–10) and (110) peak as representing the amorphous material. Furthermore, for material to be represented by the minimum intensity near 18 deg. (copper Kα radiation), the background must be subtracted. Typically, this would mean subtraction of a blank.

References

  • Agarwal UP (2014) 1064 nm FT-Raman spectroscopy for investigations of plant cell walls and other biomass materials. Front Plant Sci 5:490

    Article  PubMed  PubMed Central  Google Scholar 

  • Agarwal UP, Ralph SA (1997) FT-Raman spectroscopy of wood: identifying contributions of lignin and carbohydrate polymers in the spectrum of black spruce (Picea mariana). Appl Spectrosc 51:1648–1655. https://doi.org/10.1366/0003702971939316

    Article  CAS  Google Scholar 

  • Agarwal UP, Ralph SA, Reiner RS, Baez C (2016) Probing crystallinity of never-dried wood cellulose with Raman spectroscopy. Cellulose 23:125–144. https://doi.org/10.1007/s10570-015-0788-7

    Article  CAS  Google Scholar 

  • Ahvenainen P, Kontro I, Svedström K (2016) Comparison of sample crystallinity determination methods by X-ray diffraction for challenging cellulose I materials. Cellulose 23:1073–1086

    Article  CAS  Google Scholar 

  • Atalla RH, Vanderhart DL (1984) Native cellulose: a composite of two distinctive crystalline forms. Science 223:283–285

    Article  CAS  PubMed  Google Scholar 

  • Atalla RH, Gast JC, Sindorf DW, Bartuska VJ, Maciel GE (1980) Carbon-13 NMR spectra of cellulose polymorphs. J Am Chem Soc 102(9):3249–3251

    Article  CAS  Google Scholar 

  • Barnette AL, Bradley LC, Veres BD, Schreiner EP, Park J, Park S, Kim SH (2011) Selective detection of crystalline cellulose in plant cell walls with sum frequency generation (SFG) vibration spectroscopy. Biomacromolecules 12:2434–2439

    Article  CAS  PubMed  Google Scholar 

  • Barnette AL, Lee C, Bradley LC, Schreiner EP, Park H, Shin H, Cosgrove DJ, Park S, Kim SH (2012) Quantification of crystalline cellulose in lignocellulosic biomass using sum frequency generation (SFG) vibration spectroscopy and comparison with other analytical methods. Carbohydr Polym 89:802–809

    Article  CAS  PubMed  Google Scholar 

  • Bertran MS, Dale BE (1986) Determination of cellulose accessibility by differential scanning calorimetry. J Appl Polym Sci 32:4241–4253

    Article  CAS  Google Scholar 

  • Brunauer S, Emmett PH, Teller E (1938) Adsorption of gases in multimolecular layers. J Am Chem Soc 60:309–319

    Article  CAS  Google Scholar 

  • Chen L, Wang Q, Hirth K, Baez C, Agarwal UP, Zhu JY (2015) Tailoring the yield and characteristics of wood cellulose nanocrystals (CNC) using concentrated acid hydrolysis. Cellulose 22:1753–1762

    Article  CAS  Google Scholar 

  • Dollase WA (1986) Correction of intensities for preferred orientation in powder diffractometry: application of the March model. J Appl Crystallogr 19(4):267–272

    Article  CAS  Google Scholar 

  • Driemeier C (2014) Two-dimensional Rietveld analysis of celluloses from higher plants. Cellulose 21:1065–1073

    Article  CAS  Google Scholar 

  • Driemeier C, Calligaris GA (2011) Theoretical and experimental developments for accurate determination of crystallinity of cellulose I materials. J Appl Cryst 44:184–192

    Article  CAS  Google Scholar 

  • Driemeier C, Francisco LH (2014) X-ray diffraction from faulted cellulose I constructed with mixed Iα–Iβ stacking. Cellulose 21:3161–3169

    Article  CAS  Google Scholar 

  • Duchemin B (2017) Size, shape, orientation and crystallinity of cellulose Iβ by X-ray powder diffraction using a free spreadsheet program. Cellulose 24:2727–2741

    Article  CAS  Google Scholar 

  • Forziati FH, Stone WK, Rowen JW, Appel WD (1950) Cotton powder for infrared transmission measurements. J Res Nat Bur Stand 45:109–113

    Article  Google Scholar 

  • Foston MB, Hubbell CA, Ragauskas AJ (2011) Cellulose isolation methodology for NMR analysis of cellulose ultrastructure. Materials 4:1985–2002

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  • French AD (2012) Combining computational chemistry and crystallography for a better understanding of the structure of cellulose. Horton D, ed. Adv Carbohydr Chem Biochem 67:19–93

    Article  CAS  PubMed  Google Scholar 

  • French AD (2014) Idealized powder diffraction patterns for cellulose polymorphs. Cellulose 21:885–896. https://doi.org/10.1007/s10570-013-0030-4

    Article  CAS  Google Scholar 

  • French AD, Kim HJ (2018) Cotton fiber structure. In: Fang D (ed) Cotton fiber, physics and biology. Springer, New York, pp 13–39. https://doi.org/10.1007/978-3-030-00871-0_2

    Chapter  Google Scholar 

  • French AD, Santiago Cintrón M (2013) Cellulose polymorphy, crystallite size, and the Segal crystallinity index. Cellulose 20:583–588

    Article  CAS  Google Scholar 

  • French AD, Pérez S, Bulone V, Rosenau T, Gray D (2018) Cellulose, in encyclopedia of polymer science and technology. https://doi.org/10.1002/0471440264.pst042.pub2

  • Harris DM, Corbin K, Wang T, Gutierrez R, Bertolo AL, Petti C, Smilgies D-M, Estevez JM, Bonetta D, Urbanowicz BR, Ehrhardt DW, Somerville CR, Rose JKC, Hong M, Debolt S (2012) Cellulose microfibril crystallinity is reduced by mutating C-terminal transmembrane region residues CESA1A903V and CESA3T942I of cellulose synthase. Proc Natl Acad Sci 109:4098–4103

    Article  PubMed  Google Scholar 

  • Hearle JWS (1958) A fringed fibril theory of structure in crystalline polymers. J Polym Sci 28:432–435

    Article  CAS  Google Scholar 

  • Holzwarth U, Gibson N (2011) The Scherrer equation versus the ‘Debye–Scherrer equation’. Nat Nanotechnol 6:534

    Article  CAS  PubMed  Google Scholar 

  • Howell C, Hastrup ACS, Jara R, Larsen FH, Goodell B, Jellison J (2011) Effects of hot water extraction and fungal decay on wood crystalline cellulose structure. Cellulose 18:1179–1190

    Article  CAS  Google Scholar 

  • Huang S, Makarem M, Kiemle SN, Hamedi H, Sau M, Cosgrove DJ, Kim SH (2018a) Inhomogeneity of cellulose microfibril assembly in plant cell walls revealed with sum frequency generation microscopy. J Phys Chem B 122:5006–5019

    Article  CAS  PubMed  Google Scholar 

  • Huang S, Makarem M, Kiemle SN, Zheng Y, Xin H, Ye D, Gomez EW, Gomez ED, Cosgrove DJ, Kim SH (2018b) Investigating dehydration-induced physical strains of cellulose microfibrils in plant cell walls. Carbohydr Polym 197:337–348

    Article  CAS  PubMed  Google Scholar 

  • Ilharco LM, Garcia AR, Silva JL, Ferreira FV (1997) Infrared approach to the study of adsorption on cellulose: influence of cellulose crystallinity on the adsorption of benzophenone. Langmuir 13(15):4126–4132

    Article  CAS  Google Scholar 

  • Isogai A, Atalla RH (1991) Amorphous celluloses stable in aqueous media: regeneration from SO2–amine solvent systems. J Polym Sci Part A Polym Chem 29:113–119

    Article  CAS  Google Scholar 

  • Kim U-J, Eom SH, Wada M (2010) Thermal decomposition of native cellulose: influence on crystallite size. Polym Degrad Stab 95:778–781

    Article  CAS  Google Scholar 

  • Kirui A, Ling Z, Kang X, Dickwella Widanage MC, Mentink-Vigier F, French AD, Wang T (2019) Atomic resolution of cotton cellulose structure enabled by dynamic nuclear polarization solid-state NMR. Cellulose. https://doi.org/10.1007/s10570-018-2095-6

    Article  PubMed  Google Scholar 

  • Klug HP, Alexander LE (1974) X-ray diffraction procedures: for polycrystalline and amorphous materials, 2nd edn. Wiley-VCH, New York, p 992. ISBN 0-471-49369-4

    Google Scholar 

  • Kono H, Numata Y (2006) Structural investigation of cellulose Iα and Iβ by 2D RFDR NMR spectroscopy: determination of sequence of magnetically inequivalent d-glucose units along cellulose chain. Cellulose 13:317–326

    Article  CAS  Google Scholar 

  • Langan P, Nishiyama Y, Chanzy H (2001) X-ray structure of mercerized cellulose II at 1 Å resolution. Biomacromolecules 2:410–416

    Article  CAS  PubMed  Google Scholar 

  • Larsson PT, Hult EL, Wickholm K, Pettersson E, Iversen T (1999) CP/MAS 13C NMR spectroscopy applied to structure and interaction studies on cellulose I. Solid State Nucl Magn Reson 15:31–40

    Article  CAS  PubMed  Google Scholar 

  • Lee CM, Mohamed NMA, Watts HD, Kubicki JD, Kim SH (2013) Sum-frequency-generation vibration spectroscopy and density functional theory calculations with dispersion corrections (DFT-D2) for cellulose Iα and Iβ. J Phys Chem B 117:6681–6692

    Article  CAS  PubMed  Google Scholar 

  • Lee C, Kafle K, Park Y-B, Kim SH (2014) Probing crystal structure and mesoscale assembly of cellulose microfibrils in plant cell walls, tunicate tests, and bacterial films using vibrational sum frequency generation (SFG) spectroscopy. Phys Chem Chem Phys 16:10844–10853

    Article  CAS  PubMed  Google Scholar 

  • Lee CM, Kafle K, Huang S, Kim SH (2015a) Multimodal broadband vibrational sum frequency generation (MM-BB-V-SFG) spectrometer and microscope. J Phys Chem B 120:102–116

    Article  CAS  PubMed  Google Scholar 

  • Lee CM, Kubicki JD, Xin B, Zhong L, Jarvis MC, Kim SH (2015b) Hydrogen bonding network and OH stretch vibration of cellulose: comparison of computational modeling with polarized IR and SFG spectra. J Phys Chem B 119:15138–15149

    Article  CAS  PubMed  Google Scholar 

  • Lee CM, Chen X, Weiss PA, Jensen L, Kim SH (2016a) Quantum mechanical calculations of vibrational sum-frequency-generation (SFG) spectra of cellulose: dependence of the CH and OH peak intensity on the polarity of cellulose chains within the SFG coherence domain. J Phys Chem Lett 8:55–60

    Article  CAS  PubMed  Google Scholar 

  • Lee CM, Dazen K, Kafle K, Moore A, Johnson DK, Park S, Kim SH (2016b) Correlations of apparent cellulose crystallinity determined by XRD, NMR, IR, Raman, & and SFG. Adv Polym Sci 27:115–131

    Google Scholar 

  • Liu Y, Kim HJ (2015) Use of attenuated total reflection fourier transform infrared (ATR FT-IR) Spectroscopy in direct, nondestructive, and rapid assessment of developmental cotton fibers grown in planta and in culture. Appl Spectrosc 69:1004–1010

    Article  CAS  PubMed  Google Scholar 

  • Liu Y, Thibodeaux D, Gamble G, Bauer P, VanDerveer D (2012) Comparative investigation of Fourier transform infrared (FT-IR) spectroscopy and X-ray diffraction (XRD) in the determination of cotton fiber crystallinity. Appl Spectrosc 66:983–986

    Article  CAS  PubMed  Google Scholar 

  • Lutterotti L, Bortolotti M, Ischia G, Lonardelli I, Wenk H-R (2007) Rietveld texture analysis from diffraction images. Z Kristallogr Suppl 26:125–130

    Article  Google Scholar 

  • Makarem M, Lee CM, Sawada D, O’Neill HM, Kim SH (2017) Distinguishing surface versus bulk hydroxyl groups of cellulose nanocrystals using vibrational sum frequency generation spectroscopy. J Phys Chem Letts 9:70–75

    Article  CAS  Google Scholar 

  • Makarem M, Lee CM, Kafle K, Huang S, Chae I, Yang H, Kubicki JD, Kim SH (2019) Probing cellulose structures with vibrational spectroscopy. Cellulose. https://doi.org/10.1007/s10570-015-0788-7

    Article  Google Scholar 

  • Massiot D, Fayon F, Capron M, King I, Le Calvé S, Alonso B, Durand J-O, Bujoli B, Gan Z, Hoatson G (2002) Modelling one-and two-dimensional solid-state NMR spectra. Magn Reson Chem 40:70–76

    Article  CAS  Google Scholar 

  • Mihranyan A, Llagostera AP, Karmhag R, Strømme M, Ek R (2004) Moisture sorption by cellulose powders of varying crystallinity. Int J Pharm 269:433–442

    Article  CAS  PubMed  Google Scholar 

  • Millett MA, Effland MJ, Caulfield DF (1979) Influence of fine grinding on the hydrolysis of cellulosic materials-acid vs. enzymatic. Adv Chem Ser 181:71–89

    Article  Google Scholar 

  • Nelson ML, O’Connor RT (1964a) Relation of certain infrared bands to cellulose crystallinity and crystal lattice type. Part I. Spectra of lattice types I, II, III and of amorphous cellulose. J Appl Polym Sci 8:1311–1324

    Article  CAS  Google Scholar 

  • Nelson ML, O’Connor RT (1964b) Relation of certain infrared bands to cellulose crystallinity and crystal lattice type. Part II. A new infrared ratio for estimation of crystallinity in celluloses I and II. J Appl Polym Sci 8:1325–1341. https://doi.org/10.1002/app.1964.070080323

    Article  CAS  Google Scholar 

  • Newman RH, Hemmingson JA (1990) Determination of the degree of cellulose crystallinity in wood by carbon-13 nuclear magnetic resonance spectroscopy. Holzforschung 44:351–356

    Article  CAS  Google Scholar 

  • Newman RH, Hill SJ, Harris PJ (2013) Wide-angle X-ray scattering and solid-state nuclear magnetic resonance data combined to test models for cellulose microfibrils in mung bean cell walls. Am Soc Plant Biol 163:1558–1567

    CAS  Google Scholar 

  • Nishiyama Y, Langan P, Chanzy H (2002) Crystal structure and hydrogen-bonding system in cellulose Iβ from synchrotron X-ray and neutron fiber diffraction. J Am Chem Soc 124:9074–9082

    Article  CAS  PubMed  Google Scholar 

  • Nishiyama Y, Sugiyama J, Chanzy H, Langan P (2003a) Crystal structure and hydrogen bonding system in cellulose Iα from synchrotron x-ray and neutron fiber diffraction. J Am Chem Soc 125:14300–14306. https://doi.org/10.1021/ja037055w

    Article  CAS  PubMed  Google Scholar 

  • Nishiyama Y, Kim U-J, Kim D-Y, Katsumata KS, May RP, Langan P (2003b) Periodic disorder along ramie cellulose microfibrils. Biomacromolecules 4:1013–1017

    Article  CAS  PubMed  Google Scholar 

  • Oh SY, Yoo D, Shin Y, Kim HC, Kim HY et al (2005) Crystalline structure analysis of cellulose treated with sodium hydroxide and carbon dioxide by means of X-ray diffraction and FTIR spectroscopy. Carbohydr Res 340:2376–2391

    Article  CAS  PubMed  Google Scholar 

  • Park S, Baker JO, Himmel ME, Parrilla PA, Johnson DK (2010) Cellulose crystallinity index: measurement techniques and their impact on interpreting cellulase performance. Biotechnol Biofuels 3:10

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  • Park YB, Lee CM, Koo B-W, Park S, Cosgrove DJ, Kim SH (2013) Monitoring meso-scale ordering of cellulose in intact plant cell walls using sum frequency generation (SFG) spectroscopy. Plant Physiol 163:907–913

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  • Phyo P, Wang T, Yang Y, O’Neill H, Hong M (2018) Direct determination of hydroxymethyl conformations of plant cell wall cellulose using 1H polarization transfer solid-state NMR. Biomacromolecules 19:1485–1497

    Article  CAS  PubMed  Google Scholar 

  • Popa NC, Balzar D (2008) Size‐broadening anisotropy in whole powder pattern fitting. Application to zinc oxide and interpretation of the apparent crystallites in terms of physical models. J Appl Cryst 41:615–627

    Article  CAS  Google Scholar 

  • Reyes DCA, Skoglund N, Svedberg A, Eliasson B, Sundman O (2016) The influence of different parameters on the mercerisation of cellulose for viscose production. Cellulose 23:1061–1072

    Article  CAS  Google Scholar 

  • Rietveld H (1969) A profile refinement method for nuclear and magnetic structures. J Appl Crystallogr 2:65–71

    Article  CAS  Google Scholar 

  • Rodriguez-Navarro AB (2006) XRD2DScan: new software for polycrystalline materials characterization using two-dimensional X-ray diffraction. J Appl Crystallogr 39:905–909

    Article  CAS  Google Scholar 

  • Röhrling J, Potthast A, Rosenau T, Lange T, Borgards A, Sixta H, Kosma P (2002) A novel method for the determination of carbonyl groups in cellulosics by fluorescence labeling. 2. Validation and applications. Biomacromolecules 3:969–975

    Article  CAS  PubMed  Google Scholar 

  • Rollin JA, Zhu Z, Sathitsuksanoh N, Zhang YP (2011) Increasing cellulose accessibility is more important than removing lignin: a comparison of cellulose solvent-based lignocellulose fractionation and soaking in aqueous ammonia. Biotechnol Bioeng 108:22–30

    Article  CAS  PubMed  Google Scholar 

  • Sarko A, Nishimura H, Okano T (1987) Crystalline alkali-celllulose complexes as intermediates during mercerization. ACS Symp Ser 340:169–177

    Article  CAS  Google Scholar 

  • Schenzel K, Fischer S, Brendler E (2005) New method for determining the degree of cellulose I crystallinity by means of FT Raman spectroscopy. Cellulose 12:223–231. https://doi.org/10.1007/s10570-004-3885-6

    Article  CAS  Google Scholar 

  • Schroeder LR, Gentile VM, Atalla RH (1986) Nondegradative preparation of amorphous cellulose. J Wood Chem Technol 6:1–14

    Article  CAS  Google Scholar 

  • Schultz TP, McGinnis GD, Bertran MS (1985) Estimation of cellulose crystallinity using Fourier transform-infrared spectroscopy and dynamic thermogravimetry. J Wood Chem Technol 5:543–557

    Article  CAS  Google Scholar 

  • Segal L, Creely JJ, Martin AE, Conrad CM (1959) An empirical 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

    Article  CAS  Google Scholar 

  • Sehaqui H, Zhou Q, Berglund LA (2011) High-porosity aerogels of high specific surface area prepared from nanofibrillated cellulose (NFC). Compos Sci Technol 71:1593–1599

    Article  CAS  Google Scholar 

  • Shibazaki H, Kuga S, Okano T (1997) Mercerization and acid hydrolysis of bacterial cellulose. Cellulose 4:75–87

    Article  CAS  Google Scholar 

  • Solala I, Henniges U, Pirker KF, Rosenau T, Potthast A, Vuorinen T (2015) Mechanochemical reactions of cellulose and styrene. Cellulose 22:3217–3224

    Article  CAS  Google Scholar 

  • Stefanovic B, Pirker KF, Rosenau T, Potthast A (2014) Effects of tribochemical treatments on the integrity of cellulose. Carbohydr Polym 111:688–699

    Article  CAS  PubMed  Google Scholar 

  • Sugiyama J, Persson J, Chanzy H (1991) Combined infrared and electron diffraction study of the polymorphism of native celluloses. Macromolecules 24:2461–2466

    Article  CAS  Google Scholar 

  • Takahashi H, Lee D, Dubois L, Bardet M, Hediger S, De Paëpe G (2012) Rapid natural-abundance 2D 13C–13C correlation spectroscopy using dynamic nuclear polarization enhanced solid-state NMR and matrix-free sample preparation. Angew Chem Int Ed 51:11766–11769

    Article  CAS  Google Scholar 

  • Thygesen A, Oddershede J, Lilholt H, Thomsen AB, Ståhl K (2005) On the determination of crystallinity and cellulose content in plant fibres. Cellulose 12:563–576

    Article  CAS  Google Scholar 

  • Vanderfleet OM, Reid MS, Bras J, Heux L, Godoy-Vargas J, Panga MKR, Cranston ED (2019) Insight into thermal stability of cellulose nanocrystals from new hydrolysis methods with acid blends. Cellulose. https://doi.org/10.1007/s10570-018-2175-7

    Article  Google Scholar 

  • Vieira FS, Pasquini C (2014) Determination of cellulose crystallinity by terahertz-time domain spectroscopy. Anal Chem 86:3780–3786

    Article  CAS  PubMed  Google Scholar 

  • Viëtor RJ, Newman RH, Ha MA, Apperley DC, Jarvis MC (2002) Conformational features of crystal-surface cellulose from higher plants. Plant J 30(6):721–731

    Article  PubMed  Google Scholar 

  • Wang T, Hong M (2016) Solid-state NMR investigations of cellulose structure and interactions with matrix polysaccharides in plant primary cell walls. J Exp Bot 67:503–514

    Article  CAS  PubMed  Google Scholar 

  • Wertz J-L, Mercier JP, Bédué O (2010) Cellulose science and technology. Routledge, Taylor & Francis Group

    Book  Google Scholar 

  • Wickholm K, Larsson PT, Iversen T (1998) Assignment of non-crystalline forms in cellulose I by CP/MAS 13C NMR spectroscopy. Carbohydr Res 312:123–129

    Article  CAS  Google Scholar 

  • Wiley JH, Atalla RH (1987) Band assignments in the Raman spectra of celluloses. Carbohydr Res 160:113–129

    Article  CAS  Google Scholar 

  • Xiaohui J, Bowden M, Brown EE, Zhang X (2015) An improved X-ray diffraction method for cellulose crystallinity measurement. Carbohydr Polym 123:476–481

    Article  CAS  Google Scholar 

  • Yang H, Wang T, Oehme D, Petridis L, Hong M, Kubicki JD (2018) Structural factors affecting 13C NMR chemical shifts of cellulose: a computational study. Cellulose 25:23–36

    Article  CAS  Google Scholar 

  • Young RA (ed) (1993) The Rietveld method. IUCr Monographs in crystallography. 5. International Union of Crystallography. Oxford University Press, New York, p 298

    Google Scholar 

Download references

Acknowledgments

The authors gratefully acknowledged the support by Chinese Scholarship Council (CSC No. 201706510045) for ZL. The NMR work was supported by National Science Foundation (NSF OIA-1833040). The SFG work was supported by the Center for Lignocellulose Structure and Formation, Energy Frontier Research Center funded by the U.S. Department of Energy, Office of Science, Basic Energy Sciences, under Award Number DE-SC0001090. Prof. Nathaniel C. Gilbert at CAMD kindly helped with the synchrotron X-ray diffraction analysis, and Dr. Dongmei Cao at the Louisiana State University Shared Instrument Facility provided the FE-SEM micrographs. Stephanie Beck of FPInnovations and Hee Jin Kim of the Southern Regional Research Center reviewed the manuscript. Acknowledgements are also made to Catrina Ford for technical assistance. Mention of trade names or commercial products in this publication is solely for the purpose of providing specific information and does not imply recommendation or endorsement by the U.S. Department of Agriculture. USDA is an equal opportunity provider and employer.

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Authors and Affiliations

  1. Beijing Key Laboratory of Lignocellulosic Chemistry, Beijing Forestry University, Beijing, 100083, People’s Republic of China

    Zhe Ling & Feng Xu

  2. Southern Regional Research Center, Agricultural Research Service, USDA, 1100 Robert E. Lee Blvd., New Orleans, LA, 70124, USA

    Zhe Ling, Michael Santiago Cintrón, H. N. Cheng, Holly King, Christopher D. Delhom, Sunghyun Nam, J. Vincent Edwards & Alfred D. French

  3. Department of Chemistry, Louisiana State University, Baton Rouge, LA, 70803, USA

    Tuo Wang & Xue Kang

  4. Department of Chemical Engineering, Materials Science Research Institute, The Pennsylvania State University, University Park, PA, 16802, USA

    Mohamadamin Makarem & Seong H. Kim

  5. Department of Chemistry, Division of Chemistry of Renewable Resources, University of Natural Resources and Life Sciences, Konrad-Lorenz-Str. 24, 3430, Tulln, Austria

    Markus Bacher, Antje Potthast & Thomas Rosenau

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Ling, Z., Wang, T., Makarem, M. et al. Effects of ball milling on the structure of cotton cellulose. Cellulose 26, 305–328 (2019). https://doi.org/10.1007/s10570-018-02230-x

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