, Volume 26, Issue 1, pp 305–328 | Cite as

Effects of ball milling on the structure of cotton cellulose

  • Zhe Ling
  • Tuo Wang
  • Mohamadamin Makarem
  • Michael Santiago Cintrón
  • H. N. Cheng
  • Xue Kang
  • Markus Bacher
  • Antje Potthast
  • Thomas Rosenau
  • Holly King
  • Christopher D. Delhom
  • Sunghyun Nam
  • J. Vincent Edwards
  • Seong H. Kim
  • Feng Xu
  • Alfred D. FrenchEmail author
Original Paper


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.


Amorphous cellulose Ball milling Cellulose degradation Crystal structure Rietveld refinement 



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.

Supplementary material

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Supplementary material 1 (PDF 1818 kb)


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Authors and Affiliations

  • Zhe Ling
    • 1
    • 2
  • Tuo Wang
    • 3
  • Mohamadamin Makarem
    • 4
  • Michael Santiago Cintrón
    • 2
  • H. N. Cheng
    • 2
  • Xue Kang
    • 3
  • Markus Bacher
    • 5
  • Antje Potthast
    • 5
  • Thomas Rosenau
    • 5
  • Holly King
    • 2
  • Christopher D. Delhom
    • 2
  • Sunghyun Nam
    • 2
  • J. Vincent Edwards
    • 2
  • Seong H. Kim
    • 4
  • Feng Xu
    • 1
  • Alfred D. French
    • 2
    Email author
  1. 1.Beijing Key Laboratory of Lignocellulosic ChemistryBeijing Forestry UniversityBeijingPeople’s Republic of China
  2. 2.Southern Regional Research Center, Agricultural Research Service, USDANew OrleansUSA
  3. 3.Department of ChemistryLouisiana State UniversityBaton RougeUSA
  4. 4.Department of Chemical Engineering, Materials Science Research InstituteThe Pennsylvania State UniversityUniversity ParkUSA
  5. 5.Department of Chemistry, Division of Chemistry of Renewable ResourcesUniversity of Natural Resources and Life SciencesTullnAustria

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