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. French

Research output: Contribution to journalArticle

27 Citations (Scopus)

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.

Original languageEnglish (US)
Pages (from-to)305-328
Number of pages24
JournalCellulose
Volume26
Issue number1
DOIs
StatePublished - Jan 15 2019

Fingerprint

Ball milling
Cellulose
Cotton
X ray laboratories
Nuclear magnetic resonance
Polarization
Rietveld method
Cotton fibers
Gel permeation chromatography
Synchrotrons
Specific surface area
Field emission
Pore size
Optical microscopy
Fourier transform infrared spectroscopy
Raman spectroscopy
Thermogravimetric analysis
Fourier transforms
Tensile strength
Moisture

All Science Journal Classification (ASJC) codes

  • Polymers and Plastics

Cite this

Ling, Z., Wang, T., Makarem, M., Santiago Cintrón, M., Cheng, H. N., Kang, X., ... French, A. D. (2019). Effects of ball milling on the structure of cotton cellulose. Cellulose, 26(1), 305-328. https://doi.org/10.1007/s10570-018-02230-x
Ling, Zhe ; Wang, Tuo ; Makarem, Mohamadamin ; Santiago Cintrón, Michael ; Cheng, H. N. ; Kang, Xue ; Bacher, Markus ; Potthast, Antje ; Rosenau, Thomas ; King, Holly ; Delhom, Christopher D. ; Nam, Sunghyun ; Vincent Edwards, J. ; Kim, Seong H. ; Xu, Feng ; French, Alfred D. / Effects of ball milling on the structure of cotton cellulose. In: Cellulose. 2019 ; Vol. 26, No. 1. pp. 305-328.
@article{149fb4cfcc9143d09b72d04fd0e4f8da,
title = "Effects of ball milling on the structure of cotton cellulose",
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.",
author = "Zhe Ling and Tuo Wang and Mohamadamin Makarem and {Santiago Cintr{\'o}n}, Michael and Cheng, {H. N.} and Xue Kang and Markus Bacher and Antje Potthast and Thomas Rosenau and Holly King and Delhom, {Christopher D.} and Sunghyun Nam and {Vincent Edwards}, J. and Kim, {Seong H.} and Feng Xu and French, {Alfred D.}",
year = "2019",
month = "1",
day = "15",
doi = "10.1007/s10570-018-02230-x",
language = "English (US)",
volume = "26",
pages = "305--328",
journal = "Cellulose",
issn = "0969-0239",
publisher = "Springer Netherlands",
number = "1",

}

Ling, Z, Wang, T, Makarem, M, Santiago Cintrón, M, Cheng, HN, Kang, X, Bacher, M, Potthast, A, Rosenau, T, King, H, Delhom, CD, Nam, S, Vincent Edwards, J, Kim, SH, Xu, F & French, AD 2019, 'Effects of ball milling on the structure of cotton cellulose', Cellulose, vol. 26, no. 1, pp. 305-328. https://doi.org/10.1007/s10570-018-02230-x

Effects of ball milling on the structure of cotton cellulose. / Ling, Zhe; Wang, Tuo; Makarem, Mohamadamin; Santiago Cintrón, Michael; Cheng, H. N.; Kang, Xue; Bacher, Markus; Potthast, Antje; Rosenau, Thomas; King, Holly; Delhom, Christopher D.; Nam, Sunghyun; Vincent Edwards, J.; Kim, Seong H.; Xu, Feng; French, Alfred D.

In: Cellulose, Vol. 26, No. 1, 15.01.2019, p. 305-328.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Effects of ball milling on the structure of cotton cellulose

AU - Ling, Zhe

AU - Wang, Tuo

AU - Makarem, Mohamadamin

AU - Santiago Cintrón, Michael

AU - Cheng, H. N.

AU - Kang, Xue

AU - Bacher, Markus

AU - Potthast, Antje

AU - Rosenau, Thomas

AU - King, Holly

AU - Delhom, Christopher D.

AU - Nam, Sunghyun

AU - Vincent Edwards, J.

AU - Kim, Seong H.

AU - Xu, Feng

AU - French, Alfred D.

PY - 2019/1/15

Y1 - 2019/1/15

N2 - 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.

AB - 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.

UR - http://www.scopus.com/inward/record.url?scp=85056318187&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=85056318187&partnerID=8YFLogxK

U2 - 10.1007/s10570-018-02230-x

DO - 10.1007/s10570-018-02230-x

M3 - Article

AN - SCOPUS:85056318187

VL - 26

SP - 305

EP - 328

JO - Cellulose

JF - Cellulose

SN - 0969-0239

IS - 1

ER -

Ling Z, Wang T, Makarem M, Santiago Cintrón M, Cheng HN, Kang X et al. Effects of ball milling on the structure of cotton cellulose. Cellulose. 2019 Jan 15;26(1):305-328. https://doi.org/10.1007/s10570-018-02230-x