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Production and Applications of Cellulose Nanomaterials Production and Applications of Cellulose Nanomaterials Compiled and Edited by: Michael T. Postek Robert J. Moon Alan W. Rudie and Michael A. Bilodeau Cellulose nanocrystals incorporated within the overcoat varnish of the cover! Cover: Transmission electron microscope (TEM) image of CNCs extracted from microcrystalline cellulose; original micrograph from Moon et al., “Cellulose Nanocrystals—a material with unique properties and many potential applications,” colorized by Michael Postek. Certain commercial equipment is identified in this report to adequately describe the experimental procedure. Such identification does not imply recommendation or en- dorsement by the National Institute of Standards and Technology or the Forest Products Laboratory, nor does it imply that the equipment identified is necessarily the best avail- able for the purpose. Credits for figures on the next page: Koga and Kitaoka: Crystalline Cellulose Nanofibrils Conjugated with Metal Nanocatalysts Kangas: Cellulose nanofibrils: A class of materials with unique properties and numerous potential applications Postek and Vladar: Dimensional Metrology and Imaging of Cellulose Nanocrystals i Copyright© 2013 by TAPPI PRESS 15 Technology Parkway South Suite 115 Peachtree Corners, GA 30092 U.S.A. www.tappi.org All rights reserved The Association assumes no liability or responsibility in connection with the use of this information or data, including, but not limited to, any liability or responsibility under patent, copyright, or trade secret laws. The user is responsible for determining that this document is the most recent edition published. Certain portions of this book may not be reproduced, stored in a retrieval system, or transmitted by any means – electronic, mechanical, photocopying, recording, or otherwise – without the written permission of the copyright owner. Other portions of this book were written and/or prepared by U.S. Government employees on official time and are therefore in the public domain and not subject to copyright. To obtain copyright permission to photocopy pages from this publication for internal or personal use, or to use excerpts from this publication in another published work, contact Copyright Clearance Center, Inc. (CCC) via their website at www.copyright.com. If you have questions about the copyright permission request process, please contact CCC by phone at +1-978-750-8400. ISBN: 978-1-59510-224-9 TAPPI PRESS Order Number: 0101R332 Printed in the United States of America ii Production and Applications of Cellulose Nanomaterials Production and Applications of Cellulose Nanomaterials Michael T. Postek National Institute of Standards and Technology Robert J. Moon USDA Forest Service, Forest Products Laboratory, School of Materials Engineering, and the Birck Nanotechnology Center, Purdue University Alan W. Rudie USDA Forest Service, Forest Products Laboratory and Michael A. Bilodeau University of Maine, Process Development Center June 2013 Production and Applications of Cellulose Nanomaterials iii Table of Contents Foreword Michael T. Postek, Robert J. Moon, Alan W. Rudie, Michael A. Bilodeau .....................................................................................1 Introduction Cellulosic Nanomaterials: Sustainable Materials of Choice for the 21st Century Theodore H. Wegner, Sean Ireland and J. Philip E. Jones..............................................................................................................3 Chapter 1: Cellulose Nanocrystals Cellulose Nanocrystals – A Material with Unique Properties and Many Potential Applications Robert Moon, Stephanie Beck and Alan Rudie ........................................................................................................................9 1.1 Preparation and Characterization Cellulose Nanocrystals: Extraction from Bio-residues Martha Herrera, Aji Mathew and Kristiina Oksman ...............................................................................................................13 Thermally Stable Cellulose Nanocrystals Isolated By Phosphoric Acid Hydrolysis Sandra Camarero Espinosa, Tobias Kuhnt, Christoph Weder and E. Johan Foster ..............................................................17 Process Scale-Up of Cellulose Nanocrystal Production to 25 kg per Batch at the Forest Products Laboratory Richard S. Reiner and Alan W. Rudie .......................................................................................................................................21 Green Synthesis, Modification and Properties of Carboxylated Cellulose Nanocrystals usingAmmonium Persulfate Alfred C.W. Leung, Edmond Lam and John H.T. Luong ..........................................................................................................25 Production of Reference Materials for Cellulose Nanocrystals (CNC) Ralph E. Sturgeon and Patricia Grinberg ................................................................................................................................29 Drying Cellulose Nanocrystal Suspensions Yucheng Peng, Douglas J. Gardner, Yousoo Han, Zhiyong Cai and Mandla A. Tshabalala ...................................................31 . Dispersibility of Dried Cellulose Nanocrystals in Water Stephanie Beck, Jean Bouchard and Richard Berry ................................................................................................................35 Dimensional Metrology and Imaging of Cellulose Nanocrystals Michael T. Postek and András E. Vladár .................................................................................................................................37 Atomic Force Microscope Characterization of Cellulose Nanocrystal Transverse Properties Ryan Wagner, Arvind Raman and Robert Moon.......................................................................................................................39 Determination of Cellulose Nanocrystal Surface Sulfate Substitution Levels Jin Gu and Jeffrey M. Catchmark ............................................................................................................................................41 Crystallinity of Nanocellulose Materials by Near-IR FT-Raman Spectroscopy Umesh P. Agarwal, Richard S. Reiner and Sally A. Ralph .......................................................................................................43 iv Production and Applications of Cellulose Nanomaterials Solid-State Characteristics of Cellulose Nanocrystals Wadood Y. Hamad ....................................................................................................................................................................45 Surface Area and Porosity Characterization of Cellulose Nanocrystals from Hydrolysis by Different Acids Jing Guo and Jeffrey M. Catchmark ........................................................................................................................................49 Ring Opening Polymerization as a Tool for Tuning the Surface Topochemistry of Cellulose Nanocrystals Youssef Habibi and Philippe Dubois ........................................................................................................................................53 1.2 Health, Safety and Environment Health and Environmental Safety Aspects of CNF Jari Vartiainen and Minna Vikman ..........................................................................................................................................57 X-Ray Diffraction as a Measurement Tool for Biodegradability of Cellulose Nanocrystals Mohindar S. Seehra and Aleksandr B. Stefaniak .....................................................................................................................59 Occupational Exposure Characterization During the Manufacture of Cellulose Nanomaterials Kenneth F. Martinez, Adrienne Eastlake, Alan Rudie and Charles Geraci .............................................................................61 Incorporating Life-Cycle Thinking into Risk Assessment for Nanoscale Materials: Case Study of Nanocellulose Jo Anne Shatkin, Theodore Wegner and World Nieh................................................................................................................65 1.3 Coatings, Films, and Optical Properties Effect of Cellulose Nanocrystal Alignment on Thermo-Mechanical Response Jairo A. Diaz, Jeffrey P. Youngblood and Robert J. Moon .......................................................................................................69 Assembly of CNC in Coatings for Mechanical, Piezoelectric and Biosensing Applications Ingrid C. Hoeger, Levente Csoka and Orlando J. Rojas ..........................................................................................................71 Control of Cellulose Nanocrystal Film Iridescence Stephanie Beck, Greg Chauve, Jean Bouchard and Richard Berry .........................................................................................75 Chiral Nematic CNC Suspensions in Water Derek G. Gray ..........................................................................................................................................................................79 Chiral Nematic Films of CNC Derek G. Gray ..........................................................................................................................................................................81 Chiral Nematic Materials Derived From Cellulose Nanocrystals Michael Giese and Mark J. MacLachlan .................................................................................................................................83
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