Production And Applications Of Cellulose Nanomaterials

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ompiled and Edited by:Michael T. PostekRobert J. MoonAlan W. RudieandMichael A. BilodeauCellulose 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 andmany potential applications,” colorized by Michael Postek.Certain commercial equipment is identified in this report to adequately describe theexperimental procedure. Such identification does not imply recommendation or endorsement by the National Institute of Standards and Technology or the Forest ProductsLaboratory, nor does it imply that the equipment identified is necessarily the best available for the purpose.Credits for figures on the next page:Koga and Kitaoka: Crystalline Cellulose Nanofibrils Conjugated with Metal NanocatalystsKangas: Cellulose nanofibrils: A class of materials with unique properties and numerous potential applicationsPostek and Vladar: Dimensional Metrology and Imaging of Cellulose Nanocrystalsi

Copyright 2013 byTAPPI PRESS15 Technology Parkway SouthSuite 115Peachtree Corners, GA 30092 U.S.A.www.tappi.orgAll rights reservedThe Association assumes no liability or responsibility in connection with the use of this information ordata, including, but not limited to, any liability or responsibility under patent, copyright, or trade secretlaws. 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 anymeans – electronic, mechanical, photocopying, recording, or otherwise – without the written permissionof the copyright owner. Other portions of this book were written and/or prepared by U.S. Governmentemployees 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, orto 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 permissionrequest process, please contact CCC by phone at 1-978-750-8400.ISBN: 978-1-59510-224-9TAPPI PRESS Order Number: 0101R332Printed in the United States of AmericaiiProduction and Applications of Cellulose Nanomaterials

ichael T. PostekNational Institute of Standards and TechnologyRobert J. MoonUSDA Forest Service, Forest Products Laboratory,School of Materials Engineering, and theBirck Nanotechnology Center, Purdue UniversityAlan W. RudieUSDA Forest Service, Forest Products LaboratoryandMichael A. BilodeauUniversity of Maine, Process Development CenterJune 2013Production and Applications of Cellulose Nanomaterialsiii

Table of ContentsForewordMichael T. Postek, Robert J. Moon, Alan W. Rudie, Michael A. Bilodeau.1IntroductionCellulosic Nanomaterials: Sustainable Materials of Choice for the 21st CenturyTheodore H. Wegner, Sean Ireland and J. Philip E. Jones.3Chapter 1: Cellulose NanocrystalsCellulose Nanocrystals – A Material with Unique Properties and Many Potential ApplicationsRobert Moon, Stephanie Beck and Alan Rudie.91.1 Preparation and CharacterizationCellulose Nanocrystals: Extraction from Bio-residuesMartha Herrera, Aji Mathew and Kristiina Oksman.13Thermally Stable Cellulose Nanocrystals Isolated By Phosphoric Acid HydrolysisSandra Camarero Espinosa, Tobias Kuhnt, Christoph Weder and E. Johan Foster.17Process Scale-Up of Cellulose Nanocrystal Production to 25 kg per Batch at the Forest Products LaboratoryRichard S. Reiner and Alan W. Rudie.21Green Synthesis, Modification and Properties of Carboxylated Cellulose Nanocrystals using Ammonium PersulfateAlfred C.W. Leung, Edmond Lam and John H.T. Luong.25Production of Reference Materials for Cellulose Nanocrystals (CNC)Ralph E. Sturgeon and Patricia Grinberg.29Drying Cellulose Nanocrystal SuspensionsYucheng Peng, Douglas J. Gardner, Yousoo Han, Zhiyong Cai and Mandla A. Tshabalala.31.Dispersibility of Dried Cellulose Nanocrystals in WaterStephanie Beck, Jean Bouchard and Richard Berry.35Dimensional Metrology and Imaging of Cellulose NanocrystalsMichael T. Postek and András E. Vladár.37Atomic Force Microscope Characterization of Cellulose Nanocrystal Transverse PropertiesRyan Wagner, Arvind Raman and Robert Moon.39Determination of Cellulose Nanocrystal Surface Sulfate Substitution LevelsJin Gu and Jeffrey M. Catchmark.41Crystallinity of Nanocellulose Materials by Near-IR FT-Raman SpectroscopyUmesh P. Agarwal, Richard S. Reiner and Sally A. Ralph.43ivProduction and Applications of Cellulose Nanomaterials

Solid-State Characteristics of Cellulose NanocrystalsWadood Y. Hamad.45Surface Area and Porosity Characterization of Cellulose Nanocrystals from Hydrolysis by Different AcidsJing Guo and Jeffrey M. Catchmark.49Ring Opening Polymerization as a Tool for Tuning the Surface Topochemistry of Cellulose NanocrystalsYoussef Habibi and Philippe Dubois.531.2 Health, Safety and EnvironmentHealth and Environmental Safety Aspects of CNFJari Vartiainen and Minna Vikman.57X-Ray Diffraction as a Measurement Tool for Biodegradability of Cellulose NanocrystalsMohindar S. Seehra and Aleksandr B. Stefaniak.59Occupational Exposure Characterization During the Manufacture of Cellulose NanomaterialsKenneth F. Martinez, Adrienne Eastlake, Alan Rudie and Charles Geraci.61Incorporating Life-Cycle Thinking into Risk Assessment for Nanoscale Materials: Case Study of NanocelluloseJo Anne Shatkin, Theodore Wegner and World Nieh.651.3 Coatings, Films, and Optical PropertiesEffect of Cellulose Nanocrystal Alignment on Thermo-Mechanical ResponseJairo A. Diaz, Jeffrey P. Youngblood and Robert J. Moon.69Assembly of CNC in Coatings for Mechanical, Piezoelectric and Biosensing ApplicationsIngrid C. Hoeger, Levente Csoka and Orlando J. Rojas.71Control of Cellulose Nanocrystal Film IridescenceStephanie Beck, Greg Chauve, Jean Bouchard and Richard Berry.75Chiral Nematic CNC Suspensions in WaterDerek G. Gray.79Chiral Nematic Films of CNCDerek G. Gray.81Chiral Nematic Materials Derived From Cellulose NanocrystalsMichael Giese and Mark J. MacLachlan.83Novel Applications of Cellulose NanocrystalsYulin Deng and Arthur Ragauskas.87Polyelectrolyte Multilayer Films Containing Cellulose NanocrystalsEmily D. Cranston.89Biocomponent Ultrathin Films of Ordered Two-Dimensional Structures Based on Cell Wall PolymersLaura Taajamaa, Ingrid C. Hoeger, Eero Kontturi, Janne Laine and Orlando J. Rojas.93Production and Applications of Cellulose Nanomaterialsv

1.4 Cellulose Nanocrystals as a Reinforcing Phase in Composite StructuresMechanical and Thermal Property Enhancement in Cellulose Nanocrystal/Waterborne Epoxy CompositesShanhong, Xu, Natalie Girouard, Lionel Cross, Eric Mintz, Greg Schueneman, Meisha L. Shofner and Carson Meredith.97Cellulose Nanocomposites Processing using ExtrusionKristiina Oksman, Aji P. Mathew, Mehdi Jonoobi, Maiju Hietala and Natalia Herrera.99Melt Extrusion of CNC-based Polymer NanocompositesMariana Pereda, Nadia El Kissi and Alain Dufresne.103Ring Opening Polymerization Grafting of Polylactide from Cellulose NanocrystalsYoussef Habibi and Philippe Dubois.107Melt Processing of PVAc-Cellulose Nanocrystal NanocompositesJanak Sapkota, Matthew N. Roberts, Sandeep Kumar, Christoph Weder and E. Johan Foster.111Spatially Resolved Characterization of CNC-Polypropylene Composite by Confocal Raman MicroscopyUmesh Agarwal, Ronald Sabo, Richard Reiner, Craig Clemons and Alan Rudie.113Spinning of Continuous Biofibers Reinforced with Cellulose NanocrystalsNatalia Herrera-Vargas, Saleh Hooshmand, Aji P. Mathew and Kristiina Oksman.115Nanocomposite Electrospun Fibers with CNC ReinforcementMaria S. Peresin, Mariko Ago and Orlando J. Rojas.119In situ Conjunction of Cellulose Nanocrystals in Supramolecular Hydrogels by the Aid of Host-Guest Inclusion ComplexationNing Lin and Alain Dufresne.123Cellulose Nanocrystal-Reinforced Polymeric Bone ScaffoldsJung Ki Hong and Maren Roman.127Light-Responsive Cellulose-Based MaterialsMahesh V. Biyani, Mehdi Jorfi, Christoph Weder and E. Johan Foster.129Bio-Inspired Mechanically Adaptive Polymer Composites with Cellulose NanocrystalsStuart J. Rowan and Christoph Weder.131Performance-Enhanced Cementitious Materials by Cellulose Nanocrystal AdditionsYizheng Cao, W. Jason Weiss, Jeffrey Youngblood, Robert Moon and Pablo Zavattieri.1351.5 Modeling of Cellulose Nanocrystals and Composite ProductsModeling Mechanical Properties of Cellulose NanocrystalsMalin Bergenstråhle-Wohlert and Jakob Wohlert.137Multiscale Modeling of the Hierarchical Structure of Cellulose NanocrystalsFernando L. Dri, Robert J. Moon and Pablo Zavattieri.139Atomistic Simulation of Nanoscale Indentation on Cellulose NanocrystalsXiawa Wu, Robert J. Moon and Ashlie Martini.143viProduction and Applications of Cellulose Nanomaterials

CN-Composite Micromechanics Model with Interfaces and Short FibersJohn A. Nairn.145Multiscale Modeling of Solvation and Effective Interactions of Functionalized Cellulose NanocrystalsStanislav R. Stoyanov, Sergey Gusarov and Andriy Kovalenko.147Soft Matters with Cellulose Nanocrystals (CNC)Yaman Boluk and Usha Hemraz.1511.6 Self-Assembly and Miscellaneous ApplicationsCellulose Nanomaterials for Water Purification MembranesAji P. Mathew, Zoheb Karim, Liu Peng and Kristiina Oksman.155Cellulose Nanocrystal-Based Drug Delivery SystemsMaren Roman, Hezhong Wang and Shuping Dong.157Cellulose Nanocrystals: Novel Templates for Synthesis of NanostructuresSonal Padalkar, Robert Moon and Lia Stanciu.159Nanofibrillar Carbon from Chitin NanofibersMasaya Nogi.161Cellulose Nanocrystals as Templates for Durable Supercapacitor ElectrodesDarren A. Walsh and Wim Thielemans.163Cellulose Nanocrystal Substrates for Recyclable Printed ElectronicsYinhua Zhou, Canek Fuentes-Hernandez, Talha M. Khan, Jen-Chieh Liu, James Hsu,Jae Won Shim, Amir Dindar, Jeffrey P. Youngblood, Robert J. Moon and Bernard Kippelen.167Chapter 2: Cellulose NanofibrilsCellulose Nanofibrils – A Class of Materials with Unique Properties and Many Potential ApplicationsHeli Kangas.1692.1 Preparation and CharacterizationPreparation and Characterization of Cellulose Nanofibers from Various Plant SourcesKentaro Abe and Hiroyuki Yano.175Pilot Plant Scale-up of TEMPO-Pretreated Cellulose NanofibrilsRichard S. Reiner and Alan W. Rudie.177Microbial Cellulose Nanofibers: Producing CNFs and Controlling Their OrientationTetsuo Kondo.179Aqueous Counter-Collision for Preparation of Bio-NanofibersTetsuo Kondo.181Nanofibrillation of Cellulose Pulp using Regioselective Periodate Pre-TreatmentsHenrikki Liimatainen, Juho Sirviö, Miikka Visanko, Terhi Suopajärvi, Ngesa Ezekiel, Osmo Hormi, and Jouko Niinimäki.183Production and Applications of Cellulose Nanomaterialsvii

Low-Cost Extraction of Cellulose Nanofibers from Grass by a Household BlenderAntonio Norio Nakagaito, and Hitoshi Takagi.185Cellulose Nanofiber Isolated from Industrial Side StreamsKristiina Oksman, Aji P Mathew, Mehdi Jonoobi, Gilberto Siqueira, Maiju Hietala, and Yvonne Aitomäki.187Integrated Production of Cellulose Nanofibrils and Cellulosic Biofuel by Enzymatic Hydrolysis of Wood FibersRonald Sabo and Junyong Zhu.191Preparation of Chitin Nanofibers from the Exoskeletons of Crabs and PrawnsShinsuke Ifuku.195Enzymatic Deconstruction of the Cell Wall for Energy Efficient Production of Cellulose Nanofibrils (CNF)Junyong Zhu and Q.Q. Wang.197High Yield and Zero Cellulose Loss in Cellulose Nanocrystal (CNC) Production:Cellulose Nanofibrils (CNF) from a CNC Production Waste StreamJ.Y. Zhu, Q.Q. Wang, R.S. Reiner, and S.P. Verrill, J.M. Considine, U. Baxa and S.E. McNeil.201Bending Test for Single Cellulose Microfibrils using Atomic Force MicroscopyShinichiro Iwamoto.205Cellulose Nanomaterials: Nanocomposite Imaging using FRETMauro Zammarano, Li-Piin Sung, Douglas M. Fox, Iulia Sacui,Jeremiah Woodcock, Paul H. Maupin and Jeffrey W. Gilman.209Rheological Methods to Characterize Cellulose Nanofibrils at Moderate SolidsBehzad Nazari, Juha Salmela, Ari Jäsberg, Veli-Matti Luukkainen, Janne Poranen,Finley Richmond, Albert Co,and Doug Bousfield.211Current International Standards Development Activities for Cellulose NanomaterialWorld L-S Nieh.213Drying Cellulose Nanofibril SuspensionsYucheng Peng, Douglas J. Gardner, Yousoo Han, Zhiyong Cai, and Mandla A. Tshabalala.2152.2 Health, Safety and Medical Applications of Cellulose NanofibrilsCellulose Nanocomposites for Ligament ReplacementAji P. Mathew and Kristiina Oksman.219CNF as a Support of Bioactive Molecules for Molecule Detection and RemovalYanxia Zhang, Hannes Orelma, Ilari Filpponen, Janne Laine and Orlando Rojas.2232.3 Coatings, Films and Optical UsesAcetylation of Bacterial Cellulose Nanofibers for Property Enhancement of Optically Transparent CompositesShinsuke Ifuku and Masaya Nogi.227Cellulose Nanofibril Films and Coatings for Packaging ApplicationsChristian Aulin and Tom Lindström.229viiiProduction and Applications of Cellulose Nanomaterials

High Optical Transparency of Nanofiber Composites Against a Wide Refractive Index Range of Polymer MatrixMasaya Nogi.233Optically Transparent NanopaperMasaya Nogi.237Large-Scale Production of CNF FilmsJari Vartiainen, Timo Kaljunen, Vesa Kunnari, Panu Lahtinen, and Tekla Tammelin.239Optically Transparent Cellulose Nanocomposites: From Nanofibers to Nanostructured FibersHiroyuki Yano.241Cellulose Nanofibril/Layered Silicates Composite Films for Barrier ApplicationsTanja Zimmermann, T.T.T. Ho, P. Tingaut, and W Caseri.245Use of Cellulose Nanofibrils in Paper CoatingsFinley Richmond, Michael Bilodeau and Douglas W. Bousfield.247Nanopaper from Lignin-Containing CNFElisabet Quintana, Ana Ferrer, Ilari Filponnen, Ingrid Hoeger, J. Y. Zhu, Janne Laine and Orlando J. Rojas.249Carbon Nanotube/Nanocellulose Composite for Printed and Flexible ElectronicsHirotaka Koga.253Bendable Transparent Nanofiber Composites with an Ultra-Low Coefficient of Thermal ExpansionMasaya Nogi.255Printed Antennas and Solar Cells on NanopaperMasaya Nogi.259Cellulose Nanofibril Composite Substrates for Flexible ElectronicsRonald Sabo, Jung-Hun Seo and Zhenqiang Ma.263Surface Functionalization of TiO2-CNF Films with Au and Ag Nanoclusters for Visible Light PhotocatalysisAlexandra Snyder, Zhenyu Bo, Robert J. Moon and Lia Stanciu.265CNF for Innovative Aerogels and ElectronicsYulin Deng and Arthur Ragauskas.2672.4 Composites, Liquid Gels and AerogelsHigh-Strength Nanocomposite Based on Fibrillated Chemi-Thermomechanical PulpKentaro Abe, Fumiaki Nakatsubo and Hiroyuki Yano.269Cellulose Nanofibril Nanocomposite ProcessingYvonne Aitomäki and Kristiina Oksman.271High-Performance Transparent Composites Using NanocelluloseJames F. Snyder, Hong Dong, Joshua Steele and Joshua A. Orlicki.275Role of Cellulose Nanofibers in Processing and Toughening of PLA Microcellular NanocompositeJana Dlouhä and Hiroyuki Yano.279Production and Applications of Cellulose Nanomaterialsix

Cellulose Nanofibril-Modified Thermoset AdhesivesWolfgang Gindl-Altmutter, Stefan Veigel and Gregor Tschurtschenthaler.283Multifunctional Bacterial Cellulose NanocompositesEsra E. Kiziltas, Alper Kiziltas and Douglas J. Gardner.285Mechanical Properties of Cellulose Nanofibril-Wood Flake LaminateJen-Chieh Liu, Robert J. Moon and Jeff P. Youngblood.287High-Strength Cellulose Nanofiber-Based Composites for Semi-Structural ApplicationsAntonio Norio Nakagaito.289Nanostructured Composites from Wood Cellulose NanofibrilsHoussine Sehaqui.291Acceleration of the Molding Cycle of Semi-Crystalline Polylactic Acid by Cellulose Nanofiber ReinforcementLisman Suryanegara, Hiroaki Okumura, Antonio Norio Nakagaito and Hiroyuki Yano.295Novel Process for the Nanofibrillation of Pulp and its Melt Compounding with PolypropyleneKatsuhito Suzuki and Hiroyuki Yano.297Understanding Interfaces in Cellulose Nanofiber All-Cellulose Nanocomposites using Raman SpectroscopyStephen Eichhorn.301Processing of CNF-Reinforced Hydrophobic Nanocomposites using Functionalized Carrier SystemsAlper Kiziltas, Yousoo Han, Douglas J. Gardner, David Neivandt and Todd S. Rushing.303Mechanical Properties of Latex Films that Contain Cellulose NanofibrilsRikard Rigdal and Douglas W. Bousfield.307Formation and Characterization of Cellulose Nanofiber-Based HydrogelsKentaro Abe and Hiroyuki Yano.309Hydrogelation of Cellulose Nanofibrils Modulated by Metal CationsHong Dong and James F. Snyder.311Crystalline Cellulose Nanofibrils Conjugated with Metal NanocatalystsHirotaka Koga and Takuya Kitaoka.313Cellulose Nanofibril (CNF) Insulating FoamsNadir Yildirim, Stephen M. Shaler, Douglas J. Gardner, Douglas W. Bousfield and Robert Rice.317Author Index.321xProduction and Applications of Cellulose Nanomaterials

Foreword“Production and Applications of Cellulosic Nanomaterials” was intended to help organizeand highlight the wide range of research being conducted worldwide on the science and technologyof cellulose nanomaterials. The format of this book consists of short research summaries, targetedfor a level where they can be understood by non-specialists in the resear

Production and Applications of Cellulose Nanomaterials iii 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 Bir

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