Carbon Composites: Composites with Carbon Fibers, Nanofibers, and Nanotubes [2 ed.] 0128044594, 9780128044599

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Carbon Composites Composites with Carbon Fibers, Nanofibers, and Nanotubes Second Edition Deborah D.L. Chung University at Buffalo The State University of New York Buffalo, NY, United States

AMSTERDAM • BOSTON • HEIDELBERG • LONDON • NEW YORK • OXFORD PARIS • SAN DIEGO • SAN FRANCISCO • SINGAPORE • SYDNEY • TOKYO

Butterworth-Heinemann is an imprint of Elsevier

Butterworth-Heinemann is an imprint of Elsevier The Boulevard, Langford Lane, Kidlington, Oxford OX5 1GB, United Kingdom 50 Hampshire Street, 5th Floor, Cambridge, MA 02139, United States Copyright © 2017 Deborah D.L. Chung. Published by Elsevier Inc. All rights reserved. No part of this publication may be reproduced or transmitted in any form or by any means, electronic or mechanical, including photocopying, recording, or any information storage and retrieval system, without permission in writing from the publisher. Details on how to seek permission, further information about the Publisher’s permissions policies and our arrangements with organizations such as the Copyright Clearance Center and the Copyright Licensing Agency, can be found at our website: www.elsevier.com/permissions. This book and the individual contributions contained in it are protected under copyright by the Publisher (other than as may be noted herein). Notices Knowledge and best practice in this field are constantly changing. As new research and experience broaden our understanding, changes in research methods, professional practices, or medical treatment may become necessary. Practitioners and researchers must always rely on their own experience and knowledge in evaluating and using any information, methods, compounds, or experiments described herein. In using such information or methods they should be mindful of their own safety and the safety of others, including parties for whom they have a professional responsibility. To the fullest extent of the law, neither the Publisher nor the authors, contributors, or editors, assume any liability for any injury and/or damage to persons or property as a matter of products liability, negligence or otherwise, or from any use or operation of any methods, products, instructions, or ideas contained in the material herein. Library of Congress Cataloging-in-Publication Data A catalog record for this book is available from the Library of Congress British Library Cataloguing-in-Publication Data A catalogue record for this book is available from the British Library ISBN: 978-0-12-804459-9 For information on all Butterworth-Heinemann publications visit our website at https://www.elsevier.com/

Publisher: Matthew Deans Acquisition Editor: David Jackson Editorial Project Manager: Edward Payne Production Project Manager: Julie-Ann Stansfield Designer: Mark Rogers Typeset by Thomson Digital

In celebration of the 100th birthday of my late father

Mr. Leslie Wah-Leung Chung

(1917–2009)

President, Hong Kong Chinese Civil Servants’ Association Head, Department of Commerce and Management Studies, Hong Kong Technical College (currently Hong Kong Polytechnic University) Founding Principal, St. Mark’s School, Hong Kong British Hong Kong World War II veteran (wounded in action) Choir Director, The Church of Christ in China Mongkok Church, Hong Kong

Preface This is the second edition of the book “Carbon Fiber Composites” (Butterworth-Heinemann, 1994) by the same author. Due to the explosive growth of research on carbon nanotubes and nanofibers over the last two decades, the second edition is broader in scope than the first edition. Thus, the second edition is titled “Carbon Composites: Composites with Carbon Fibers, Nanofibers, and Nanotubes.” Furthermore, the fields of cement-matrix composites, carbon-matrix composites and ceramic-matrix composites with carbon fibers have made dramatic advances since 1994. In addition, since the first edition, applications other than structural ones have grown greatly and multifunctional structural materials have become a scientifically rich and technologically significant field. The relatively new applications of composite materials pertain to electrical, dielectric, electrochemical, electromechanical, and electromagnetic behavior, in addition to energy generation and energy storage. All these advances make the preparation of the Second Edition a daunting but necessary task. This book provides an up-to-date coverage of carbon fiber, carbon nanofiber, and carbon nanotube composites with polymers, cements, carbons, ceramics, and metals as matrices in relation to the processing, structure, mechanical properties, thermal properties, functional properties, and applications, with almost 2000 references cited. The overlap between the two editions is very small. Essentially the whole book has been rewritten in preparing the second edition. This book addresses in Chapters 1 and 2 carbon fibers, carbon nanofibers, and carbon nanotube, and their various configurations of assembly, in addition to their applications. Then Chapters 3–5 address polymer-matrix composites, with Chapter 3 focusing on the processing and structure, Chapter 4 focusing on the mechanical and thermal behavior, and Chapter 5 focusing on the functional behavior, which includes the electrical conductivity, lightning protection ability, electromagnetic behavior, dielectric properties, electromechanical behavior, thermal conductivity, and thermoelectric behavior. The fact that three chapters are devoted to polymer-matrix composites reflects the dominance of this field in research and applications. Chapters 6–9 address cement-matrix composites, carbon-matrix composites, ceramic-matrix composites, and metal-matrix composites, respectively. For each type of matrix, the processing, structure, and properties are systematically presented. This book assumes only introductory undergraduate materials science knowledge from the readers. Thus, concepts on the associated science and applications are introduced and the structures of materials and molecules are described. The advances of the field, particularly in relation to carbon-matrix and ceramic-matrix composites, have involved the use of molecules. In recognition of the fact that the readers may not be chemists, the structures of molecules are given. Also in recognition of the fact that the readers may not have much background on the functional behavior of materials, this book provides the associated basic concepts. Electrochemical applications (e.g., batteries, fuel cells, and supercapacitors) have grown greatly since the first edition, so they are covered along with the associated basic concepts. This book is suitable as a textbook for senior undergraduate students and graduate students in materials science/engineering, chemical engineering, mechanical engineering, aerospace engineering, civil engineering, chemistry, and physics. This book distinguishes itself from other

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books on composite materials in its emphasis on materials science and engineering rather than mechanics. Books on composite materials tend to emphasize mechanics, because of the focus on the mechanical properties, with little attention on the functional properties. Furthermore, books on composite materials tend to emphasize established materials rather than emerging materials. In addition, they tend to emphasize polymer-matrix composites, with little coverage of composite with other matrices. By covering composites with a broad range of matrices, this book provides the scientific common thread for these materials. Through the detailed discussion of the relationships among the processing, structure and properties, this book provides the principles for the development and design of composite materials, which are dominant among materials that are being developed or that have been recently developed. This book is suitable as a reference book for researchers, engineers, scientists, technicians, and technology business managers. The up-to-date references, the coverage of both established and emerging materials, the specific examples of materials processing and design, the broad coverage of materials, and the holistic view of processing, structure, properties, and applications, all make this book a particularly useful reference book. In addition, the topics are differentiated and organized in each chapter so as to facilitate information look-up. The writing of this book was facilitated by the large amount of composite materials research that has occurred in Composite Materials Research Laboratory, University at Buffalo, The State University of New York. I particularly thank my Ph.D. graduate students (about 40) who have conducted research with me over the last few decades. Most importantly, I thank my Ph.D. thesis advisor, Professor M.S. Dresselhaus of the Massachusetts Institute of Technology, for introducing me to the field of carbon.

Deborah D.L. Chung Buffalo, NY June 29, 2016

1 Carbon Fibers, Nanofibers, and Nanotubes 1.1  Introduction to Carbon Science 1.1.1 Graphite Graphite is the thermodynamically stable form of carbon at ordinary temperatures and pressures. It exhibits a layered crystal structure with an AB stacking sequence of the layers (Fig. 1.1A–C). This crystal structure is based on the hexagonal lattice with four atoms associated with each lattice point. The density of graphite is 2.26 g/cm3. Carbon fibers also consist of carbon layers, but they typically do not exhibit the AB stacking sequence due to the loss of registry between adjacent layers. Furthermore, the layers in a carbon fiber are typically limited in size and parallelism. As a result, the carbon layers in a carbon fiber typically do not form a periodic structure, so that the carbon in a carbon fiber is typically amorphous and this form of carbon is known as turbostratic carbon (Fig. 1D) rather than graphite. The amorphous state is also known as the noncrystalline state or the glassy state. As a result, the carbon layers in a carbon fiber are typically not as well packed as those in graphite. Thus, the density of carbon fibers is less than that of graphite, typically ranging from 1.75 to 1.85 g/cm3. In general, the structure of carbon fibers can be crystalline, amorphous, or partly crystalline, though they are typically completely amorphous. ­Furthermore, there can be various degrees of order (or various degrees of disorder) for the amorphous form. Nevertheless, all carbon fibers belong to the graphite family (Chung, 2002a). This means that the crystalline part (if any) of a carbon fiber has the graphite structure (Fig. 1.1A–C), whereas the amorphous part of a carbon fiber has a disordered structure that relates to the graphite structure (Fig. 1.1D). The amorphous form has a structure that is still layered; both there is no long-range order. The distance between the carbon layers (known as the interplanar spacing or d002) is higher for carbon fibers than graphite. As shown in Fig. 1.1A, the interplanar spacing is 3.35 Å for graphite. Moreover, the carbon layers in the amorphous form can be not exactly parallel to one another, and can be crooked (not flat). In addition, the size of the layers in the plane of the layers is limited and the number of layers in a stack is also limited. The greater is the degree of order, (1) the greater are the size, degree of flatness, and degree of parallelism of the layers, (2) the greater is the number of layers in a stack, and (3) the smaller is the interplanar spacing. The graphite structure consists of sp2-hybridized carbon atoms arranged two-­ dimensionally in a honeycomb structure in the x–y plane. Carbon atoms within a layer are bonded by (1) covalent bonds provided by the overlap of the sp2-hybridized orbitals, and Carbon Composites. http://dx.doi.org/10.1016/B978-0-12-804459-9.00001-4 Copyright © 2017 Deborah D.L. Chung. Published by Elsevier Inc. All rights reserved.

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FIGURE 1.1  The structure of materials in the graphite family. (A) The three-dimensional crystal structure of graphite, showing two adjacent carbon layers. (B) The edge view of the three-dimensional crystal structure of graphite, showing three carbon layers in the AB stacking sequence. (C) The two-dimensional structure of two adjacent carbon layers in graphite that is superimposed to show their registry relative to one another. (D) Turbostratic carbon, with the dimension of the layers in the plane of the layers known as La and the c-axis stack height of the layers known as Lc. Part B, https://commons.wikimedia.org/wiki/File:Graphite-layers-side-3D-balls.png, public domain; part C, https:// commons.wikimedia.org/wiki/File:Graphite-layers-top-3D-balls.png, public domain; part D, http://thehealthscience.com/ thsattachs/939954/Turbostratic%20amorphous%20structure.gif, public domain.

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  3

(2) metallic bonding provided by the delocalization of the pz orbitals, i.e., the π-electrons. This delocalization makes graphite a good electrical conductor and a good thermal conductor in the x–y plane. The bonding between the layers is van der Waals bonding, so the carbon layers can easily slide with respect to one another; graphite is an electrical insulator and a thermal insulator perpendicular to the layers. Due to the difference between the inplane and out-of-plane bonding, graphite has a high modulus of elasticity parallel to the plane and a low modulus perpendicular to the plane. Thus, graphite is highly anisotropic. Furthermore, due to the easy sliding of the layers relative to one another, graphite is a good solid lubricant. Due to the easy sliding and the black color, graphite is used for pencils. The adjacent carbon layers in graphite (ideal crystalline graphite) are registered with respect to one another, as shown in Fig. 1.1C. In other words, the positions of the layers relative to one another are not random. The registration is such that half of the atoms of a layer (shown by solid circles in Fig. 1.1A) are directly above and below atoms of an adjacent layer, whereas the remaining half of the atoms of the layer (shown by open circles in Fig. 1.1A) have no neighboring atom directly above or below them. This stacking is known as AB (i.e., in the order ABABAB…), where A and B indicate two adjacent layers. The hexagonal close-packed (HCP) structure is a crystal structure that is common among metals, such as titanium. This structure also has the AB stacking sequence, but the atom arrangement within each layer differs between the graphite structure and the HCP structure, and the geometry associated with the registration between the A and B layers also differs between the two structures. Graphitization refers to the process of converting amorphous carbon to crystalline carbon by heating. It is a crystallization process and is spontaneous because the crystalline state has a lower energy than the amorphous state. The degree of graphitization (G, also known as the graphitization rate) refers to the degree of crystallinity and is obtained using the equation:

o o G = (d002 − d002 )/(d002 − 3.354 Å)

(1.1)

o where d002 is the interplanar spacing for the case of no graphitization (i.e., G = 0), d002 is the value for the particular carbon under consideration, and 3.354 Å is the d002 of ideal graphite. The temperature required for graphitization is high, ranging from 2000 to 3000°C. Due to the tendency of carbon to be oxidized in the presence of heat and oxygen, graphitization must be conducted in an inert atmosphere, such as argon gas. Nitrogen gas is not suitable, because of the tendency for carbon to react with nitrogen to form cyanide, which is poisonous. The higher is the heat-treatment temperature used in the fiber fabrication, the higher is the degree of crystallinity (i.e., the fraction of the carbon fiber that is crystalline), the ­higher is the degree of order in the amorphous state, and the higher is the density. The effect of heating on the degree of crystallinity is because the crystalline state is the thermodynamically stable state (i.e., the lowest energy state, or, more exactly, the lowest free energy state)

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FIGURE 1.2  Calculated phase diagram of carbon, showing the equilibrium phases for various combinations of pressure (vertical axis) and temperature (horizontal axis). https://commons.wikimedia.org/wiki/File:Carbon_basic_phase_ diagram.png, public domain.

whereas the amorphous state is only metastable (not thermodynamically state). The effect of heating on the degree of order in the amorphous state is because the energy is lower for a higher degree of order. Upon heating to a sufficiently high temperature, thermal energy is available to cause the carbon atoms to move in the solid state (without melting) and the atoms would move automatically so that the degree of crystallinity and/or the degree of order increases. A main shortcoming of carbon is its tendency to be oxidized when it is heated in the presence of oxygen. The oxidation reaction results in the formation of gases, such as carbon dioxide formed through the following reaction. C + O 2 → CO 2

As a consequence, the carbon experiences mass loss (i.e., volume loss). Due to the lower energy state for the crystalline state than the amorphous state, the crystalline state is superior in the oxidation resistance. The higher is the degree of order, the better is the oxidation resistance. As shown in the calculated phase diagram in Fig. 1.2, graphite is the thermodynamically stable form of carbon at ordinary temperatures and pressures. The application of a high pressure can convert graphite to diamond. At ordinary temperatures and pressures, diamond is not thermodynamically stable and tends to change to graphite. However, the rate of this change is very low, unless the diamond is heated. The melting of graphite occurs at extremely high temperatures, so liquid carbon is rarely studied and is not addressed in this book. For a carbon composite, the oxidation resistance depends on the carbon content, specimen size, and temperature (Hou and Chou, 2010).

1.1.2  The Allotropes of Carbon Graphite, diamond, and fullerene are the three allotropes (polymorphs or crystalline forms) of solid carbon (Astefanei et al., 2015; Gogotsi, 2015; Mojica et al., 2013). Diamond

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  5

FIGURE 1.3  The structure of a fullerene (C60) molecule. http://www.plexoft.com/SBF/images/wustlmirror/bballt.gif, public domain.

is the hardest known mineral, due to its three-dimensional (3D) covalent network. The fullerene (C60) is a molecule with 60 carbon atoms and no other atom, such that the atoms are covalently bonded together, make hexagons and pentagons, with the pentagons being necessary to form a closed structure (Fig. 1.3A). Without the pentagons, the structure would be planar.

1.1.3  Energy Band Structure Graphene, which consists of a single layer of the 3D graphite [Fig. 1.1A], can be considered a part of the graphite family, though it can also be considered as the fourth allotrope of carbon. In spite of this original definition of graphene, current use of the term has been broadened to mean graphite with 10 or less layers in the stack. As a result, the term “few-layer graphene” is often used. This broadened definition of graphene is partly due to the difficulty of making single-layer graphene by the disintegration of the layers of graphite. Graphene is most attractive for its electronic properties that stem from the fact that its conduction and valence energy bands in reciprocal space meet at a point, which is known as the Dirac point. This band structure makes graphene a semiconductor with a zero energy bandgap. By applying a voltage, graphene can be rendered an electron conductor (n-type) or a hole conductor (p-type), such that the effective mass of the carriers is essentially zero. Hence, graphene exhibits exceptionally high charge carrier mobility. It is an excellent electrical conductor, transporting electrons tens of times faster than silicon. By limiting the size of one of the two dimensions of graphene, a graphene nanoribbon (GNR) is obtained. Depending on the in-plane orientation and width of the nanoribbon, the electronic properties differ, with properties ranging from metallic to semiconducting behavior (Pefkianakis et al., 2015). In contrast to graphene, ideal graphite is a semimetal, which is a material having a very small overlap between the bottom of the conduction band and the top of the valence

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FIGURE 1.4  The energy and momentum of the electrons and holes in ideal graphite. (A) One-dimensional energy bands of graphite. The valence band (hatched region) and conduction bands (dotted region) have an overlap of 0.03 eV. The Fermi energy (EF) lies within the band overlap region, resulting in pockets of holes and electrons. The overlap of the valence and conduction bands is characteristic of a semimetal. (B) Three-dimensional energy bands of graphite, showing schematically the wave vector (ξ, σ) dependence of the energy (E) of the graphite π-bands. The dashed line represents the Fermi level (EF) for pure graphite. (a) Energy vs. dimensionless wave vector σ in the plane ξ = 0 about the K point. (b) Energy vs. dimensionless wave vector ξ along the edges HKH and H’K’H’. (c) Energy vs. σ in the plane ξ = 1/2 about the H point. (C) The conventional Brillouin zone of graphite. The electron and hole Fermi surfaces are located in the vicinity of the edges HKH and H’K’H’ (Chung, 2002a).

band. In case of graphite, the overlap amounts to 0.03 eV [Fig. 1.4A]. There is no energy bandgap, so the material is not a semiconductor. The energy bands of ideal graphite can be illustrated in one dimension as shown in Fig. 1.4A. In three dimensions, the energy bands are shown in Fig. 1.4B. Along the HKH and H’K’H’ axes, the four π-bands are labeled E1, E2, and E3, where the E3 band is doubly degenerate along the zone edges. The E1 band is empty. The E2 band is nearly full and defines the minority hole pocket near the zone corner. The E3 band is partly occupied and defines

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  7

the majority electron and hole carrier pockets. The wave vector coordinates shown are ξ and σ, where ξ is the dimensionless wave vector along the c-axis and the other coordinate σ is the dimensionless wave vector in the basal plane. The conventional Brillouin zone of graphite is shown in Fig. 1.4C. The electron and hole Fermi surfaces are located in the ­vicinity of the edges HKH and H’K’H’. Carbon fibers are in the graphite family (as opposed to the diamond family), but they deviate from ideal graphite. Therefore, carbon fibers have energy band structures that deviate from those in Fig. 1.4. For example, some carbon fibers are p-type (with more holes than electrons) (Wen and Chung, 2004).

1.1.4  Intercalation of Graphite Graphite can be doped with a reactant known as intercalate. This process, known as intercalation, results in a graphite intercalation compound that has the intercalate (typically as a single atomic or molecular layer) between the graphite atomic layers. The number of carbon layers between adjacent intercalate layers is known as the stage. The higher is the stage number, the lower is the intercalate concentration. Within an intercalate layer, there can be two-dimensional (2D) ordering of the intercalate (Ghosh and Chung, 1983). The 3D structure of the stage-1 graphite–potassium intercalation compound C8K is illustrated in Fig. 1.5. Due to the charge transfer between the graphite and the intercalate, the intercalation compound can become an electron metal (the case of graphite intercalated with potassium) or a hole metal (the case of graphite intercalated with bromine) (Dresselhaus and Dresselhaus, 2002; Guerard and Fuzellier, 1991). Graphite–bromine lamellar compounds exist in at least four stages (stages 2–5), as illustrated in Fig. 1.6 (Chung, 2002a). As a consequence of the change from a semimetal to a metal, the electrical conductivity is increased by orders of magnitude.

FIGURE 1.5  The structure of stage-1 graphite–potassium intercalation compound C8K. (A) Side view, (B) top view. Part A, https://upload.wikimedia.org/wikipedia/commons/a/ae/Potassium-graphite-xtal-3D-SF-A.png, public domain; part B, https://upload.wikimedia.org/wikipedia/commons/5/55/Potassium-graphite-xtal-3D-SF-B.png, public domain.

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FIGURE 1.6  Interlayer ordering in graphite–bromine intercalation (lamellar) compounds of stages 2–5. The dashed lines indicate bromine intercalate layers; the solid lines indicate carbon layers. (A) 2nd stage structure of C16Br2 (6.25 mol.% Br2). (B) 3rd stage structure of C24Br2 (4.17 mol.% Br2). (C) Forth stage structure of C32Br2 (3.13 mol.% Br2). (D) 5th stage structure of C40Br2 (2.50 mol.% Br2) (Chung, 2002a).

FIGURE 1.7  The structure of a graphite intercalation compound according to Daumas and Herold (1969). The solid lines indicate the carbon layers. The dashed lines indicate the intercalate layers. The carbon layers are bent at certain locations, thus resulting in intercalate islands between the bend locations. The intercalation compound illustrated here has stage-2, but the concept applies to any stage (Chen and Chung, 2013a).

The intercalate is typically present in the form of islands, in accordance with the ­ aumas–Herold model (Daumas and Herold, 1969), in which the graphite layers bend, D thereby resulting in domains, each of which is an intercalate island (Fig. 1.7). This ­model has been confirmed by electron microscopy (Heerschap et al., 1964; Heerschap and Delavignette, 1967). It means that, for stages greater than 1, the intercalate layer does not necessarily extend all the way from one end of the graphite crystal to the other.

1.1.5  Exfoliation of Graphite During the heating of intercalated graphite, each intercalate island expands tremendously along the c-axis of the graphite. The larger are the intercalate islands, the greater is the degree of expansion (Anderson and Chung, 1984a). The expansion can be up to a few hundred times (Anderson and Chung, 1983; Chung, 1987; Herold et al., 1994). The driving force of the expansion is the vaporization or decomposition of the intercalate upon heating. The expansion phenomenon is known as exfoliated. The resulting material is known as exfoliated graphite (EG), which has a cellular structure (Fig. 1.8), which reflects

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  9

FIGURE 1.8  Scanning electron microscope (SEM) image of a part of a piece of exfoliated graphite. The piece is obtained by the exfoliation of a single graphite flake that has been intercalated with sulfuric acid. (A) Low-magnification view. (B) High-magnification view (Lin and Chung, 2009).

the ­intercalate island structure. Each piece of EG derived from a graphite flake looks like a worm [Fig. 1.8A], so it is known as a worm. Upon extensive mechanical agitation (such as sonication), a worm disintegrates into platelets, thus losing the cellular structure of the worm. These platelets (Fig. 1.9) are more than 10 carbon layers thick, so they are known as graphite nanoplatelets (GNP) rather than graphene. The GNP is useful as a filler in composite materials for providing electrical/­ thermal conductivity (Chung, 2016). In order for the large expansion to be able to occur during exfoliation, the graphite layers that make up the wall of an intercalate island must be able to stretch greatly (Fig. 1.10). The stretching of the wall enables an intercalate island to expand like a balloon. The force during exfoliation irreversibly loosens the bond between the carbon layers, so that the ease of sliding between the layers is irreversibly increased. As a consequence of

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FIGURE 1.9  SEM image of graphite nanoplatelets (Lin and Chung, 2009).

FIGURE 1.10  The structure of a cell wall, with each line representing a carbon layer (rather than a cell wall). In the case of exfoliated graphite made from sulfuric acid-intercalated graphite flakes, the cell wall typically consists of about 60 carbon layers. The substantial sliding between adjacent carbon layers necessitates that each carbon layer in the wall of a given cell wall does not extend from one end of the cell wall to the other; as illustrated, the carbon layers in a cell wall are not continuous (Chen and Chung, 2013a).

the enhanced ease of sliding and the large area of the interface between the carbon layers in a cell wall (Fig. 1.10), EG exhibits strong viscous behavior under dynamic strain (Chen and Chung, 2013a; Chung, 2014) and elastomeric behavior under static strain (Chen and Chung, 2015). The viscous behavior and elastomeric behavior are valuable for vibration damping and vibration isolation respectively. In addition, the elastomeric character is valuable for applications related to gasketing and sealing. The elastomeric character of EG is shown by instrumented indentation (nanoindentation), which shows that the reversible shear strain of the cell wall is as high as 39 (not 39%) (Chen and Chung, 2015). The extensive strain is enabled by the sliding of the graphite layers. The viscous behavior of EG stems primarily from the mechanical energy loss during the sliding of the cell walls relative to one another at locations where adjacent cell walls merge to form each cell extremity (Xiao and Chung, 2016). The contribution of sliding between graphite layers within a cell wall (Fig. 1.10) is relatively small. The greater is the solid content, the smaller is the displacement, the higher is the friction force, the less is the energy loss, and the lower is the degree of viscous character. This interface-derived viscous mechanism is in contrast to the well-known bulk viscous deformation mechanism that rubber exhibits.

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  11

Even though the amplitude of the sliding is small under dynamic loading, the sliding is easy and the back-and-forth sliding during vibration provides a significant degree of ­viscous behavior. The degree of viscous character is described by the loss tangent (i.e., tan δ, where δ is the phase lag between the stress wave and the strain wave during dynamic loading), which is equal to the ratio of the loss modulus (the viscous modulus) to the storage modulus (the elastic modulus). The viscous behavior of EG is associated with the loss tangent as high as 35 under dynamic flexure and as high as 25 under dynamic compression (Chen and Chung, 2013a). Both values of 35 and 25 are obtained by dividing the measured values by the solid volume fraction in the EG so as to reflect the behavior of the solid part of the porous material. These values are unprecedentedly high values among solid materials. The values decrease with increasing degree of compaction of the EG (i.e., with increasing solid content in the compact), due to the associated decreasing ease of sliding between the layers as the compact becomes more tightly packed. This means that an adequate degree of looseness of the binding between the layers is required for the viscous behavior to be substantial. In contrast to EG, the loss tangent is only 0.7 for rubber under dynamic flexure (Fu and Chung, 2001). “Flexible graphite” is EG that has been severely compacted uniaxially in the absence of a binder to form a flexible sheet (Chung, 2000a, 2002a, 2004a; Luo and Chung, 2001a) (Fig. 1.11). The sheet formation is enabled by the mechanical interlocking of the EG. This material is resilient in the direction perpendicular to the plane of the sheet (Chen and Chung, 2013a), due to the preferred orientation of the graphite layers in the plane of the sheet (a consequence of the tremendous consolidation during the compaction) and the cellular structure that remains after the compaction. The resiliency is similar in scientific origin as the elastomeric character of EG. Due to this resiliency, flexible graphite is commercially used as a gasket material, particularly for chemically and thermally harsh environments. The effectiveness of flexible graphite as a gasket material indicates that ­suitably

FIGURE 1.11  Flexible graphite. http://www.aliexpress.com/item/500x600x4mm-Flexible-Graphite-Paper-Pure-graphitepaper-Thermal-material-flexible-graphite-film-sheet/32235783640.html, public domain.

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nanostructured carbons or ceramics can be rendered to be appreciable in the viscous character. Intercalation requires the graphite raw material to be sufficiently graphitic. Exfoliation requires the graphite layers to be well oriented, so that the expansion along the c-axis is not hindered geometrically. Thus, exfoliation is much easier and much more extensive for graphite flakes than carbon fibers (including the fibers that are relatively graphitic). Nevertheless, by using a relatively graphitic form of carbon fiber, exfoliation has been achieved. Though the degree of expansion is limited, the cross-sectional shape of the fiber is changed (Anderson and Chung, 1984b)

1.1.6  Graphite Oxide In contrast to the aforementioned ionic type of graphite intercalation compounds, graphite oxide (GO and also known as graphitic acid) is a covalent type of graphite intercalation compounds. The covalent bonding stems from the presence of conjugated double bonds within the carbon planes. The layer planes assume a wavy form because of the change of the carbon bonding from the trigonal (sp2) form to the tetrahedral (sp3) form. The GO is a compound of carbon, oxygen, and hydrogen, with the oxygen and hydrogen being associated with functional groups (Fig. 1.12). This compound is prepared by treating graphite with strong oxidizing agents. When GO is oxidized to its maximum degree, the solid is yellow in color and the C:O ratio is between 2.1 and 2.9. Due to this structure, GO is much less conductive than graphite, with an electrical conductivity that depends on the oxygen content, which may be determined by using the Boehm titration method (Contescu et al., 1997; Goertzen et al., 2010; Kim et al., 2012b; Lausevic and Lausevic, 2011; Oickle

FIGURE 1.12  A structural model of graphite oxide, showing oxygen-containing functional groups. A, Epoxy bridges; B, hydroxyl groups; C, pairwise carboxyl groups. https://commons.wikimedia.org/wiki/File:Graphite_oxide.svg, public domain.

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  13

et al., 2010). The GO retains the layer structure of graphite, but it has a much larger and irregular interplanar spacing. Due to the relatively easy separation of the somewhat puckered topography of its atomic layers, GO can be easily exfoliated through dispersion in water, thereby forming stacks (flakes) with about 10 carbon layers or less per stack. Such stacks are also known as graphene oxide. As the chemical reduction of GO forms graphite, the dispersed GO is a widely used precursor for graphene (Hansora et al., 2015; Srivastava and Pionteck, 2015; Zhu et al., 2010). A graphene-based fiber, also known as graphene fiber, refers to a fiber in the form of graphene flakes that cling together and exhibit preferred orientation along the fiber axis. It can be prepared by the wet spinning of a liquid (e.g., water) dispersion of GO flakes to form a GO fiber, followed by the chemical or thermal reduction of the GO to graphene (Meng et al., 2015; Xu and Gao, 2014). The resulting fiber is attractive for its ductility (about 5.8%), but it is inadequate for structural applications, due to the low modulus (7.7 GPa) and low strength (140 MPa) (Xu and Gao, 2014).

1.1.7  Lattice Vibrations of Graphite Diffraction, such as X-ray diffraction is effective for probing the crystalline part, with the dominant diffraction peak being the 002 peak. However, diffraction is not effective for probing the amorphous or disordered part. On the other hand, Raman scattering is effective for probing both the crystalline and amorphous parts, both of which give a peak at a Raman shift of 1580 cm−1, due to the E 2 g 2 vibrational mode of graphite (Fig. 1.13). This peak is known as the G peak, due to its association with ordered graphite and involves the

FIGURE 1.13  The lattice vibration modes of graphite. Both in-plane and out-of-plane vibrations are involved.

14  Carbon Composites

in-plane bond-stretching motion of sp2-hybridized carbon atoms. In addition, the amorphous or disordered carbon gives a Raman peak (known as the D peak, with D referring to disorder) at 1350 cm−1. The ratio of the intensities of the two peaks is commonly used as an indication of the degree of order of the carbon material (Reich and Thomsen, 2004; Pimenta et al., 2007; Dresselhaus et al., 2010). A decrease of the D/G ratio indicates an increase in the degree of order. In addition, Raman spectroscopy is able to distinguish among the various allotropes of carbon (Hodkiewicz, 2010).

1.2  Carbon Fibers 1.2.1  Properties of Carbon Fibers Carbon fibers refer to fibers which are at least 92 wt.% carbon (elemental carbon) in composition. Their diameter typically ranges from 5 to 10 µm. They are attractive for their combination of low density, high elastic modulus and high strength, as needed for lightweight structures (Beckwith, 2010; Liu and Kumar, 2012). In addition, carbon fibers are attractive for their thermal conductivity, which is valuable for heat dissipation, as n ­ eeded for relieving the thermal load of aircraft. Furthermore, carbon fibers exhibit electrical conductivity, which enables their use for electromagnetic interference (EMI) shielding (Chung, 2004a, 2012; Rahaman et al., 2011) and resistive (Joule) heating ­(Athanasopoulos and Kostopoulos, 2012). In addition, carbon fiber polymer-matrix composites may be used to replace metal (titanium) bone implants (Petersen, 2011). The properties of carbon fibers vary widely depending on the structure of the fibers. In general, attractive properties of carbon fibers include the following: • • • • • • • • • • •

low density, high tensile modulus and strength, low thermal expansion coefficient, thermal stability in the absence of oxygen to over 3000°C, excellent creep resistance, chemical stability, particularly in strong acids, biocompatibility, high thermal conductivity, low electrical resistivity, availability in a continuous form, decreasing cost (versus time). Disadvantages of carbon fibers include the following:

• anisotropy (in the axial versus transverse directions), • low strain to failure, • compressive strength is low compared to tensile strength (∼50% of the tensile strength, Zhang et al., 2011b),

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  15

• tendency to be oxidized and become a gas (e.g., CO) upon heating in air above about 400°C • oxidation of carbon fibers is catalyzed by an alkaline environment. As each property is determined by the structure, the different properties are interrelated. The following trends usually go together: • increase in the tensile modulus, • decrease in the strain to failure, • decrease in the compressive strength. The quality of carbon fibers depends significantly on the detailed processing conditions used in the fabrication of the fibers. The conditions affect the porosity of the precursor fiber, the uniformity of the fiber diameter, the crystallite size, etc. The processing ­conditions include the conditions for spinning, plasticization drawing, finishing and ­drying (Radishevskii et al., 2005). Table 1.1 shows a comparison of the properties of the three main types of s­ tructural fibers, namely carbon fiber, glass fiber, and Kevlar fiber, in addition to carbon steel (­ Wonderly et al., 2005). The density of carbon fiber is lower than that of glass fiber, but is higher than that of Kevlar fiber. For any of the three types of fiber, the density is much lower than that of carbon steel. The specific modulus refers to the modulus divided by the specific gravity (i.e, the density in g/cm3). The specific strength refers to the strength ­divided by the specific gravity (i.e, the density in g/cm3). The tensile modulus and the specific tensile modulus of carbon fibers are higher than those of glass fibers and Kevlar (aromatic polyamide, i.e., polyaramid) fibers. The tensile modulus of carbon fiber is slightly higher than that of steel, while the specific tensile modulus of carbon fiber is much higher than that of steel. The tensile strength and specific tensile strength are comparable for the three types of fiber and the values for both quantities are higher than those of steel. Table 1.1  Comparison of the Basic Properties of Carbon Fiber, Glass Fiber and Kevlar Fiber and Carbon Steel Property

Carbon Fiber (T300)

Glass Fiber (S-2) Kevlar Fiber (49)

Carbon Steel (Not Fiber)

Density (g/cm3) Tensile modulus (GPa) Specific tensile modulus (GPa) Tensile strength (GPa) Specific tensile strength (GPa) Tensile strain (ductility) Compressive strength (GPa) CTE (axial, 10−6 K−1)

1.76 230 131 3.53 2.010 1.5% 0.87a −0.41

2.46 86.9 35.3 4.89 1.990 5.7% 1.60 2.9

7.85 190–210 24.2–26.8 0.276–1.882 0.035–0.24 10–32% / 11.0–16.6

1.45 112 77.2 3.00 2.070 2.4% / −6

There are various grades of each type of fiber. A commonly used grade is chosen to represent each type of fiber. The data are from the manufacturers’ datasheets, unless stated otherwise. CTE, Coefficient of thermal expansion. a Calculated value (Kumar et al., 2013).

16  Carbon Composites

As shown in Table 1.1, the compressive strength of carbon fiber is lower than that of glass fiber. For carbon fiber, the tensile strength is much higher than the compressive strength. The tensile strain at failure (the ductility) is considerably lower for carbon fiber than glass or Kevlar fiber. For all three types of fiber, the strain at failure is much lower than that of steel. The coefficient of thermal expansion (CTE) along the fiber axis is negative for carbon fiber and Kevlar fiber, but is positive for glass fiber. The negative CTE value of carbon fiber is due to the carbon in-plane interatomic bond distance increasing as the temperature increases, such that this bond distance increase is accompanied by increase in the degree of waviness of the layers. As a consequence of the increased waviness, the carbon layers are shortened. The fact that the axial CTE of carbon fiber is negative, is consistent with the fact that the in-plane CTE of graphite is negative below 400°C. The negative value is a consequence of the lattice vibration modes of graphite (Kelly and Walker, 1970). These modes are illustrated in Fig. 1.13. The higher is the temperature, the greater is the amplitude of the thermal vibration. An asymmetry in the extent of inward and outward vibration of the atoms that make up a bond gives rise to the change in the average bond distance as the temperature increases, and hence the phenomenon of thermal expansion. The negative CTE value of Kevlar fiber is similarly due to the long polyamide molecules becoming wavier in the molecular configuration, in spite of the increase in interatomic bond distance, as the temperature increases. The axial CTE is much more negative for Kevlar fiber than carbon fiber, due to the greater ease of bending for a molecule than a carbon layer. For all three types of fiber, the CTE magnitude is much lower than that of steel. Compared to glass fiber and Kevlar fiber, carbon fiber is clearly advantageous in the high tensile modulus and the low magnitude of the CTE. Additional advantages not shown in Table 1.1 are the high temperature resistance, chemical resistance, electrical conductivity and thermal conductivity, although the electrical/thermal conductivity is advantageous for some applications (e.g., lightning protection, electrostatic energy harvesting, EMI shielding, resistance heating, microelectronic heat sinks, and thermal straps) and disadvantageous for some other applications (e.g., printed circuit boards that require electrical insulation ability). EMI shielding refers to the blocking of radio waves, so that they cannot interfere electronic devices (Chung, 2012). The mechanisms include both absorption and reflection of the radiation. Electrostatic energy harvesting refers to the collection of the static electricity and storing the associated charges in a capacitor during the flight of a carbon fiber composite aircraft (Xie et al., 2015). Resistance (Joule) heating refers to the use of the carbon fibers as a heating element (Athanasopoulos and Kostopoulos, 2012). When a high electric current (current density 98,400 A/m2) is applied to a carbon fiber polymer-matrix composite, Joule heating causes the temperature to rise substantially both within the specimen and at the two electrical contacts used to pass the current (Deierling and Zhupanska, 2011). The quality of the electrical contacts is important. Lightning protection is needed for aircraft and requires a good electrical conductor for dissipating the electric charges resulting from the lightning. The electrical c­ onductivity of

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  17

carbon fiber polymer-matrix composites is not adequate for lightning protection, particularly due to the common presence of excess polymer matrix on the surface of the composite. The most common method of alleviating this problem is the inclusion of a metal (e.g., copper) wire mesh as the outer layer of a carbon fiber polymer-matrix laminate during composite fabrication (Kawakami and Feraboli, 2011). Another method involves the coating of the composite with aluminum; one of the methods involves plasma spraying (giving aluminum that adheres better) followed by cold spraying (spraying aluminum particles of size 3 µm to form a coating of thickness 30 µm, thereby giving aluminum that conducts better) (Affi et al., 2011). Yet another method involves coating the carbon fibers with ­nickel-coated carbon nanotubes (CNTs), which lie on the fiber surface like a mat and improve the electrical conductivity of the fibers (Chakravarthi et al., 2011). Compared to glass fibers and Kevlar fibers, carbon fibers are advantageous in the ability to withstand higher temperatures. The softening point of the glass fiber is 1056°C. The maximum service temperature of the Kevlar fiber is around 149–177°C. In contrast, in the absence of oxygen, carbon fiber can withstand temperatures as high as 3000°C. In addition, carbon fibers are advantageous in their low CTE. Heat sinks are needed for heat dissipation from microelectronics and a low CTE (as provided by the presence of carbon fibers) is attractive for this application, due to the low CTE of semiconductors (Kuroda et al., 2012). A thermal strap refers to a flexible linkage between a heat source (such as a sensor) and a heat sink (such as a cold finger, a heat pipe, and a radiator). It typically uses metals in the form of aluminum or copper wires that may be braided. However, carbon fiber polymer-matrix composites that utilize a high-thermal-conductivity type of carbon fiber are attractive for both the thermal conductivity and the weight saving, which is important for aerospace applications (Usinger et al., 2012). Pitch-based carbon fibers tend to be superior to polyacrylonitrile (PAN)based carbon fiber in the thermal conductivity, with values up to about 1000 W/(m·K) (Murakami and Ohno, 2012; Uetani et al., 2014), which is higher than the value of 400 W/ (m·K) for copper. The radial CTE of carbon fiber is positive and much greater in magnitude than the axial CTE. For example, for a carbon fiber with axial CTE −0.7 × 10−6 K−1 (negative), the radial CTE is +10 × 10−6 K−1. This reflects the preferred orientation of the carbon layers along the fiber axis and the weak out-of-plane bonding (van der Waals’ forces) compared to the strong in-plane bonding (covalent plus metallic bonding). Kevlar fiber is even more anisotropic, with the axial CTE being −6 × 10−6 K−1 and the radial CTE being +54 × 10−6 K−1. In general, weaker bonding is associated with a higher CTE. Carbonization refers to the conversion of an organic substance into carbon or a carboncontaining residue through pyrolysis. Pyrolysis refers to a thermochemical ­decomposition of an organic material at an elevated temperature in the absence of a reactive gas, such as oxygen and halogen. The decomposition is irreversible and involves a change in the chemical composition. Carbon fibers are commonly made by the carbonization of organic materials, such as from polymers and pitch (Lewis, 1982). PAN is the most common polymeric carbon

18  Carbon Composites

Table 1.2  Mechanical Properties of Selected PAN-Based and Pitch-Based Carbon Fibers (Naito et al., 2009a, 2009b) PAN-Based

Pitch-Based

Property

Toray T300

Toray T1000GB

Mitsubishi K13D

Nippon XN-05

Diameter (µm) Density (g/cm3) Tensile modulus (GPa) Tensile strength (GPa) Failure strain (%) Flexural strength (GPa) Flexural modulus (GPa)

7.7 1.76 220 3.2 1.5 5.2 220

5.1 1.80 290 5.7 2.1 8.2 260

11.5 2.20 940 3.2 0.4 2.1 1000

9.3 1.65 41 1.1 2.8 3.0 55

PAN, Polyacrylonitrile.

f­ iber precursor material. It is a semicrystalline polymer with chemical formula (C3H3N)n. ­Although PAN is a thermoplastic polymer, it does not melt under normal conditions. This is because it tends to degrade before melting. The PAN family of polymers is commonly copolymers made from mixtures of monomers with acrylonitrile as the main component. Pitch is composed of aromatic hydrocarbons and is produced by the distillation of carbonaceous materials, such as crude oil, coal, and plants. It is isotropic, though it can be made anisotropic by heat treatment. Table 1.2 shows that the mechanical properties vary considerably among the different grades of carbon fiber. The pitch-based carbon fibers are among those that give the highest values of the modulus (tensile or flexural), as shown for the Mitsubishi K13D fiber, although not all pitch-based fibers exhibit high modulus. For example, the pitch-based Nippon XN-05 fiber does not exhibit high modulus, but high ductility. The PAN-based carbon fibers are among those that give the highest values of the strength (tensile or flexural), as shown by the PAN-based Toray T1000GB fiber. The Mitsubishi K13D fiber exhibits an exceptionally high modulus that exceeds 900 GPa. This fiber also exhibits a relatively high density, which indicates a higher degree of order in the microstructure. The density of 2.20 g/cm3 for this fiber approaches the value of 2.26 g/cm3 for graphite. The Toray T1000GB fiber exhibits an exceptionally high strength of around 6 GPa or above. This fiber also exhibits a relatively small diameter, which promotes high strength, due to the smaller chance of having a flaw within the small diameter. Table 1.3 shows that the increase in the longitudinal tensile modulus (which is due to an increase in the degree of graphitization) is associated with a decrease in the transverse compressive modulus, and hence an increase in the ratio of the longitudinal tensile modulus to the transverse compressive modulus. In other words, the fiber becomes more anisotropic as the degree of graphitization increases. In addition, Table 1.3 shows that the transverse compressive strength decreases while the longitudinal tensile strength varies slightly in a nonsystematic manner as the degree of graphitization ­increases.

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  19

Table 1.3  Mechanical Properties of a Family of Mesophase-Pitch-Based Carbon Fibers in the Longitudinal and Transverse Directions (Kawabata, 1990) Longitudinal Transverse Ratio of Longitudinal Ten- Longitudinal Transverse Fiber Type Tensile Modulus Compressive sile Modulus to Transverse Tensile Strength Compressive (Thornel) (GPa) Modulus (GPa) Compressive Modulus (GPa) Strength (GPa) P-25 P-55 P-75 P-100 P-120

190 505 528 758 762

9.95 6.75 4.85 4.07 3.08

19 75 109 186 247

2.45 2.35 4.73 3.24 3.43

0.64 0.34 0.22 0.13 0.079

1.2.2  Carbon Fibers vs. Competing Materials Table 1.4 shows a comparison of the specific strength (strength divided by the density) of various materials. In terms of the specific strength, carbon fiber is better than glass fiber and spider silk, is comparable to Kevlar fiber, but is inferior to Spectra fiber (made from ultra-high-molecular-weight polyethylene). The specific strength of carbon fiber is higher than those of metals (steel alloy and aluminum alloy), and is higher than those of monolithic polymers (polypropylene and Nylon) and wood (balsa and oak). It is also higher than that of carbon fiber composite, which has only a part of its volume occupied by the fibers. Table 1.5 shows the tensile strength of various materials in comparison. Carbon fiber exhibits higher strength than any of the other materials listed, though carbon steel 1090 and E-glass fiber are almost as strong. Stainless steel AISI 302 and aluminum alloys exhibit much lower strength than carbon fiber. Among the polymers listed, Kevlar exhibits the highest strength, though its value is much lower than that of carbon fiber. Table 1.4  The Specific Strength of Various Materials in Comparison Material

Specific strength (Pa·m3/g)

Nylon Oak Polypropylene Aluminum alloy Steel alloy Balsa axial load Carbon fiber epoxy-matrix composite Spider silk Glass fiber Carbon fiber Polyaramid (Kevlara) fiber Polyethylene (Spectraa) fiber

69 87 89 222 254 521 785 1069 1307 2457 2514 3619

Spectra fiber is made from ultra-high-molecular-weight polyethylene. Polyaramid fibers are made from a polymer, namely ­­­ poly(p-phenylenediamine terephthalate). a Trademark. Source: http://www.christinedemerchant.com/carboncharacteristics.html, public domain.

20  Carbon Composites

Table 1.5  Tensile Strength of Various Materials in Comparison Material

Strength (MPa)

Polypropylene HDPE High density polyethylene Pine wood (parallel to grain) Aluminum alloy 6063-T6 Aluminum alloy 2014-T6 E-glass fiber polymer-matrix composite Carbon fiber polymer-matrix composite Kevlar fiber (49) Carbon fiber (T300) Glass fiber (S-2)

19.7–80 37 37 40 248 483 1500 1600 3000 3530 4890

E-glass stands for electrical grade glass, which is a low alkali glass that was originally developed for electrical insulators associated with electrical wiring. However, it is now used mostly as reinforcement in composites. HDPE, High-density polyethylene. Source: http://www.christinedemerchant.com/carboncharacteristics.html, public domain.

Table 1.6  Electrical Resistivity (at 20°C) of Various Materials in Comparison Material

Resistivity (Ω·cm)

Copper Iron Nichrome (Ni-Cr20) Carbon Silicon Paraffin Quartz (fused) Teflon (polytetrafluoroethylene)

1.59 × 10−6 1.0 × 10−5 1.1 × 10−4 3.5 × 10−3 6.40 × 104 1019 7.5 × 1019 1024–1026

Due to the electrical conductivity of carbon fibers, carbon fiber composites are used for EMI shielding, which is needed to protect electronics from interference from radio waves, such as those emitted from cellular phones and microwave devices and to prevent the radiation to be emitted from the sources. In addition, the conductivity allows the carbon fiber composites to provide electrostatic dissipation (antistatic). As shown in Table 1.6, carbon is intermediate in resistivity between the values of metals and insulators. The electrical resistivity of carbon fibers is typically around 2 × 10−3 Ω·cm, which is the value for Toray T800H carbon fiber (Nishi and Hirano, 2007). The higher is the degree of crystallographic order in the fiber, the lower is the resistivity. Due to their thermal conductivity, carbon fibers are attractive for heat dissipation, with applications, such as heat sinks in microelectronics. In contrast to copper or aluminum heat sinks, carbon fiber composite heat sinks exhibit low values of the CTE. Low CTE is needed due to the low CTE of the semiconductor chips and the need to reduce thermal stress resulting from CTE mismatch. Structures may also need heat dissipation, as in the case of aircraft, which can get hot near the engine (particular high-power e ­ ngines) and near high-power devices (e.g., lasers) that may be present in military aircraft. Table 1.7 shows

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  21

Table 1.7  Thermal Conductivity of Various Materials in Comparison Material

Thermal Conductivity [W/(m·K)]

Air Mineral wool insulation Pine Plywood Borosilicate (Pyrex) glass Quartz Carbon fiber epoxy-matrix composite Carbon steel Aluminum

0.024 0.04 0.12 0.13 1 3 24 54 250

Source: http://www.christinedemerchant.com/carboncharacteristics.html, public domain.

Table 1.8  CTE Values of Various Materials in Comparison Material

CTE (10−6 K−1)

Steel Aluminum Brass Glass fiber polymer-matrix composite Carbon fiber polymer-matrix composite (unidirectional)

13 23 20 13–14 −0.6 to + 14

Source: http://www.christinedemerchant.com/carboncharacteristics.html, public domain.

the thermal conductivity of various materials in comparison. Carbon fiber p ­ olymer-matrix composites are not as thermally conductive as carbon steel or aluminum, but they are much higher than those of quartz and glass. Carbon fiber differs from most metals in their low CTE, as shown in Table 1.8. The value for carbon fiber varies, depending on the degree of crystallinity, and can even be slightly negative. The value for carbon fiber composite depends on the degree of fiber alignment and the fiber volume fraction.

1.2.3  Structure of Carbon Fibers A carbon fiber is typically cylindrical, with a surface that is not completely smooth, as shown in Fig. 1.14, which is for an unsized (i.e., without coating) PAN-based carbon fiber (manufactured by Zoltek) of diameter 7.3 µm, electrical resistivity 1.55 × 10−3 Ω·cm, tensile strength 3800 MPa, tensile modulus 228 GPa, elongation at failure 1.5%, and density 1.81 g/cm3. The surface undulations are typically in the form of striations along the fiber axis. The carbon atomic layers in a carbon fiber (whether crystalline or amorphous) are not randomly oriented. Rather, they have a preferred orientation such that the layers tend to be aligned along the axis of the fiber. This does not mean that all the layers are exactly aligned. Moreover, it does not mean that the layers are flat. In fact, the layers tend to be

22  Carbon Composites

FIGURE 1.14  SEM photograph of the side view of a PAN-based carbon fiber (Muthusamy and Chung, 2010).

bent while the preferred orientation exists (Fig. 1.15). For example, the layers can be circumferential at the cylindrical edge of the fiber; they can be radial (akin to the spokes of a bicycle wheel) (Fig. 1.16); they can also be randomly bent. In the same fiber, there can be more than one type of bending. An example is the combination of circumferential bending at the cylindrical edge (skin) and radial microstructure at the interior part (core), as illustrated in Fig. 1.16B. The radial microstructure tends to be present in relatively graphitic fibers. It can be exposed by burning off the skin by heating, thereby improving the electrochemical behavior of the fiber (Frysz et al., 1994). Another example is the combination of circumferential bending at the skin and random bending in the core. The random microstructure tends to be present in fibers that are not graphitic. Such heterogeneity in the microstructure is known as skin-core heterogeneity. Even for the case in which the fiber is essentially all glassy, a thin graphitic skin can be present (Kaburagi et al., 2005). The thickness of the skin is typically around 0.1 µm for PAN-based carbon fiber heat treated at 2500°C. For PAN-based carbon fibers heat treated at 1000 or 1500°C, the skin

FIGURE 1.15  Preferred orientation of a bent carbon layer along the axis of a carbon fiber.

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  23

FIGURE 1.16  The cross-sectional microstructure of a mesophase-pitch-based carbon fiber (Thornel P-100). (A) SEM photograph obtained after 17% burn-off, which removes the skin. (B) Schematic of the fiber before the burn-off, with the carbon layers being circumferential in the skin, so that the c-axis is radial. (C) Schematic of the fiber after the burnoff, with the skin removed and the radial carbon layers being exposed at their edges (Frysz et al., 1994).

thickness is smaller, corresponding to just a few carbon layers. This is attributed to the growth of the skin inward as the heat-treatment temperature increases above 1800°C (Bennett, 1976; Oberlin, 1988). The fiber texture with a circumferential skin and a radial core tends to occur for highly graphitized pitch-based carbon fibers. Heating can cause the burning off of the skin, thereby exposing the edges of the carbon layers that make up the radial core. This exposure results in the formation of oxygen-containing surface functional groups (Fig. 1.17) that reduce the surface tension (improving the wettability), thereby improving the electron transfer rate and the electrochemical reversibility when the fiber is used as an electrochemical electrode (Frysz et al., 1994). The functional groups on carbon fiber desorb primarily carbon monoxide (rather than carbon dioxide) upon heating and are thus mainly phenol, carbonyl, and quinone. Preferred orientation (also known as crystallographic texture) means that there is a degree of alignment so that the orientation is not random. This texture stems from the fiber fabrication process, which typically involves the conversion of polymer fibers to carbon fibers by heating. The heating causes a decomposition reaction known as pyrolysis or carbonization, and that preferably occurs around 1500°C, such that the heating must be conducted in an inert atmosphere (in the absence of oxygen). Alternatively and less conventionally, carbonization may be conducted using a microwave-assisted plasma. The higher is the heat-treatment temperature during fiber fabrication, the greater is the degree of preferred orientation, due to the associated higher degree of order. The high modulus

24  Carbon Composites

FIGURE 1.17  Some functional groups on carbon (Frysz et al., 1994).

of a carbon fiber stems from the fact that the carbon layers, though not necessarily flat, tend to be parallel to the fiber axis. This crystallographic preferred orientation is known as a fiber texture. A model of a pitch-based carbon fiber involves continuous defective GNRs that are arranged in stacks (Emmerich, 2014). The properties of carbon fibers strongly depend on the microstructure (Huang and Young, 1995). The properties include tensile modulus, tensile strength, electrical resistivity, and thermal conductivity. The structural aspects that are particularly important are (1) the degree of crystallinity, (2) the interlayer spacing (d002), (3) the crystallite sizes or, more accurately, the coherent lengths perpendicular (Lc) and parallel (La) to the carbon layers (Yamamoto et al., 2001), (4) the texture (preferred orientation of the carbon layers) parallel and perpendicular to the fiber axis, (5) the transverse and longitudinal radii of curvature (rt and rl) of the carbon layers, (6) the domain structure, and (7) the volume

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  25

fraction, shape, and orientation of microvoids. A high degree of crystallinity, a low interlayer spacing, large crystallite sizes, a strong texture parallel to the fiber axis, and a low density of in-plane defects (disclinations, i.e., line defects in which rotational symmetry is violated.) generally result in a high tensile modulus, a low electrical resistivity, and a high thermal conductivity. A weak texture perpendicular to the fiber axis, small values of rt and rl, a large amount of defects and distortions within a layer, a large value of Lc, and a low volume fraction of microvoids contribute to a high tensile strength. However, a large Lc value may be accompanied by reduced lateral bonding between the stacks of carbon layers, thereby degrading the strength. The structure is affected by the processing of the fibers, particularly the heat-treatment temperature and the ease of graphitization of the carbon fiber precursor. PAN-based carbon fibers, even after heat treatment beyond 2000°C, remain turbostratic (i.e., no graphitic ABAB stacking of the carbon layers) (Duerbergue and Oberlin, 1992). Turbostratic carbon fibers typically have the carbon layers in a folded and crumpled configuration, though the layers have preferred orientation along the fiber axis (Fig. 1.10). The interplanar spacing d002 decreases while Lc and La increase with the heat-treatment temperature. The Lc increases with the heat-treatment temperature, such that its value is higher for pitch-based carbon fibers than PAN-based carbon fibers that have been heattreated at the same temperature. For PAN-based fibers, Lc increases sharply above 2200°C, whereas Lc increases smoothly with increasing temperature for pitch-based fibers. The ­fiber density tends to increase with Lc (Takaku and Shioya, 1990). Table 1.9 shows the structural parameters of various carbon fibers, as determined by X-ray diffraction. The interplanar spacing d002 is relatively low for the Thornel P-100 ­mesophase-pitch-based carbon fiber, which exhibits a high degree of graphitization, though the value is still higher than that of graphite [3.35 Å, Fig. 1.1A]. For the fibers of lower degrees of graphitization (Thornel P-25 mesophase-pitch-based carbon fiber and the PAN-based AS-4 carbon fiber), d002 is even larger than that of the P-100 fiber. The Lc and La values are much higher for P-100 than P-25 or AS-4. The azimuthal spread, which describes the spread of the carbon layer orientation relative to the fiber axis (the lower the spread, the higher is the degree of preferred orientation), is much lower for P-100 than P-25 or AS-4 (Ferguson et al., 2010). The La parallel to the fiber axis is referred to as La||; La perpendicular to the fiber axis is referred to as La⊥. Both quantities increase with increasing Lc, but La|| is larger than La⊥. for the same value of Lc (Takaku and Shioya, 1990). The volume fractions of crystallites (vc) describe the degree of crystallinity; it increases with increasing Lc. Table 1.9  The Structural Parameters of Various Carbon Fibers (Ferguson et al., 2010) Fiber

Precursor

d002 (Å)

Lc (Å)

La (Å)

Azimuthal Spread (°)

AS-4 P-25 P-100

PAN Pitch Pitch

3.420 3.439 3.382

17 26 227

23 28 235

34 32 5.6

26  Carbon Composites

As a result of the texture, a carbon fiber has a higher modulus along the fiber axis than directions perpendicular to the fiber axis. The direction perpendicular to the fiber axis is known as the transverse direction. Similarly, the electrical and thermal conductivities are higher along the fiber axis than the transverse direction, and the CTE is lower along the fiber axis than the transverse direction. The greater is the degree of alignment of the carbon layers parallel to the fiber axis (i.e., the stronger the fiber texture), the greater are Lc, the density, the carbon content, and the tensile modulus, electrical conductivity, and thermal conductivity along the fiber axis. The correlation of a stronger texture with a higher density relates to the correlation of a stronger texture with a higher degree of crystallinity/order, which in turn correlates with a lower interplanar spacing. The correlation of a stronger texture with higher carbon content relates to the correlation of a stronger texture with a higher degree of crystallinity/ order, which in turn correlates with a higher degree of purity. Moreover, the stronger is the fiber texture, the smaller are the fiber’s CTE and tensile strength. The effect of the texture on the CTE stems from the higher CTE in the direction perpendicular to the carbon layers than the direction in the plane of the carbon layers. Strength refers to the resistance to fracture, whereas the modulus describes the resistance to elastic deformation. A stronger texture results in a lower tensile strength, because of the greater ease of sliding between the carbon layers when the texture is strong. In contrast, a stronger texture results in a higher modulus, because of the higher modulus in the plane of the carbon layers than in the direction perpendicular to the layers. Therefore, a strong texture, which tends to occur when the degree of crystallinity/order is high, is not attractive for achieving high strength, though it is attractive for achieving high modulus. As a consequence, carbon fibers are broadly classified into two types, namely high-­modulus fibers (which have a low degree of crystallinity/order) and high-strength fibers (which have a high degree of crystallinity/order).

1.2.4  Fabrication of Carbon Fibers Carbon fibers are fabricated from pitch fibers (e.g., petroleum pitch or coal tar pitch), polymer fibers (e.g., PAN Fig. 1.18, and cellulosic fiber), or carbonaceous gases (e.g., a ­ cetylene).

FIGURE 1.18  The polymerization reaction to from PAN, with the chemical formula (C3H3N)n from acrylonitrile. Though PAN is thermoplastic, it effectively does not melt because it degrades before melting. To convert a PAN fiber to a carbon fiber, the PAN fiber is first thermally oxidized in air at 230°C to form an oxidized PAN fiber and then carbonized above 1000°C in an inert atmosphere. PAN is used as the precursor for 90% of carbon fiber production. http://textilelibrary. weebly.com/polyacrylonitrile-pan-mfg-process.html, public domain.

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  27

Pitch, polymers, and carbonaceous gases are known as carbon precursors. A carbon precursor is converted to carbon by a reaction that occurs upon heating. Due to the evolution of gases during this conversion (known as carbonization), weight loss occurs. The weight loss is preferably low, so that the carbon yield is high. The weight loss of PAN fibers is higher than that of pitch fibers, but lower than those of other polymer fibers. In particular, the carbon yield of PAN is about double that of rayon, although PAN fibers are more expensive than rayon fibers. Moreover, PAN fibers have a higher degree of molecular orientation than rayon fibers. Pitch tends to be more graphitizable (i.e., having a greater tendency for becoming crystalline carbon upon heat treatment of the resulting carbon fiber) than polymers, such as PAN. As a result, graphitized carbon fibers made from pitch are attractive for the high values of their modulus, thermal conductivity, and electrical conductivity along the fiber axis. However, due to the high temperatures associated with the graphitization process, these fibers are relatively expensive. In contrast, polymers, such as PAN, are not graphitizable, so carbon fibers made from polymers, such as PAN, are relatively low in the degree of crystallinity. A low degree of crystallinity is attractive for high strength in the fibers. High strength is important for structural applications. In contrast, graphitized carbon fibers made from pitch are low in strength but high in modulus and thermal/electrical conductivity. Therefore, carbon fibers made by polymers, such as PAN are dominant in the commercial market, whereas graphitized carbon fibers made from pitch are used in special applications that require high thermal/electrical conductivity or high modulus. On the other hand, amorphous carbon fibers made from pitch without graphitization are relatively inexpensive, so they are used in low-cost structures, such as concrete. The price of pitch-based carbon fibers is expected to drop when the production volume increases. High thermal conductivity is needed for aircraft thermal management (Banisaukas et al., 2005). Table 1.10 shows that the thermal conductivity of carbon fibers varies over a wide range [from 9.4 to 1100 W/(m·K)]. Pitch-based carbon fibers tend to have much higher thermal conductivity, much higher tensile modulus, and higher density than PANbased carbon fibers, due to the high degree of graphitization and the higher degree of preferred orientation of the carbon layers along the fiber axis. However, the tensile strength tends to be lower for the pitch-based fibers. Table 1.10  The Thermal Conductivity of Continuous Carbon Fibers (Yu et al., 2015) Precursor PAN

Pitch

Fiber Designation

Density (g/cm3)

Thermal Conductivity Tensile Modulus Tensile Strength [W/(m·K)] (GPa) (MPa)

T300 T700 M55J K13D2U P120 P130 K1100

1.76 1.8 1.91 2.21 2.17 2.19 2.20

10.5 9.4 155.7 800 640 1100 900–1100

230 230 540 938 827 923 965

4210 4900 4020 3703 2410 2870 3172

28  Carbon Composites

Ribbon-shaped 3000°C-graphitized mesophase-pitch-based carbon fiber that exhibits high thermal conductivity [calculated to be >1100 W/(m·K) at room temperature]. The fibers are prepared by the melt spinning of naphthalene-derived mesophase pitch, followed by stabilization at 240–250°C in oxygen for 10–20 h, and subsequent heat treatment at 450°C in nitrogen for 1 h for the purpose of strengthening the fibers. The cross-sectional dimensions of a fiber are 1000 × 20 µm. As shown for fibers that have been graphitized at 2800°C, the carbon layers in a fiber are preferentially oriented along the 1000-µm dimension of the cross-section. The longitudinal electrical resistivity of the ribbon-shaped fibers graphitized at 3000°C is about 1.1 × 10−4 Ω·cm at room temperature. The oxidation resistance stability of this fiber is superior to that of the K-1100 pitch-based carbon fiber (Table 1.10). The tensile strength and elastic modulus of the ribbon-shaped fiber approach 2.53 and 842 GPa, respectively (Yuan et al., 2014a, 2014b). In general, carbon fibers made from PAN have high strength (3–7 GPa), moderately high modulus (200–500 GPa), compressive strength (1–3 GPa), shear modulus (10–15 GPa), and low density (1.75–2.00 g/cm3), so they are valuable for structural applications. Carbon fibers made from pitch excel in the high values of their modulus (≤1000 GPa), thermal conductivity [≤1100 W/(m·K)], and electrical conductivity (≤106 S/m), respectively (Minus and Kumar, 2005).

1.2.4.1  Fabrication of Carbon Fibers From Pitch Pitch used as a precursor for carbon fibers can be a petroleum pitch (such as a distillation residue obtained by the distillation of crude oil under atmospheric or reduced pressure, or a heat-treated product of the by-product tar obtained by the pyrolysis of naphtha), a coal tar pitch, or other pitches. Coal pitches are, in general, more aromatic than petroleum pitches. The coal pitch has a much higher benzene and quinoline-insoluble (QI) content. A high QI content usually means that the material has a high solid content. These solid carbon particles can accelerate coke formation during subsequent thermal processing of the pitch and lead to fiber breakage during extrusion, and thermal treatment. Therefore, although petroleum pitches are less aromatic, they are more attractive as precursors for carbon fibers (Edie, 1990). During the conversion of a pitch or polymer fiber to a carbon fiber, the fiber shape must be maintained. If the pitch or polymer melts, the fiber shape will be lost. Thus, the melting must be suppressed. This can be achieved by a chemical change of the molecular structure of the pitch or polymer, so that melting does not occur. This chemical change commonly involves cross-linking the polymer so as to prevent relaxation and chain scission during subsequent carbonization. The process involves oxidation of the molecules and is conducted in the presence of oxygen (air) at a moderately high temperature, typically in the range from 200 to 400°C. It is a diffusion process and thus takes time, for example, a few hours, depending on the diameter of the fiber. In case of PAN fibers, tension is applied during stabilization and carbonization in order to prevent relaxation of the molecular chains, thereby maintaining preferred orientation of the molecules and resulting in preferred orientation of the carbon obtained by carbonization. This process is known as stabilization or infusiblization, and must be conducted prior to carbonization.

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  29

FIGURE 1.19  The structure of a liquid crystal (B) compared to those of a crystalline solid (A) and an ordinary liquid (C). http://plc.cwru.edu/tutorial/enhanced/files/lc/intro.htm, public domain.

The carbon yield (also known as the char yield) refers to the fraction by mass of the precursor that becomes carbon after the carbonization process. The higher is the carbon yield, the less is the porosity after the carbonization. Porosity is detrimental to the mechanical properties. Therefore, carbon precursors that have a high carbon yield are preferred. The carbon yield of pitch is in the range from 80 to 85 wt.%, whereas that of PAN is in the range from 55 to 60 wt.% (http://pac.iupac.org/publications/pac/pdf/1985/ pdf/5711x1553.pdf). A liquid crystal is a liquid that has a degree of order for the molecules in the liquid (Fig. 1.19). A liquid crystal is said to be thermotropic if the degree of order is determined by the temperature; the higher is the temperature, the lower is the degree of order. Liquid crystals are typically thermotropic. Pitch is composed of aromatic hydrocarbons with a range of molecular size. It is thermoplastic, i.e., it softs and melts upon heating. The molten form of usual pitch is isotropic, but it can be made anisotropic by heat treatment. The heat treatment polymerizes the isotropic pitch to form a material with a higher molecular weight, namely mesophase pitch, which is in the form of fused aromatic chains and melts at around 300°C (higher than the melting temperature of isotropic pitch). Mesophase pitch is a type of anisotropic pitch that has its molten form being a liquid crystal, as enabled by its large molecules that involve aromatic rings in the molecular structure. Due to this structure, mesophase pitch can form linear molecular chains without the application of tension. Moreover, it can be melt spun into fibers without fiber breakage. In contrast, PAN requires the application of tension during the conversion of PAN fiber to carbon fiber. Furthermore, mesophase pitch has a high carbon yield and is effective as a precursor for making carbon fiber with a high degree of crystallinity and a strong texture. It is also attractive in that it does not degrade as the melting temperature is approached. As a consequence, it can be melt extruded without the need for solvents. The processing of mesophase pitch to form fibers is more difficult than that of isotropic pitch. This is because of its relatively high viscosity and the relatively strong dependence of the viscosity on the temperature. Nevertheless, mesophase pitch is a precursor of choice for making high-performance carbon fibers (Matsumoto, 1985). Pitch is a thermoplastic polymer, so it melts upon heating. The melt can be spun to form pitch fibers. The pitch fibers must be pyrolyzed (decomposed to carbon) by heating at ≥1000°C to form carbon fibers and they must maintain their shape during c­ arbonization,

30  Carbon Composites

so they must first undergo infusiblization (stabilization). Infusiblization is a process for rendering the pitch infusible. This process involves air oxidation at 250–400°C. After carbonization at ≥1000°C in an inert atmosphere, graphitization is optionally carried out at ≥2500°C, if a high modulus, a high thermal conductivity, or a low electrical resistivity is desired. The higher the graphitization temperature, the more graphitic is the resulting fiber. High-strength HT-type carbon fibers are formed after carbonization whereas highmodulus HM-type carbon fibers are formed after graphitization. If isotropic pitch is used as the precursor, the graphitization heat treatment has to be carried out while the fiber is being stretched. This costly process, called stretch-graphitization, helps to improve the preferred orientation in the fiber. On the other hand, if anisotropic pitch is used as the precursor, stretching is not necessary, because the anisotropic pitch has an inherently preferred orientation of its molecules. Isotropic pitch can be converted to anisotropic pitch by heating at 350–450°C for a number of hours (Okuda, 1990; Donnet and Bansal, 1990). The anisotropy refers to optical anisotropy; the optically anisotropic parts shine brightly if the pitch is polished and observed through the crossed nicols (polarizers) of a reflection type polarized light microscope. The anisotropy is due to the presence of a liquid crystalline phase, which is called the mesophase. The mesophase is in the form of small liquid droplets. Within each droplet, large planar molecules line up to form nematic order. The droplets (spherules) grow in size, coalesce into larger spheres, and eventually form extended anisotropic regions. The so-called mesophase pitch is a heterogeneous mixture of an isotropic pitch and the mesophase. The relative amounts of the two phases can be determined approximately by extraction with pyridine or quinoline. The isotropic fraction is soluble in pyridine, while the mesophase is insoluble due to its high molecular weight. The mesophase has a higher surface tension than the low-molecular-weight isotropic liquid phase from which it grows. As the proportion of mesophase increases, the viscosity of the pitch increases, so a higher temperature is required for subsequent spinning of the pitch into fibers. As the mesophase is heated, its molecular weight increases (it polymerizes), cross-linking occurs and the liquid eventually becomes solid coke. This solidification must be avoided in the spinning of carbon fibers. Moreover, the difference in density between the two phases in mesophase pitch causes sedimentation of the mesophase spherules. Although the sedimentation can be decreased by agitating the pitch, it makes it difficult to obtain homogeneous fibers from the pitch. Hence, there are pros and cons about the presence of the mesophase. Nevertheless, mesophase pitch is important for producing high-performance pitch-based carbon fibers. A method to produce mesophase pitch involves (1) heating the feed pitch (e.g., at 400°C in N2 for 14–32 h (Union Carbide, 1977), with or without deashing and distillation, to transform to mesophase pitch containing 70–80% mesophase, (2) allowing to stand at a slightly lower temperature so that the mesophase sinks, and (3) separating the mesophase by centrifuging (Donnet and Bansal, 1990; Otani and Oya, 1986). Mesophase pitch is used in the UCC process (Union Carbide, 1977). Due to the shortcomings of mesophase pitch, neomesophase pitch (optically anisotropic), dormant anisotropic pitch (optically isotropic), and premesophase pitch (optically isotropic) are used (Okuda, 1990).

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  31

The neomesophase pitch is produced by first removing the high-molecular-weight component by solvent extraction (using an aromatic solvent, such as toluene), as this component tends to form coke upon heating, and then heating at 230–400°C (Okuda, 1990). The neomesophase has a lower softening temperature than the mesophase, so it can be spun at a lower temperature, which reduces the coke formation (Donnet and Bansal, 1990). Neomesophase pitch is used in the EXXON process (Exxon, 1980/81). The dormant anisotropic pitch is between isotropic and mesophase pitches in nature. It is dormant in the sense that it does not interfere with spinning, but, on heating after spinning, it becomes active and orients itself (Donnet and Bansal, 1990). The process of forming dormant anisotropic pitch involves (1) heating pitch at 380,450°C to form anisotropic pitch containing several percent of mesophase, (2) hydrogenation of the anisotropic pitch to form isotropic pitch with a lower softening temperature, and (3) heating the isotropic pitch at 350–380°C to form dormant anisotropic pitch. This pitch results in a carbon fiber between GP and HP grades and with high elongation (Otani and Oya, 1986). The premesophase pitch is formed by (1) hydrogenation at 380–500°C using hydrogen donor solvents (such as tetrahydroquinoline), H2/catalysis and other techniques, and (2) heating the hydrogenated pitch at >450°C for a short time. This pitch is optically isotropic at the spinning temperature, but orients readily during heating subsequent to spinning. Coal-derived pitch is preferred to petroleum-derived pitch for this method, which is called the Kyukoshi method (Okuda, 1990; Otani and Oya, 1986). Dormant anisotropic pitch and premesophase pitch have a rather naphthenic nature, which is caused by hydrogenation (Okuda, 1990). A process not involving hydrogenation but involving the polymerization of naphthalene has been reported for producing an optically anisotropic pitch (Seo et al., 1991). The preparation of mesophase pitch from isotropic pitch involves heat treatment at 350,450°C. During the heating, an inert gas, such as nitrogen is often bubbled through the pitch to agitate the fluid and to remove the low-molecular-weight components. However, retention of some of these components is vital for the mesophase to have a low QI content and a low melting point. For retaining some of these components, a prior heat treatment either in the presence of a reflux or under a moderate pressure is effective (Rhee et al., 1991). The conversion from isotropic pitch to mesophase pitch is a time-consuming process which can take as long as 44 h. To promote this transformation, an oxidative component can be added to the inert purging gas. For example, the modified sparging gas can be nitrogen containing 0.1–2.0 vol.% oxygen (Fu and Katz, 1991). Other than having a high degree of aromaticity, pitches for making carbon fibers should have 88–93 wt.% C, 7–5 wt.% H, and other elements (e.g., S and N) totalling below 4 wt.% (Fu and Katz, 1991). Therefore, feed pitch needs to undergo deashing and distillation prior to the various processes mentioned previously. The spinning of mesophase pitch to form pitch fibers is difficult for a number of reasons (Donnet and Bansal, 1990).

32  Carbon Composites

1. The mesophase is viscous. 2. The higher spinning temperature of mesophase pitch compared to isotropic pitch causes additional polycondensation, which leads to gas evolution. Thus, the spinneret needs to be vented to avoid entrapping the gas bubbles in the carbon fibers. 3. The mesophase pitch has a heterogeneous structure, which consists of anisotropic mesophase and isotropic regions. In spite of the difficulties mentioned previously, mesophase pitch is used to produce high-modulus, high-strength carbon fibers having a highly oriented structure ­(Singer, 1977, 1978). The spinning of mesophase pitch is performed by a variety of conventional spinning methods, such as centrifugal spinning, jet spinning, and melt ­spinning. Melt spinning (more accurately termed melt extrusion) is most commonly used. It involves extruding the melted pitch into a gaseous atmosphere (e.g., N2) through nozzles directed downward, so that the extruded fibers are cooled and solidified. In the melt spinning process, an extruder is typically used to melt the pitch and pump it to the spin pack, which contains a filter for removing solid particles from the melt. After passing through the filter, the melt exits the bottom of the spin pack through a spinneret, which is a plate containing a large number of parallel capillaries. Airflow is often directed at the melt exiting from these capillaries in order to cool the fibers. The solidified fiber is finally wound onto a spinning spool. The capillary or orifice has a typical diameter of 0.1–0.4 mm. For spinning 10-µm diameter fibers at 2.5 m/s from an orifice of diameter 0.3 mm, a draw ratio of about 1000:l is required. The temperature of the nozzles is determined depending on the type of the pitch and the melt viscosity most suitable for spinning. An increase in the spinning temperature decreases the viscosity of the pitch. The viscosity in turn controls the microstructure of the resulting fiber. For example, when the spinning temperature is 349°C or below, a radialtype structure forms; when the spinning temperature is raised above 349°C, the structure changes from the radial-type structure to either the random-type structure or the radialtype structure surrounded by the onion-skin-type (concentric-circle-type) structure; at very low spinning temperatures, the structure is often accompanied by V-shaped grooves or cracks extending from the circumference toward the center of a fiber, so it is not desirable for the mechanical properties of the fiber (Otani and Oya, 1986). The design of the spinneret also affects the microstructure of the resulting fiber. Since the radial-type structure results from a laminar flow of mesophase pitch through the spinneret, it can be suppressed by changing the flow from laminar to turbulent. A turbulent flow can be obtained by using a spinneret hole with narrower and wider parts along the length of the hole or a hole containing a filter layer of stainless steel particles or mesh (Otani and Oya, 1986; Takai et al., 1990). The cross-sectional shape of the spinneret hole can be used to control the microstructure and cross-sectional shape of the resulting fiber (Otani and Oya, 1986). ­Noncircular carbon fibers are attractive in their increased surface area to volume ratio and the p ­ resence of crevices in some of the shapes. The crevices result in increased fiber wetting through

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  33

c­apillary action. Thus, noncircular carbon fibers may provide improved fiber-matrix bonding in composites (Edie et al., 1986). Short pitch fibers are made by melt blowing rather than melt spinning. Melt blowing involves melting the pitch and then extruding the pitch through a spinneret, such that a gas stream is passed through the spin head and allowed to exit parallel to the extruding fibers. The spin head heats the gas, and this hot gas draws the fibers down as they emerge from the spinneret capillary. The fibers are blown onto a moving conveyor. No winding takes place. This process is mostly used for producing short isotropic pitch-based carbon fibers (Edie, 1990). Before carbonization, as-spun pitch fibers are infusiblized or stabilized in order to prevent softening and resulting deformation of the pitch fibers upon heating. Stabilization (also called thermosetting) involves oxidation of the pitch molecules; the intermolecular interactions result in a higher softening point. The heating during stabilization is performed in air at 250–350°C, as provided by a cylindrical furnace placed below the spinning nozzles prior to windup or by blowing hot air through a spool of as-spun pitch fibers. The direct oxygen attack of individual pitch molecules results in the formation of ketone, carbonyl, and carboxyl groups (Hein, 1990). The oxidation reaction is accelerated by methyland hydro-groups, which also react with carbonyl groups (Lavin, 1992). The introduction of polar CO groups leads to hydrogen bonding between adjacent molecules. During subsequent carbonization at ∼1000°C, the oxidized molecules may serve as starting points for 3D cross-linking (Hein, 1990). A pitch with a higher softening point permits oxidation to take place at a higher temperature, thereby greatly reducing the time required for oxidation. Therefore, in isotropic pitch fiber production, a pitch with a higher softening point is preferred, even though it is less spinnable (Edie, 1990). Mesophase pitch fibers have higher softening points than isotropic pitch fibers, so they can undergo stabilization at a higher temperature, which makes the process faster. Indeed minutes are required for stabilizing mesophase pitch fibers, whereas hours are required for stabilizing isotropic pitch fibers (Donnet and Bansal, 1990). A skin-core structure with the skin richer in oxygen than the core can be introduced in mesophase pitch fibers by incomplete oxidative stabilization. The longer the time of stabilization, the thicker the skin; the skin is the stabilized part. However, stabilization slows down as it proceeds to the interior of a fiber. The oxygen distribution corresponds to a skin thickness of 5 µm. After 30 min of stabilization, the skin thickness has increased to 9 µm; after 90 min of stabilization, the skin has fully grown, leaving behind no core (Mochida et al., 1989; Matsumoto and Mochida, 1993). Incomplete oxidative stabilization may be followed by solvent extraction to help avoid adhesion among the fibers after carbonization. The solvent, such as tetrahydrofuran (THF) or benzene, serves to remove the soluble or fusible fractions in the surface layer. Incomplete oxidative stabilization followed by solvent extraction is called two-step stabilization (Mochida et al., 1991; Zeng et al., 1990). Due to the low tensile strength of pitch fibers (isotropic or mesophase pitch), fiber handling should be minimized during stabilization. The tensile strength and modulus of the

34  Carbon Composites

as-spun mesophase pitch fiber are much lower than those of the carbonized mesophase pitch fiber. In order to reduce fiber sticking and fusion during the stabilization treatment, colloidal graphite, an aqueous suspension of carbon black in ammonium 2-ethylhexyl s­ ulfate, silicone, or other lubricants, can be applied on the surface of the pitch fibers before ­stabilization (Donnet and Bansal, 1990; Koga et al., 1985). The separability of the individual filaments can be improved by using a suspension comprising a silicone oil (e.g., dimethylpolysiloxane) and fine solid particles (e.g., graphite, carbon black, silica, calcium carbonate, etc., of particle size 0.05–3 µm preferably) (Koga et al., 1985). After stabilization, the pitch fibers are carbonized by heating in a series of heating zones at successively higher temperatures ranging from 700–2000°C. An inert atmosphere is used to prevent oxidation of the resulting carbon fibers. During carbonization, the remaining heteroatoms are eliminated. This is accompanied by the evolution of volatiles, so a gradated series of heating zones is needed to avoid excessive disruption of the structure. The greatest quantity of gases, mainly CH4 and H2, are evolved below 1000°C. Above 1000°C, hydrogen is the principal gas evolved (Edie, 1990). For temperatures ≤2000°C, nitrogen can be used for the inert atmosphere. For temperatures >2000°C, nitrogen is not suitable because of the danger of nitrogen reacting with carbon to form a cyanogen; argon can be used instead. After carbonization, graphitization is carried out (optionally) by heating in an inert atmosphere at 2500–3000°C. The transverse (cross-sectional) fiber microstructure developed during fiber formation is retained after carbonization. This microstructure is influenced by the flow profile during extrusion from the spinneret and by the fiber elongation prior to windup (Edie, 1990). A variation of the melt spinning method involves spinning the pitch upward, such that the molten pitch goes through the spinneret upward and the extrusion face of the spinneret is in contact with a liquid (177–450°C), which has a density greater than that of the pitch. The density difference causes the fiber to move upward (due to buoyancy). On top of and in contact with this liquid layer is another layer of the same liquid at a higher temperature (500–650°C), which causes dehydrogenation of the fiber. The higher-temperature liquid is less dense than the lower-temperature liquid below it, so it stays on top. The liquid may be LiCl or KCl. On top of the top liquid layer is inert atmosphere at an even higher temperature (above 900°C) for further dehydrogenation, which results in carbon fibers containing more than 95 wt.% C. The main attraction of this form of melt spinning is the elimination of the oxidation step due to the support of the weak spun fiber by the high-density liquid around it (Kohn, 1976). By using a naphthalene-derived mesophase pitch as the carbon precursor, highly ­oriented ribbon-shaped carbon fibers have been obtained by melt spinning, oxidative stabilization, carbonization, and graphitization (Yuan et al., 2014a,c). These fibers provide uniform shrinkage upon heat treatment. This is in contrast to the shrinkage cracking that tends to occur in round-shaped fibers.

1.2.4.2  Fabrication of Carbon Fibers From Polyacrylonitrile The PAN fibers are produced from solutions of PAN spun into a coagulation bath. After this, PAN is converted to carbon through a number of chemical steps, which change the

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  35

FIGURE 1.20  (A) PAN fiber changing color (eventually to black) as it goes through the stabilization process. (B) Oxidized fibers moving to a high temperature furnace, where they are converted to carbon fibers. Part A, http://www.zoltek. com/carbonfiber/how-is-it-made/, public domain; part B, http://energy.gov/eere/articles/carbon-fiber-and-clean-energy-4uses-industry, public domain.

color of the fibers from gold to brown and to black (Fig. 1.20). The first step is the formation of rings in the molecular structure (the ring formation being known as cyclization) through the change from CqN to C═N (Fig. 1.21A) at around 300°C. The initiation of cyclization may be promoted by the use of additives (e.g., itaconic acid, which serves as a comonomer). The second step is the evolution of hydrogen gas at around 700°C (Fig. 1.21B). The third step is the bonding of adjacent molecular chains to form ribbons (Fig. 1.21C), along with more hydrogen gas evolution, upon slow heating at 400–600°C. The fourth step is the formation of wider ribbons through the evolution of nitrogen gas (Fig. 1.21D) at 600– 1300°C. The final product of the decomposition is carbon. This is akin to the conversion of oil to char (which is carbon) during cooking (e.g., barbeque). The reaction is known as pyrolysis (i.e., carbonization, which involves the removal of oxygen, nitrogen, and hydrogen from molecules to form carbon). Charring in barbeque, for example, is carbonization, but it differs from the aforementioned process in that it is conducted in the presence of oxygen from the air. Thus, pitch or polymer fibers are converted to carbon fibers.

36  Carbon Composites

C

N

C

N

C

N

C

C

N

C

N

C

N

N

C

N

Heat

Polyacrylonitrile

C

N

C

C

N

C

N

N

C

C

N

C

N

C

N

(A)

C

N

C

N

C

N

C

N

C

N

C

N

C

N

N

N

C

Heat, this time to 700°C

N

N

N +

(B)

N

N

H2 gas

FIGURE 1.21  The chemical steps associated with the conversion of PAN to carbon. http://web.mit.edu/3.082/www/ team2_f01/chemistry.html, public domain.

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  37

FIGURE 1.21  (cont.)

The polymerization to acrylonitrile to form PAN can yield a precipitated polymer by using a solvent in which the polymer is soluble. Suitable solvents include dimethyl formamide, dimethyl sulfoxide, and concentrated aqueous solutions of zinc chloride and sodium thiocyanate. All are liquids with highly polar molecular structures, as the polar groups attach to the nitrile groups, thereby breaking the dipole–dipole bonds (Watt, 1985).

38  Carbon Composites

The initiators used for the addition polymerization can be the usual ones, such as peroxides, persulfates, azo compounds, such as azo-bis-isobutyronitrile, and redox systems (Watt, 1985). The initiators provide free radicals for the initiation, which is the addition of a radical to an acrylonitrile molecule to form a larger radical. PAN is a white solid with a glass transition temperature of about 80°C and a melting temperature of about 350°C. However, PAN degrades on heating prior to melting. Polymer fibers can be fabricated by various spinning methods. 1. Melt spinning: extruding a melt of the polymer. 2. Melt-assisted spinning: extruding a homogeneous single-phase melt in the form of a concentrated polymer–solvent blend. 3. Dry spinning (Fitzer and Heine, 1988): extruding a solution of the polymer in a volatile organic solvent into a circulating hot gas environment in which the solvent evaporates. 4. Wet spinning (Fitzer and Heine, 1988): extruding a solution of the polymer in an organic or inorganic liquid into a coagulating liquid (a mixture of a solvent and a nonsolvent); this precipitates the polymer, which is then drawn out as a fiber. 5. Dry-jet wet spinning: extruding a solution of the polymer into an air gap (∼10 mm), followed by a coagulating bath, in order to enhance orientation prior to coagulation. All methods involve pumping the melt or solution of the polymer through a large number of small holes in a stainless steel disc, called a spinneret, such that the hole diameter is about twice the final diameter of the fiber. Spinning in clean-room conditions produces better PAN fibers (Gupta et al., 1991). Since PAN decomposes below its melting temperature, melt spinning is not possible. Melt-assisted spinning of PAN uses a solvent in the form of a hydrating agent to decrease the melting point and the melting energy of PAN by decoupling nitrile–nitrile association through the hydration of pendant nitrile groups. With a low melting point, the polymer can be melted without much degradation (Daumit et al., 1990a, 1988). Water is most commonly used as the hydrating agent. Water-soluble polyethylene glycol (PEG) can also be used (Gupta et al., 1991). The PAN/water system (1 part PAN to 3 parts water) forms a single-phase solution above 180°C and the solution phase-separates with solidification of the polymer on cooling to 130°C (Damodaran et al., 1990). Carbon fibers with satisfactory mechanical properties have been obtained by extruding at 140–190°C a homogeneous melt consisting essentially of (1) an acrylic polymer containing at least 85 wt.% of recurring acrylonitrile units, (2) approximately 3–20 wt.% of C1 to C2 nitroalkane based upon the polymer, (3) approximately 0–13 wt.% of C1 to C4 monohydroxy alkanol based upon the polymer, and (4) approximately 12–28 wt.% of water based upon the polymer (Daumit et al., 1990a, 1988). However, PAN fibers made by melt-assisted spinning contain more internal voids and surface defects than those made by wet or dry spinning (Gupta et al., 1991). On the other hand, PAN fibers made by melt-assisted spinning can have a larger variety of cross-sectional shapes: trilobal, multilobal, for example. Such shapes provide a greater surface area, which enhances fiber-matrix bonding in composites. Since

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  39

melt-assisted spinning of PAN does not require potentially harmful solvents, solvent recovery is not needed and wastewater treatment is not critical, in contrast to the harmful solvents required for dry spinning, wet spinning, and dry-jet wet spinning. Due to this, melt-assisted spinning is technologically attractive (Daumit et al., 1990b). However, its use in carbon fiber production is unfortunately not being pursued because of the enormous cost involved in performing the US military qualification tests required for any new carbon fiber product to be used for military purposes. Dry spinning, wet spinning, and dry-jet wet spinning are all referred to as solution spinning, as they all use a polymer solution, which is known as dope. The dope is not 100% liquid; its solid content (7–30 wt.%) is used to adjust the viscosity of the dope. Dopes for dry spinning generally have a higher solid content than those for wet spinning. The dope is stored at 25°C for about 24 h before the start of spinning in order to remove the air bubbles from the viscous dope. This storage of the dope is known as ripening. A higher solid content tends to reduce the void content in the fibers (Gupta et al., 1991). Wet spinning is the standard method for spinning PAN fibers. The spinning solution consists typically of 10–25% of the polymer in a solvent, which can be a mixture of dimethyl formamide and water, a mixture of dimethyl sulfoxide and water, or others. The molecular weight of PAN is in the range 70,000–200,000 and is chosen to yield a solution viscosity that provides a compromise between fiber drawability and final fiber properties. A coherent spinline is formed by phase separation in a suitable coagulating medium, which contains a mixture of a solvent (the same as used for the preparation of dope) and a nonsolvent (water most commonly). The higher the concentration of the nonsolvent, the higher the coagulation rate. The higher the temperature of the coagulation bath, the faster the coagulation. A lower coagulation rate is preferred because a higher coagulation rate causes surface irregularities, greater pore density, and the formation of a skin-core structure. The residence time in the bath is around 10 s. By using a low concentration of the nonsolvent and a low temperature, PAN fibers in a gel state (i.e., the state prior to coagulation of the extruded dope) can be obtained. The molecular chains in the gel can be quite easily oriented upon stretching because the trapped solvent decreases the cohesive forces among the nitrile groups of the polymer chains. To provide sufficient time to stretch the gel fiber (Gupta et al., 1991), coagulation is slowed down by allowing the gel fiber to pass through several baths containing varying compositions of the coagulation mixture. The coagulated fibers are called protofibers. They are stretched about 2.5 times in the coagulation bath. After washing, a further stretch of about 14 times in steam at 100°C aligns the molecular chains along the fiber axis (Donnet and Bansal, 1990). The greater the stretching temperature, the greater the draw ratio that can be attained. Similar stretching is applied to PAN fibers fabricated by dry spinning after evaporation of the solvent. Dry-jet wet spinning is replacing wet spinning because it yields fibers of better mechanical properties and controlled noncircular cross section. Moreover, the spinning speed is higher and the dope can be spun at a higher temperature, so that dopes of higher solid contents can be used. PAN fibers made by dry-jet wet spinning have superior mechanical properties to those made by dry spinning (Gupta et al., 1991).

40  Carbon Composites

A tow of a large number of filaments (∼50,000 or more) can be produced by wet spinning but not by dry or dry-jet wet spinning. However, fibers of controlled noncircular cross sections can be obtained by dry and dry-jet wet spinning, whereas the cross-sectional shape of fibers made by wet spinning depends on the collapse during coagulation. A lower polymer concentration or a lower temperature in the spinning solution leads to more collapse of the coagulating fiber and more away-from-round shape (even though the spinneret orifices are round) (Thorne, 1985). The greater surface area, resulting from the noncircular cross section, provides better heat flux during stabilization and carbonization; this reduces chain scission and weight loss to produce superior tensile strength and modulus in the resulting carbon fibers (Gupta et al., 1991). The drawability of a homopolymer (100% PAN) is limited because of the hydrogen bonds in the structure. Therefore, 5–10 mol.% of a comonomer is typically added. The comonomer is a more bulky acrylic monomer, which diminishes the crystallinity of the PAN structure, thereby acting as an internal plasticizer and improving the drawability. Hence, commercial PAN fibers are copolymers. A second comonomer is often added to initiate ladder-polymer formation (cyclization reaction) during subsequent stabilization of the PAN fibers. It is an acidic comonomer, such as acrylic acid and itaconic acid at concentration levels of about 1 mol.% (­ Damodaran et al., 1990). Among the comonomers, itaconic acid is particularly effective in helping ­cyclization because its two carboxylic groups increase the possibility of interaction with the nitrile group, in spite of the dipole–dipole repulsion between the carboxylic and nitrile groups (Gupta et al., 1991). A third comonomer with basic or acidic pendant groups may be added to make dyeing easier and more controllable. For example, vinyl pyridine is used for acid dyes, and sulfonic vinyl benzene and acrylic acids are used for basic dyes. The amount used is about 0.4–1.0 mol.% (Watt, 1985). General requirements of the polymer are the following (Gupta et al., 1991): • high molecular weight (∼105), • a molecular weight distribution corresponding to a polydispersity ratio of 2–3 Mw/Mn, • minimum molecular defects. General requirements of the precursor fibers are the following (Gupta et al., 1991): • a diameter of 10–12 µm, • high strength and modulus, • a broad exothermic peak due to nitrile group oligomerization during heating and it should start at a low temperature, • a high carbon yield (>50%). A small diameter of the precursor fiber is desirable for dissipating heat during conversion of the precursor fiber to a carbon fiber, since the heat evolved during the exothermic oligomerization reaction may lead to a low carbon yield. For controlling the heat flux, the rate and initiation temperature of the exothermic reaction should be lowered (Gupta

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  41

et al., 1991). The use of a microporous precursor fiber (as obtained by heating with water at 100°C or higher) also helps the conversion to a carbon fiber (Kimmel et al., 1975). The spun PAN fibers typically have a diameter of 11–19 µm, a tensile modulus of 8 GPa, and a tensile strength of 0.5 GPa (Damodaran et al., 1990). The ratio of the modulus of the carbon fiber to that of the precursor fiber is about 20 (Gupta et al., 1991). The higher the draw ratio, the greater the modulus and strength. The tensile stress–strain curve shows an initial elastic region, which could be due to the resistance of the CN─H bonds, followed by a regime of plastic flow of increasing resistance to stress until fracture occurs at about 30% elongation (Watt, 1985). Surface finish oil is applied to the spun PAN fibers to assist in handling. The oils are usually volatile above 130°C, so they are removed during subsequent stabilization of the PAN fibers (Thorne, 1985). Other than silicone oil, fatty acid derivatives, and guar gum can be used (Gupta et al., 1991). The conversion of a PAN fiber to a carbon fiber involves stabilization and carbonization. To further increase the modulus, graphitization can be carried out after carbonization. After carbonization (and optionally graphitization), the fibers are given a surface treatment. For example, plasma treatment can strengthen the bond between the fibers and a polymer matrix (Park et al., 2012; Shelestova et al., 2011). Another type of surface treatment involves anodic oxidation, with the carbon fibers being the anode of an electrochemical cell. To produce continuous carbon fibers these steps are performed in a continuous sequence along a production line. A variation of the anodic oxidation involves electrochemical impulse. The treatment involves alternating 5-min anode (carbon fibers) charging and 20-min cathode (platinum) charging, with a total treatment time of 5 h. By using sulfuric acid (1 M H2SO4) as the electrolyte, the treatment of a PAN-based carbon fiber increases the surface oxygen content from 17.0 to 24.7 atm.%, decreases the surface carbon content from 82.1 to 72.2 atm.%, increases the surface nitrogen content from 0.9 to 3.1 atm.%, increases the surface O/C atomic ratio from 0.21 to 0.34, increases the interplanar spacing d002 from 3.585 to 3.691 Å, and decreases the c-axis crystallite size Lc from 16.7 to 16.4 Å (Ma et al., 2013b). In the carbon fiber fabrication process, PAN fibers in the form of tows are brought off bobbins into a collimated array to pass through the first stage, which is stabilization. Stabilization involves oxidation in air at 180–300°C (preferably below 270°C) under controlled tension and speed. The tension is applied to prevent shrinkage or even cause elongation of the fiber; PAN fibers, when fully relaxed by heating, shrink by about 25% due to the formation of nitrile conjugation cross-links between the polymer chains (Watt, 1985). ­During stabilization, gases (NH3, HCN, etc.) are evolved, so the temperature is controlled by heated air circulation. The stabilization serves to increase the carbon yield during subsequent c­ arbonization at 300–1500°C. It converts the thermoplastic PAN into a nonplastic cyclic compound that can withstand the high temperatures during carbonization. The cyclized structure is called a ladder polymer. The cyclization initiates through a radical mechanism in the case of the PAN homopolymer and an ionic mechanism in the presence of acid comonomers

42  Carbon Composites

(Gupta et al., 1991). It occurs during heating under tension in an inert or oxidizing atmosphere. An oxidizing atmosphere is used because it results in a higher rate of cyclization, a higher carbon yield after subsequent carbonization, and improved mechanical properties of the carbon fibers. Hence, the process is called thermo-oxidative stabilization. In ­addition to cyclization, stabilization results in dehydrogenation and 3D cross-linking of the parallel molecule chains by oxygen bonds; the cross-links keep the chains straight and parallel to the fiber axis, even after the release of tension poststabilization. However, the poststabilization cross-linking is not extensive as shown by the low secondary modulus, indicative of easy plastic flow. Oxygen acts in two opposite ways during stabilization. On the one hand it initiates the formation of activated centers for cyclization, while on the other hand it retards the reactions by increasing the activation energy. In spite of this, oxygen is desirable because it results in the formation of some oxygen-containing groups (such as ─OH, C═O, ─COOH) in the backbone of a ladder polymer. These groups subsequently help in fusion of the ­ladder chains during carbonization (Gupta et al., 1991). Due to the cyclization, the fiber density increases along with the oxygen content during stabilization (Fitzer and Frohs, 1990). An oxygen content of 8–12 wt.% is present in fully stabilized fibers (Fitzer and Frohs, 1990). In the stabilization reactions of cyclization, dehydrogenation, and oxidation ­(Gupta et al., 1991), numerous gaseous by-products evolve during the pyrolysis (Fitzer and Frohs, 1990). The process has been modeled to describe the temperature and composition in the fibers during stabilization (Dunham and Edie, 1992). The duration of the stabilization must be sufficient for oxidation to take place throughout the entire cross section of the fibers; otherwise the unoxidized cores give rise to ­central holes in the carbon fibers. The oxidation is diffusion controlled. Stabilization in air usually takes several hours. For a PAN copolymer containing about 2% methacrylic acid [H2C═C(CH3)COOH, Fig. 1.22], it takes only 25 min (Donnet and Bansal, 1990). An increase in the comonomer content reduces the time required for stabilization and ­improves the mechanical properties of the carbon fibers, but it does reduce their yield (Gupta et al., 1991). Prestabilization treatments are also used to reduce the stabilization time by decreasing the energy of activation of stabilization reactions. These treatments involve the impregnation of PAN precursor fibers with solutions of persulfate, cobalt salts, a combination of a salt of iron (11) and hydrogen peroxide, acids, guanidine carbonate, dibutylindimethoxide, and potassium permanganate (Gupta et al., 1991).

FIGURE 1.22  The molecular structure of methacrylic acid, H2C═C(CH3)COOH. http://www.sigmaaldrich.com/catalog/ product/aldrich/155721?lang=en®ion=US&gclid=Cj0KEQjw17i7BRC7toz5g5DM0tsBEiQAIt7nLGs9qK4-MelLBavdVCN4 fv6z3FLMcEX8LnOBfZ37j4EaAr4V8P8HAQ, public domain.

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  43

An acidic medium (such as sulfur dioxide and hydrogen chloride) during stabilization causes an increase in the reaction rate and a greater degree of stabilization. This is due to a shift of the equilibrium of the stabilization reactions in the forward direction. The removal of ammonia as a salt shifts the equilibrium to the forward direction (Gupta et al., 1991). A fiber is taken as being properly stabilized when the oxygen content is 8–12%. An oxygen content in excess of 12% results in deterioration of the fiber quality, whereas an oxygen content below 8% results in a low carbon yield (Donnet and Bansal, 1990). Due to the introduction of oxygenated groups and evolution of hydrogen cyanide, ammonia and other gases, the overall weight change during stabilization is small. However, at temperatures just above that of stabilization, significant weight loss can occur, especially if stabilization is not complete. The density of the fiber increases from 1.17 g/cm3 for the original PAN fiber to about 1.40 g/cm3 for the stabilized fiber. However, the exact density depends on the precursor and the tension condition (Gupta et al., 1991). Stabilization is accompanied by a change in the color of the fiber from white, through shades of yellow and reddish brown, ultimately to shiny black. An adequately stabilized fiber resists chemical attack by mineral acids and bases, and does not burn when held inside a flame (Damodaran et al., 1990). The shrinkage during stabilization consists of a physical contribution called entropy shrinkage, which is completed below 200°C, and a chemical contribution called reaction shrinkage, which starts at about 200°C. Entropy shrinkage is incipient contraction of PAN molecules that have been highly aligned during stretching prior to stabilization. Reaction shrinkage is due to the shortening of the PAN molecules during cyclization and oxygengroup formation. Higher copolymer content causes a larger chemical shrinkage. An increased heating rate (beyond 5°C/min) enhances chemical shrinkage, while the entropy shrinkage remains unchanged. Thus, the optimum heating rate should be less than 5°C/ min, i.e., l–3°C/min (Donnet and Bansal, 1990; Gupta et al., 1991). As the nitrile group gradually vanishes during stabilization, there is a transient ability for the polymer chains to slide past each other; this results in elongation after the initial shrinkage. After stabilization, the fibers are carbonized or pyrolyzed by heating in an inert atmosphere (nitrogen) at 400–1500°C. Tension is not required during carbonization as the all carbon backbone of PAN remains largely intact after stabilization. In contrast, the rayon precursor has one oxygen atom in the backbone per monomer unit, so it undergoes considerable structural reorganization as the heteroatoms are lost during carbonization. During carbonization about 50% by weight of the fiber is lost as gases, such as water, ammonia, hydrogen cyanide, carbon monoxide, carbon dioxide, nitrogen, hydrogen, and possibly methane. The volume of gas evolved is 105 times the volume of the fibers (Thorne, 1985). Thus, an inert gas is used to dilute the toxic waste gas in the gas extract system, as well as to prevent ingress of atmospheric air. The treatment and disposal cost for the hydrogen cyanide by-product increases the production cost of PAN-based carbon fibers. The rate of heating in the early stages of carbonization is low (less than 5°C/min up to about 600°C) so that the release of volatiles is slow and does not cause pores or ­surface

44  Carbon Composites

irregularities in the fiber. At 600–1500°C, higher heating rates can be used because of the completion of the by-product evolution by 600°C, leaving only carbon (>92 wt.%) and nitrogen (∼6 wt.%). At 1000–1500°C, the residual nitrogen is progressively removed. The overall residence time for carbonization is of the order of an hour, with residence at temperatures above 1000°C of the order of minutes (Thorne, 1985). During carbonization, intermolecular cross-linking occurs through oxygen-containing groups or through dehydrogenation, and the cyclized sections coalesce by cross-linking to form a graphite-like structure in the lateral direction. The modulus starts to increase at 300°C (Watt, 1985). Carbonization increases the fiber density from 1.45 to 1.70 g/cm3 and decreases the fiber diameter from 10–15 µm to 6–9 µm (Thorne, 1985). An increase of the PAN carbonization temperature from 550 to 950°C (for 1 h in nitrogen) decreases the nitrogen content of the resulting carbon fiber from 18.8% to 10.5%, decreases the hydrogen content from 0.76% to 0.20%, increases with carbon content from 69.2% to 81.3%, decreases the electrical resistivity from 5 × 104 to 4 × 10−2 Ω·cm, and decreases the Raman peak intensity ratio (D/G) from 2.02 to 1.23 (Wei et al., 2011). Graphitization (optional) is carried out after carbonization by heating at 1500–3000°C in an inert atmosphere, which is nitrogen up to 2000°C and argon above 2000°C. Nitrogen cannot be used above 2000°C because of the reaction between nitrogen and carbon to form cyanogen, which is toxic. A low cooling rate after the heating is preferred (Gupta et al., 1991). During graphitization, very little gas is evolved, but the crystallite size is increased and preferred orientation is improved, so the fiber becomes more graphitic. The residence time is just minutes for graphitization. The high temperatures make graphitization an expensive step, hence it is often skipped. The long stabilization time required for PAN adds much to the cost of PAN-based carbon fibers. A polymer which does not require stabilization is poly(p-phenylene benzobisoxazole) (PBO) (Edie, 1990). The high cost of PAN makes it attractive to use lower-cost polymers for making carbon fibers. An example of a low-cost polymer is polyethylene (PE). Melt spun PE fibers are cross-linked with chlorosulfonic acid for stabilization then carbonized at 900°C (Postema et al., 1990). Carbon fibers with a tensile strength of 2.16 GPa, a modulus of 130 GPa, a high strain at break of 3%, and a diameter of 13 µm have been obtained from PE (Pennings et al., 1991). The choice of the polymer can affect the microstructure of the resulting carbon fiber. By using a linear stiff-chain polymer, namely poly(p-phenylene benzobisthiazole) (PBZT), carbon fibers with well-defined fibrils along the fiber direction were obtained (Jiang et al., 1991). Axially graded carbon fiber with the electrical resistivity varying periodically (e.g., sinusoidally) along the axis of the fiber is a form of functionally graded material. It can be made by periodic variation of the pyrolysis time as the polymer fiber is fed through a furnace for conversion to a carbon fiber (Hu et al., 2011). The applications for this type of fiber are functional rather than structural, since the mechanical properties are not competitive. The functional applications mainly concern electromagnetic radiation absorption and

Chapter 1 • Carbon Fibers, Nanofibers, and Nanotubes  45

electromagnetic shielding, due to the periodic variation allowing interaction with certain frequencies of the radiation.

1.2.5  Classification of Carbon Fibers Carbon fibers can be classified in various ways—in accordance with the mechanical ­properties (modulus and strength), the carbon precursor, or the final heat-treatment temperature (i.e., the temperature of the last heat-treatment step in the process of fiber fabrication) (Hegde et al., 2004). In accordance with the tensile modulus and strength, they are classified as the following: 1. ultra-high-modulus (UHM) type, with modulus >450 GPa, 2. high-modulus (HM) type, with modulus ranging from 350 to 450 GPa, 3. intermediate-modulus (IM) type, with modulus ranging from 200 to 350 GPa, 4. low-modulus high-strength (HT) type, with modulus 3.0 GPa, and 5. superhigh strength (SHT) type, with strength >4.5 GPa. Fig. 1.23 shows various grades of PAN-based carbon fibers manufactured by Toray Industries, Inc. (Japan). The grade T1000 is particularly high in tensile strength, whereas the

FIGURE 1.23  Various grades of Toray PAN-based carbon fiber exhibiting various combinations of tensile strength and tensile modulus. The fiber designations are given by the manufacturer Toray Industries, Inc. http://www.pantherpools. com/superiorpools, public domain.

46  Carbon Composites

Table 1.11  Mechanical Properties of Standard-Modulus and High-Modulus PAN-Based Carbon Fibers in Comparison Property Tensile modulus Tensile strength Tensile strain Density Diameter CTE Specific heat Thermal conductivity Electrical resistivity Carbon content Na and K

Standard-Modulus High-Modulus Carbon High-Modulus Carbon Fiber With Carbon Fiber (Toray T300) Fiber (Toray M40) Strength Enhancement (Toray M35J) 230 GPa 3530 MPa 1.5% 1.76 g/cm3 7 µm −0.41 × 10−6 K−1 780 J/(kg·K) 10 W/(m·K) 1.7 × 10−3 Ω·cm 93 wt.% 99 wt.% 99 wt.% 90%. The Raman peak (the disordered carbon peak to the graphite peak) intensity ratio is  Mg > Zn > Ni > Sn > Ti. The ranking of the matrices in relation to the CTE is Zn > Al > Mg > Sn > Ni > Ti (Munir et al., 2015). This means that Ti and Ni are attractive for high harness, high modulus and low CTE, but they give low thermal conductivity; Al and Mg are attractive for high thermal conductivity, but they give low modulus and low hardness (Munir et al., 2015).

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Index A AAO. See Anodic aluminum oxide (AAO) Ablation resistance, 418 Abrasion resistance, 335 Absolute thermoelectric power, moisture, effect of, 352 Acetylacetone, molecular structure of, 552 Acetylene, decomposition reaction, 68 Acetylene flame blasting treatment, 413 Acid phosphate, 446 Acoustic emission (AE), 286, 433, 504 Acrylic dispersion, admixture uses, 343 Acrylic glass, 79 Acrylonitrile, polymerization, 37 Acrylonitrile butadiene copolymer, 231, 243 Acrylonitrile butadiene styrene (ABS), 204 Acryloyl chloride (C3H3ClO) molecular structure of, 531 Activated carbon fibers, 81 application of, 85–86 ceramic fibers, 86–87 incorporation of CNTs, 85 metal oxides, 84–85 metals, 84 pores on surface of, 81 processing, 82–84 structure, 81 Active brazing alloys, 558 Adhesive wear, 244 Admixture method, 533 AE. See Acoustic emission (AE) Air-carbon interfaces, 300 ALD. See Atomic layer deposition (ALD) Alite, 333 crystal structure, 335 Alkoxide anions, 540 Al-Shaheed Monument, 378 Alternating current (AC) electrical impedance, 277, 358  

Aluminosilicate coating, 496 joining of components, 496 laser beam machining (LBM), 497 preparing porous SiC from C/SiC, 497 Aluminum, 264, 304 Aluminum isopropoxide molecular structure of, 553 Aluminum-matrix composite, 544 aluminum carbide formation, 544 fabrication, 538–539 powder metallurgy, 544–545 squeeze casting/pressure casting, 546 friction and wear behavior, 549 mechanical properties of, 547 ductility values, 547 electrical resistivity, 548 Poisson’s ratio values, 547 tensile strengths, 547 thermal conductivity, 548 radiation resistance, 549 thermal conductivity, 546 thermal expansion, 547 Aluminum-oxide-matrix composites, 517 Aluminum phyllosilicate, 461 Aluminum tri-sec-butoxide molecular structure, 385 Aluminum trisecutoxide, 424 American Airlines Flight 589 accident of, 193 3-(2-Aminoethylamino) propyltrimethoxysilane, 347 molecular structure, 347 3-Aminopropyl triethoxysilane (APTES), 114 c-Aminopropyltriethoxy silane molecular structure of, 57 Ammonium heptamolybdate, 459 Ammonium paramolybdate tetrahydrate, 459 Amorphous and semicrystalline polymers molecular arrangement, 166 Anatase, tetragonal crystal structure, 552

655

656 Index

Aniline, molecular structure, 53 Anisotropic pitch, 30 Anisotropy, 129, 264, 278 Anodic aluminum oxide (AAO), 102 Anodic oxidation, 41 Antiferroelectric coupling, 292, 293 Antiicing, 194, 382 antiicing fluid, 194 freezing point, 194 temperature variation during, resistance heating, 195 Antioxidant migration, 427 APTES. See 3-Aminopropyl triethoxysilane (APTES) Arall, 254 Armchair orientation, 65 Arrhenius plot, interlaminar interface log contact conductivity vs. inverse absolute temperature of crossply continuous carbon fiber epoxy-matrix composite, 186 Arylacetylene, 390 Atomic layer deposition (ALD), 101, 233 B Ballistic energy dissipation, 298 Basalt fiber, 252 Batch process, 70, 71 Belite, 333 crystal structure, 334 Bentonite, 380 Benzene, 33 Bismaleimide (BMI), 248 Bismalemide-matrix composite, 231 Bismuth oxide, 362 Bismuth telluride (Bi2Te3), 51, 314, 320, 325 Bisphenol, 163 Blast damage, 264 BMI. See Bismaleimide (BMI) BN. See Boron nitride (BN) Boehmite, 472 Bohr radius, 155 Bond with cement, carbon surface treatment effect, 344 Borate glazes, 421 Borazine, molecular structure, 507

Boric acid, 386 Boron-based inhibitors, 422 Boron carbide, 482 coating consisting of silicon carbide and, 495 hardest materials, 482 melting temperature, 482 Boron-doped carbon fibers, 386 Boron nitride (BN), 112 crystal structure of, 506 Boron trichloride, molecular structure, 436 Borosilicate glass, 384 Bottom surface resistance, 369 Breaking strain, 251 Brick-to-mortar bond strength, 383 Bromine, 313 Brown millerite, 333 Bruggeman’s effective media theories, 198 Buckminsterfullerenes, 77 Bulk diffusion, 403 Bulk viscous deformation, 238 1,3-Butadiene, molecular structure, 340 C Cadmium sulfide (CdS), 157 Cadmium telluride (CdTe), 154 CAGR. See Compounded annual growth rate (CAGR) Calendering process, 251 Capacitance, 277, 292, 293 measurement, 292 Capacitive effect, 258 Capacitor, 290, 292–294 Carbide-matrix composites, 482 boron carbide, 482 silicon carbide, 482 Carbon functional groups on, 24 phase diagram of, 4 structure of cell wall, 10 Carbonaceous gases fabrication of carbon nanofibers/nanotubes from, 68–77 batch process, 70, 71 catalytic method, 72 conversion of, 69

Index 657

coprecipitation method, 72 CVD process, 68, 69 decomposition reaction, 68 floating-catalyst process, 70 hydrogasification, 75 pyrolysis, 71 rate-limiting step, 75 Carbon black (CB), 257, 261, 288, 305, 320, 325 spreadability, 351 squishability, 351 vs.carbon fibers, 354 Carbon-carbon (C/C) composites applications, 465 aircraft brakes, 465 biomedical implants, 465 engine turbine blades, 465 heat pipes, 465 hip replacements, 465 reentry vehicles, 465 rocket motor nozzles, 465 with carbon nanofiber (CNF) incorporation, 456–458 by applying dispersion, 457 by catalytic growth of CNFs, 456 by CVI in presence of catalyst, 457 by dispersion of CNFs, 457 by electrophoretic deposition, 458 ceramic coating with hafnium carbide and silicon carbide, 415 silicon carbide, 412–413 silicon carbide and molybdenum silicide, 415 zirconium carbide, 413–414 zirconium carbide and silicon carbide, 414 ceramic incorporation with silicon carbide, 415–417 silicon carbide and zirconium boride, 419 silicon carbide and zirconium carbide, 418–419 silicon carbide or boron carbide, 417 silicon dioxide, 420–421 titanium carbide, 417 zirconium carbide, 418 zirconium carbide and titanium carbide, 419

zirconium carbide and zirconium silicide, 418 with CNT incorporation, 453–456 on carbon fiber preform, 453 by CVI, 454 by dispersion in carbon precursor resin, 455–456 by electrophoretic deposition on carbon fiber preform, 455 companies, 466 disadvantage, 387 electrical conductivity, 443 electromechanical behavior, 443–445 damage sensing by electrical resistance measurement, 443–445 strain sensing by electrical resistance measurement, 445 fabrication, 388–389 flexural stress-strain curves, 461 with grown silicon nitride nanofibers, 453 hybrid, 447–464 carbon and ceramic hybrid, 447–452 C/C-SiC with SiC nanofibers, 458 with filler incorporation, 460–464 with carbon black, 460 with fumed alumina, 462–464 with organobentonite, 461–462 with infiltrated metal, 459–460 copper as metal infiltrant, 459 copper-tin-lead alloy as metal infiltrant, 459 copper-titanium alloy as metal infiltrant, 460 interfacial layer, use of, 459 zirconium-titanium alloy as metal infiltrant, 460 with two types of reinforcement, 452–458 with incorporation of SiC fibers and CNTs, 458 joining methods, 445–446 brazing, 445, 446 glass bonding, 445 inorganic phosphate adhesive bonding, 445 mechanical joining, 445 organic precursor bonding, 445

658 Index

Carbon-carbon (C/C) composites (cont.) by SiC nanofiber incorporation, 446 solid-state diffusion bonding, 445 by TiB whisker incorporation, 446 made with carbon fiber thermal conductivity, 442 magnetoresistance, 443 mechanical behavior, 429–437 dynamic mechanical properties, 433–434 fatigue behavior, 433 viscoelastic behavior, 433–434 high-temperature mechanical properties, 437 improving wear resistance of C/C by coating C/C, 437 improving wear resistance of C/C by incorporating ceramics to matrix, 434–436 boron nitride incorporation, 436 silicon carbide and titanium silicon carbide incorporation, 436 silicon carbide incorporation, 434–436 static mechanical properties, 430–433 carbon fiber surface treatment, effect of, 430 carbon matrix precursor, effect of, 431 crystallographic texture of the carbon matrix, effect of, 431 damage mechanisms, 432–433 heat treatment, effect of, 431–432 interfacial shear strength of the fibermatrix interface, 430 residual stress, 430 SiC coating, effect of, 432 strength and elastic modulus, 430 wear resistance, 434 mullite coating by chemical vapor deposition, 426 by electrophoretic deposition of mullite sol, 424–425 by pack cementation, 425–426 oxidation protection, 410–411 above 1700˚C, 427–429 chromium carbide coating, 427 four ceramic layers coating, 428 hafnium carbide incorporation, 429

hafnium carbide, silicon carbide, and hafnium silicide coating, 428 hafnium diboride incorporation, 429 silicon carbide coating, 427 zirconium oxide and silica coating, 428 below 1700˚C, 411–427 alumina-based ceramic coating, 426 antioxidant coating, 427 ceramic coatings, 412–415 ceramic incorporation, 415–421 dense HfC nanowire-toughened outer coating on SiC-coated C/C, 422 fumed alumina particle as filler in C/C, addition of, 423 glass sealants, 421 graphite coatings, 415 high-temperature silicon-based alloy coating, 426 inhibitors, 422 mullite coating, 423–426 other methods, 427 phosphoric acid impregnation, 422 thermal conductivity, 439–442 carbon fiber type, effect of, 441–442 carbon matrix precursor, effect of, 441 carbon nanotube array composite, 442 heat treatment, effect of, 439–440 low-temperature behavior, 442 thermal conductivity anisotropy, 439 thermal expansion, 437–439 carbon matrix precursor, effect of, 439 heat treatment, effect of, 438 thermal expansion anisotropy, 437–438 Carbon dioxide phase diagram, 395 Carbon fiber, 14, 50, 88, 257, 278, 280, 288, 291, 293, 294 alkylsilane-treated, 346, 347 assemblies, 88 basic concepts of composites, 124 coating, 132 conductivity enhancement, 125 configurations, 124 fabrication, 125 method, effects of, 130 fiber length effect, 128

Index 659

fiber-matrix bond effect, 126 fiber-matrix bonding, 124 hybrid, 132 joining, 132 mechanical properties, 126 mechanical testing methodology, 133 recycling, 133 secondary reinforcement effect, 128 short carbon fiber composites, 129 with various matrices, 126 volume fraction effect, 128 carbon foams, 109 carbons deposition, 104 ceramic coating, 50 chemical stability of, 478 choice of, 391 sizing material, 49 classification of, 45–51 coating with, 537 carbons, 112 ceramic coatings, 538 chemical vapor deposition (CVD), 538–539 liquid metal transfer agent, 538 solution coating method, 539–542 metal coatings, 537 mullite, 509 silicon carbide, 508 silicon nitride, 508 wettability and interfacial reaction, 537 with ZnO, 300 coefficient of thermal expansion (CTE), 16 cross-sectional shapes, 48 degree of graphitization, 25 diameter of, 14 doped carbons, 109 effect of, graphitization heat-treatment on, 47 electrical conductivity, 14 with embedded fillers, 110 for EMI shielding, 20 fabrication, 26 from pitch, 28–34 from polyacrylonitrile, 34–44 schematic illustration of, 48 felts, 90

with filled core channel, 103 films, 101 functional properties of, 51–52 growth on ceramic, 107 growth on metals, 109 materials CTE Values of, 21 electrical resistivity, 20 specific strength, 19 tensile strength, 20 thermal conductivity, 21 mats, 93 for electrical conductivity, 94 for electrochemical applications, 97 fabrication, 94 for friction materials, 95 mechanical properties, 95 for thermoelectricity, 95 mechanical properties of, 18 nonstructural applications, 145 polymer fibers with carbon filling, 111 preferred orientation, 23 bent carbon layer, 22 properties of, 14, 24 pyrolytic carbon deposition, 107 quality of, 15 recycling, 250 resistance (Joule) heating, 16 SEM photographs of, 48 specific strength, comparison, 19 structural applications, 135 structural parameters of, 25 structure of, 21, 410 atomic layers, 21 tensile modulus, 16 thermal conductivity, 14, 20 types of, 15 vertically aligned carbons, 101 volume fraction, 358 vs. competing materials, 19 vs. glass fiber and Kevlar fiber and carbon steel, 15 yarns, 98 fabrication, 98 mechanical behavior, 99 for microelectrodes, 100

660 Index

Carbon fiber cement piezoresistive strain sensor, role as, 369 strain-sensing ability, 366 Carbon fiber composite, 229, 264, 281–283, 303 Carbon fiber nitride-matrix composites, 507 Carbon fiber polymer-matrix composite, 257, 264, 436 electrical resistance measurement methodology, 175–176 current spreading, 176 four-probe method vs. two-probe method, 175 fabrication of, 205–215 fiber prepreg method, 213–215 filament winding process, 211 general concepts, 205–206 molding methods, 206–211 robotic method, 215 glass transition and melting, effect of, 170–173 thermoplastic polymers, properties of, 169 Carbon fiber preform architecture, 469 chemical vapor infiltration (CVI), 469 effect on mechanical properties, 469 yarn size, 469 Carbon fiber-reinforced cement, 337 piezoresistivity model for explaining, 371 wet mix method, 337 Carbon fiber reinforced polymers (CFRP), 136 Carbon fiber reinforced thermoset polymers upcycling, 250 Carbon fiber SiC-matrix composites (C/SiC), 483 brake on Porsche Carrera, 484 corrosion resistance, 503 electrical conductivity, 500 EMI shielding, 500 emissivity of, surface material, 503 fabrication, 486 annealing of, 493 chemical vapor infiltration, 491–492 coating of composite, 493–496 mixture sintering, 491 polymer impregnation, 486–488 polymer pyrolysis, 492 pyrolysis, 486–488 reactive liquid infiltration, 489–490

silica-sucrose impregnation and pyrolysis, 488–489 slurry infiltration, 490–491 mechanical behavior, 497 ballistic performance, 500 CVI infiltration time, 498 effect of, graphite addition, 499 fatigue loading, effect, 499 loading rate effect, 500 microstructure, 497 modeling of, 500 through-thickness stitching yarn spacing, 498 wear behavior, 500 yarn size, 499 nondestructive evaluation, 504 oxidation resistance, 502–503 thermal conductivity, 501–502 thermal expansion, 501 Carbon fiber silica fume cement paste electrical conduction behavior heating effect, 360 Carbon filaments. See Carbon nanofibers (CNFs) Carbon filler, 258, 336 Carbon foam, 109, 392 Carbon ion irradiation, 98 Carbonization, 17, 43, 389 Carbonization-impregnation cycles, 394 Carbon-matrix composite, 126 Carbon matrix precursor, 389–391, 397, 407 Carbon matrix, structure of, 408–410 degree of graphitization, 409–410 texture, 409 Carbon nanofiber, 88 on cordierite, 108 Carbon nanofibers (CNFs), 52, 336, 340, 345, 346 arrangements of, carbon layers in, 61 coiled, 62 composites, 197–201 electrical conductivity, 198 electrical resistivity, 198 nickel-coated CNF, 199 tunneling, 198 definition, 54 experimental set-up for, electroplating of nickel on, 62

Index 661

fabrication, 68 from carbonaceous gases, 68–77 from electrospun polymer nanofibers, 79 by spinning, carbon-precursor polymer and pore-forming polymer, 79 by template, 80 fishbone structure, 58 functionalization of, 56 graphitization of, 80 growth on carbon fiber materials, 57 microscope photographs of, 54 nickel-coated, 62 oxidation resistance of, 65 platelet type structure, 61 properties of, 66–68 structural applications of, 56 structure of, 54 x-ray diffraction patterns of, 60 Carbon nanoparticles, 304 Carbon nanospheres, 363 Carbon nanotubes (CNTs), 52, 135, 336, 340 alignment, 296 on alumina, 107 applications in, 157 aerospace, 158 automotive, 158 biomedicine, 158 electronics, 157 energy, 157 filtration, 158 healthcare, 158 photonics, 157 polymer composites, 158 sensors, 159 carbon deposition, 106 and cellulose dope, 269 composites, 201, 464–465, 504, 521 aligned CNT sheet, 505 carbon fibers with deposited CNTs, 504 compact composites, 465 comparison, with various metal matrices, 562 growth of, 511 horizontally aligned, 464–465 joining C/C and silicate with aligned CNTs, 465 vertically aligned, 464

vertically aligned CNT array, 504 yarn composites, 465 definition, 54 fabrication, 68 from carbonaceous gases, 68–77 from electrospun polymer nanofibers, 79 functionalization of, 56 graphene ratio, 260 growth on carbon fiber materials, 57 interfaces, 266 market size, 159 microscope photographs of, 54 PE interfacial tension, 258 properties of, 66–68 on silica fibers, 107 structural applications of, 56 structure of, 54 Carbon nanotube silicon nitride-matrix composites ablation resistance, 512 CNT/CNF array composites, 514 CNT composites, 513 CNT dispersion, 513 electrical behavior, 514 electrical conductivity, 515 fabrication of, 511 friction and wear behavior, 515 mechanical behavior, 515 oxidation, 512 sintering of CNTs, and silicon nitride, 514 thermal and mechanical behavior, 514 Carbon precursor, 26, 400, 403 concentration, 404 Carbon preforms, 392–394 carbon fiber preform density, effect of, 393 carbon fiber preform fabrication, 392–393 nonwoven carbon fiber preform, 392 short carbon fiber reinforced carbon foam perform, 392 woven carbon fiber fabric preforms, 392 degree of carbon fiber orientation, effect of, 393 exfoliated graphite, 394 with nanofiber/nanotube incorporation, 393 pyrolytic carbon interfacial layer thickness, effect of, 393

662 Index

Carbon-reinforced aluminosilicates, 383–386 aluminoborosilicate, 384 aluminosilicate, 383–384 barium aluminosilicate, 385 lithium aluminosilicate, 386 Carbons deposition, 104 Carborane compound structure of, 390 Carbothermic reduction, 428 Carbothermic reduction reaction, 416 Carboxyl-terminated butadiene-acrylonitrile (CTBN), 252 Carboxymethylcellulose molecular structure, 337 Carboxy-terminated nitrile butadienes (CTBNs), 226 Carrier gas, 399 Casing, 380 Catalytic chemical vapor deposition (CCVD), 69 Cathodic protection, 382 CBT. See Cyclic butylene terephthalate (CBT) C/C composites. See Carbon-carbon (C/C) composite fractional weights during heating, 424 CCVD. See Catalytic chemical vapor deposition CdS. See Cadmium sulfide (CdS) CdTe. See Cadmium telluride (CdTe) Cellulose, 259 molecular structure of, 53 Cement-based materials electrical resistivity short carbon fiber volume fraction, effect of, 349 electric polarization, 357 Cement grout, 380 Cement-matrix composites applications, 378–383 antistatic ability, 381 cathodic protection, 382 damage, self-sensing of, 379–381 deicing, antiicing, and heating, 382 EMI shielding, 381 energy conservation of buildings, 379 lateral guidance, 381 masonry, 383

strain/stress, self-sensing of, 379–381 structural applications, 378–379 temperature, self-sensing of, 379–381 traffic monitoring, 381 weighing-in-motion (WIM), 381 electrical behavior, 352–358 cement-based p-n junction, 353 controlled resistivity materials, 354 electrical conduction by ions and electrons, 352 electric polarization, 355–358 electromagnetic interference shielding, 354–355 new and old concretes, joining of, 358 various conductive admixtures in comparison, 353 electrical percolation, 348–352 carbon black and short carbon fiber, by using, 351 carbon nanotubes and short carbon fiber, by using, 352 double percolation, 350–351 single percolation, 348 triple percolation, 351 electrochemical behavior, 364–376 electrical resistivity, effect of strain, 364–376 damage sensing, 372–376 under flexure, 369–371 strain-sensing coating, 371 under uniaxial compression or tension, 364–369 relative dielectric constant, effect of strain, 376 mechanical behavior, 362–364 dynamic mechanical properties, 364 static mechanical properties, 362–363 thermal behavior, 358–362 electrical resistivity, effect of temperature, 359 specific heat, 359 thermal conductivity, 358 thermoelectric behavior, 361–362 Cement matrix damage, 374 Cement mortar conductivity effect of short carbon fiber volume fraction, 351

Index 663

Cement paste absolute thermoelectric power, 361 flexural toughness carbon fiber volume fraction, effect of, 339 progressively increasing amplitude tensile strain, effect of, 366 relative dielectric constant compressive stress, effect of, 377 thermoelectric power carbon fiber content, effect of, 361 with and without short carbon fiber electrical resistivity, 341 Cement paste containing short ozone-treated carbon fiber electrical resistance effect of cyclic strain at fixed amplitude, 365 effect of dynamic compressive loading, 367 electrical resistivity effects of strain and damage, 368 resistance flexure, effect of, 370 Cement pastes containing conductive admixture electrical resistivity, 353 electromagnetic interference (EMI) shielding effectiveness, 353 Cement pastes containing short carbon fiber (CF) with/without ozone treatment mechanical properties, 346 tensile properties, 345 Cement science, 333–336 admixtures, 334–335 carbon fiber, 334–335 hydraulic cement, constituents of, 333–334 pozzolans, 336 Cement slurry, 338 Ceramic coatings, 538 Ceramic fibers, 86–87 Ceramic matrix, 476 ceramic phases, 476 high-temperature stability, 476 polymorphic transformation, 477 Ceramic-matrix composites (CMCs) in ballistic armored vests, 468

fabrication of, 469 carbon fiber preform architecture, 469 chemical vapor infiltration (CVI), 471–472 interfacial layer on, carbon fibers, 470 lattice composite, 476 liquid metal infiltration, 475 metal reaction with gas, 475 polymer impregnation, 471 pyrolysis, 471 reactive gas infiltration, 475 reactive liquid infiltration, 473–475 sintering of solids, 475 slurry infiltration (SI), 472–473 fiber-matrix interface, 478 matrix of, 482 overview, 467–469 CFRP. See Carbon fiber reinforced polymers (CFRP) Charge-dissipating coatings, 354 Charpy impact energy, 231 Charpy impact test, 231, 437 Chemical activation method, 83 Chemical liquid-vapor deposition (CLVD), 405, 472 Chemical supercritical fluid infiltration, 395 Chemical vapor deposition (CVD), 225, 411, 538–539 Chemical vapor infiltration (CVI), 92, 397–398, 471–472 carbon coating, 471 chemical liquid-vapor deposition (CLVD), 472 methodology, 398–405 carbon fiber preforms, 401–404 CVI process modeling, 403–404 infiltration pressure, effect of, 402 infiltration temperature, effect of, 403 residence time, effect of, 403 isothermal isobaric CVI, 398 limitations, 401 pressure gradient method, 401 special techniques, 404–405 carbon black slurry impregnation, 404 film boiling CVI, 405 microwave pyrolysis, 405 preform shaping, 405

664 Index

Chemical vapor infiltration (CVI) (cont.) temperature gradient, 398–401 induction heating, provided by, 399 microwave heating, provided by, 400–401 resistive heating of a graphite mat sandwiched by two carbon performs, provided by, 400 resistive heating of graphite rod with carbon preform around it, provided by, 399 resistive heating of the carbon preform, provided by, 400 two graphite heaters, provided by, 400 methyltrichlorosilane (MTS, CH3SiC13), 471 Monte Carlo method, 472 pressure gradient method, 471 rate of deposition, 471 thermal gradient method, 471 Chimneys, 336 Chitosan, 332 CIGS. See Copper indium gallium selenide (CIGS) Circular fibers, 391 Citric acid, molecular structure of, 73 Classical lamination theory, 220, 247 CLVD. See Chemical liquid-vapor deposition (CLVD) CMCs. See Ceramic-matrix composites CMT. See X-ray computerized microtomography (CMT) CNFs. See Carbon nanofibers (CNF) CNT. See Carbon nanotubes (CNT) CNTs. See Carbon nanotubes Coated carbons, 112 Coated-filler method, 533 Coating, 132 Cobalt acetate tetrahydrate structure of, 511 Coefficient of friction (COF), 435 Coefficient of thermal expansion (CTE), 174, 221, 387, 532 COF. See Coefficient of friction (COF) Complex permittivity, 289 Composite fabrication, 88 Composite modulus, 219

Composite panels, 264 Composites, 257, 259, 293 with carbon black, 261 with CNT or CNF, 259 with continuous carbon fibers, 262 with short carbon fibers, 257 Composite skeletons, 197 Compounded annual growth rate (CAGR), 160 Compression molding, 207 Compression surface resistance, 287 Compressive deformation, 246 Concrete, 333, 335, 351, 358, 362, 371, 378, 382 fine aggregate particles, fitting of, 334 Conduction behavior, 294 Conductive, 259 Conductive filler, 288 Conductive materials, 291 Conductive particles, 279 Conductive reinforcement, 279 Conductivity, 258, 296, 307 enhancement, 125 fiber volume fraction, effect of, 348 matrix composition, effect of, 348 Conductivity ratio, 341 Conformability, 325 Contact angle, 560 Contact resistance, 278 Continuous carbon fiber composites, 509, 521 Continuous carbon fiber epoxy-matrix composite contact electrical resistivity variation with time and of relative humidity, 184 crossply interlaminar interface contact electrical resistivity variation with temperature, 185 contact electrical resistivity variation with time and stress with time during compressive stress cycling, 192 cross-section optical microscope photographs, 183 dynamic flexural properties, 241 interlaminar interface impact damage sensor, 191 mechanical properties, 221

Index 665

static flexural strength, modulus, and ductility lay-up configuration and curing pressure, effects of, 224 Continuous carbon fiber epoxy-matrix composite lamina curing pressure, effect of, 181 Continuous carbon fiber epoxy-matrix composite laminate electrical contact cross-section optical microscope photograph, 177 Continuous carbon fiber polymer-matrix composite, 197, 221–230, 273, 289 contact electrical resistivity, 246 curing pressure and lay-up configuration, effect of, 224–225 filler addition, effect of, 225–229 polymeric interlayer, effect of, 229 processing, effect of, 229–230 unidirectional composite longitudinal properties vs. transverse properties, 223 vs. woven fabric composite, 221–222 Continuous carbon fibers thermal conductivity of, 27 thermoplastic-matrix composite crossply interlaminar interface contact electrical resistivity, 190 Continuous carbon fiber thermoplastic-matrix composite crossply interlaminar interface variation of the contact electrical resistivity with the temperature, 187 interlaminar interface contact electrical resistivity measurement four-probe method, 188 Continuous carbon fiber thermoplastic polymer-matrix composite glass transition and melting temperature, effect of, 171 Continuous fibers, 88 composite, 281 laminates, 178–181 fiber volume fraction determination, 181 forms, 178–179 structural parameters curing pressure, effect of, 179

polymer-matrix composite, 202 fabrication of, 205 curing of resin, 205 molding methods, 206–211 resistance heating, 205 fiber prepreg method, 213–215 filament winding process, 211, 212 polymerization, 205 robotic method, 215, 216 skeletal composites, 195–197 Controlled resistivity materials, 354 controlled electrical conduction, use in, 354 lightning protection, use in, 354 static charge dissipation, use in, 354 Copper-based powder metallurgy materials, 415 Copper indium gallium selenide (CIGS), 154 Copper-matrix composites, 554 coatings on, carbon fibers, 555 electrical conductivity, 556 fabrication, 555 friction, 557 thermal conductivity, 555–556 thermal expansion, 557 wear behavior, 557 Corundum (α-Al2O3) 3D model of, 517 Countercations, 383 Crack-bridging fibers, 371 Crack-pinning process, 254 Creep resistance, 437 Cross-bundle cracking, 410 Crossply continuous carbon fiber epoxy-matrix composites dynamic flexural properties effect of filler, 241 Crystalline carbon fibers intercalation of, 355 Crystallinity, degree of, 3 CTBN. See Carboxyl-terminated butadiene-acrylonitrile (CTBN) CTBNs. See Carboxy-terminated nitrile butadienes (CTBNs) CTE. See Coefficient of thermal expansion (CTE)

666 Index

Cured cement, 334 Curing age with short carbon fiber, 342 without carbon fiber, 342 CVD. See Chemical vapor deposition (CVD) CVI. See Chemical vapor infiltration (CVI) Cyanate ester resin, 420 Cyclic butylene terephthalate (CBT), 235 Cyclic compressive loading fractional resistance change, 373 Cyclic loading, 374 Cyclic olefin compound, 257 Cyclic tensile loading fractional resistance change, 375 Cytocompatibility, 253 D Damage-induced resistance, 374 Damage monitoring, 372 Daumas-Herold model, 8 Decoupling, 292 Defoamer, 338 Degradation, 272 Deicing, 194, 382 deicing fluid, 194 for operation and safety of aircraft, 194 Deicing and antiicing, 194 Delamination, 221, 281, 286, 288 Densification kinetics, 403 Diamond, 4 Diamond-like carbon (DLC), 437 Diatomite, 380 Dicalcium silicate, 333 Dichloroethylene, 84 Dichlorosilane (DCS, SiCl2H2) molecular structure of, 511 Dielectric capacitor, 290, 291 coating, 123 constant, 258, 292, 293, 296 loss factor, 289 properties, 295 Dielectric behavior, 289, 291 above 30 MHz, 296 continuous carbon fiber polymer-matrix composites, 297

polymer-matrix composites with discontinuous carbon fillers, 298 carbon nanofiber composites, 301 carbon nanotube composites, 302 short carbon fiber composites, 298–301 below 30 Hz, 291 continuous carbon fiber polymer-matrix composites, 291–293 polymer-matrix composites with discontinuous carbon fillers, 294–296 Differential scanning calorimetry (DSC), 170 thermogram, 170 Diffusion bonding method, 534 2,2′-dimethylbenzidine (DMBZ), 165 molecular structure, 166 Dirac point, 5 Direct current (DC) electrical resistance measurement, 272, 277 electrical resistivity, 257 resistance, 277 Direct methanol fuel cell (DMFC), 109 Discontinuous carbon fillers, 294 Distillation-precipitation-polymerization process, 235 Distortion, 286 Divinylbenzene, C10H10 molecular structure of, 488 DLC. See Diamond-like carbon (DLC) DMBZ. See 2,2′-dimethylbenzidine (DMBZ) DMFC. See Direct methanol fuel cell (DMFC) Dodecylbenzene, 545 structure of, 545 Doloma-matrix composites, 524 Dope, 39 Doped carbons, 109 Dormant anisotropic pitch, 31 Double cantilever beam test, 220 Double-walled CNT (DWCNT), 233 Drilling fluid, 379 Dry-jet wet spinning method, 38, 39 Dry spinning method, 38, 39 DSC. See Differential scanning calorimetry (DSC) DSSC. See Dye-sensitized solar cell (DSSC) Ductile fibers, 251 DWCNT. See Double-walled CNT (DWCNT)

Index 667

Dye-sensitized solar cell (DSSC), 155, 156 Dynamic flexural behavior of materials, 242 Dynamic strain amplitude, 239 Dynamic stress amplitude, 239 E ECVI. See Electrified preform heating chemical vapor infiltration (ECVI) Eddy current, 399 EG. See Exfoliated graphite Elastic modulus, 218 Elastomeric ethylene-octene copolymer (EOC), 332 Electrical conductivity, 161, 256, 264, 265, 296 of carbon fibers, 291 Electrical contact configurations for sensing without spatial resolution, 275 for sensing with spatial resolution, 277 resistivity, 343 Electrically conductive cement-based materials, 348 hydrogel materials, 260 Electrically dissimilar cement pastes, 353 Electrical neutrality, 383 Electrical resistance, 267, 278 apparent volume, electric field effect, 356 damage sensing, 443 measurement, 281 four-probe method, 355 four-probe scheme, extent of current spreading, 178 self-sensing, 278, 352, 379 method of, 274 Electrical resistance tomography (ERT), 379 Electrical resistivity, 259, 264, 265, 267, 269, 294, 341 effect of damage, 273 effect of temperature, 358 Electrical signal processing, 279 Electric permittivity, 289 Electric polarization, 258, 289 during electric field application, 356 Electrified preform heating chemical vapor infiltration (ECVI), 400 Electrochemical electrodes, 145

Electroless plating, 63 Electromagnetic radiation, 290, 297, 300 signal, 290 Electromagnetic behavior, 289, 291. See also Dielectric behavior Electromagnetic induction, 399 Electromagnetic interference (EMI), 145 shielding, 64, 290, 353 Electromechanical behavior, 267 Electron beam weld, 396 Electron hopping, 359 Electronic conduction, 352 Electron spectroscopic depth profiling, 408 Electron tunneling, 266 Electrophoretic deposition (EPD), 98, 424 Electroplasma process, 249 Electroplating, 63 Electrospinning, 79, 119 Electrospun polymer nanofibers electrospinning, 79 fabrication of carbon nanofibers, 79 Electrostatic precipitators, 336 Elementary surface reactions, 404 EMI. See Electromagnetic interference (EMI) Encircling, 417 Energy storage, 290 Entropy shrinkage, 43 Environmental barrier coating (EBC), 493 Enwrapping, 417 EPD. See Electrophoretic deposition (EPD) Epichlorohydrin, 163 Epoxide glycidol chemical structure, 164 Epoxy, 127 film, 288 matrix, 439 composite, 140, 221, 310 sizing, 228 Epoxy polymers, trade names, 163 Epoxy resin, silica nanoparticles incorporation, 227 Equivalent electrical circuit, 272 Erosion, 264 ERT. See Electrical resistance tomography (ERT)

668 Index

Ether general structure, 165 molecular structure, 340 Ethylene glycol dimethacrylate, molecular structure, 235 Ethylene glycol, molecular structure of, 194 Eutectic temperature, 416 Euythritol-matrix composite, 311 Exfoliated graphite (EG), 8 degree of compaction, 11 flexible graphite, 11 mechanical interlocking, 11 scanning electron microscope (SEM) image of, 9 viscous behavior of, 10 Extrusion molding process, 211 F Fabrication, 125 FAST, Field–assisted sintering technique Fatigue, 281 Fatigue loading in conjunction, 283 Fatigue resistance comparison of materials, 237 temperature, effect of, 238 Fatigue testing, 372 Feldspar, 383, 385 Felts, 90 Ferrocene decomposition of, 70 molecular structure of, 70 Ferrosilicon alloy, 336 Fiber alignment, 280 Fiber anisotropy, 306 Fiber-cement interface, contact electrical resistivity variations, 344 Fiber-fiber interface, 266, 305 Fiber fracture, 286 Fiber lay-up configuration, 180 Fiber length effect, 128 Fiber-matrix bond effect, 126 Fiber-matrix bonding, 124 Fiber-matrix covalent coupling, 347 Fiber-matrix debonding, 247 Fiber-matrix interface, 294, 297, 359, 406–408, 478 carbon fiber surface treatment, effect of, 406

carbon fiber type, effect of, 406 deflection of microcracks, 478 effect of interfacial layer on carbon fibers, 407–408 effect of, interfacial layer on fiber surface boron nitride interfacial layer, 480 carbon and silicon carbide interfacial layers, 481 carbon interfacial layer, 481 infiltrant viscosity, effect, 479 silicon carbide interfacial layer, 480 silicon nitride interfacial layer, 480 fiber-matrix bond strength, effect of, 406 fiber preoxidation effect, 481 graphitization, effect of, 407 infiltration pressure, effect of, 479 interfacial bonding, 434 interfacial microstructure, 482 microstructural characterization, 406–408 slippage, 347 thermal contraction, 482 Fiber-metal laminate (FML), 89, 254 Fiber packing geometry, 219 Fiber-polymer bonding effects, 173–175 composite fibers apparent modulus, 174 fraction of load carried, 173 residual stress, 174 fiber fragmentation test, 175 Fiber reinforced metal laminate (FRML), 89 Fibers, 278, 309 Fiber texture, 23 Fiber volume fraction, 219, 330 Fiber waviness, fiber-fiber contact, resulting in, 179 Field-assisted sintering technique (FAST), 545 Field emission (FE), 64 Field polarity switching effects, 356 Filament winding process, 211, 212 Flexible graphite, 11 Flexural shear cracking, 254 Flexural storage modulus, 346 Flexural testing, 133 Floating-catalyst process, 70 Fluorescence sensors, 145

Index 669

Fluorine-doped tin oxide (FTO), 155 Fly ash, 336 composition, 336 FML. See Fiber-metal laminate (FML) Foam thermal insulation, 378 Formaldehyde, molecular structure, 80 Four-layer coating scheme, 428 Four-probe method, 445 Fractography, 408 Fracture crack propagation, modes, 220 Free space, 292 Freeze-thaw durability, 362 Friction, types, 243 dry friction, 243 internal friction, 243 lubricated friction, 243 skin friction, 243 FRML. See Fiber reinforced metal laminate (FRML) FTO. See Fluorine-doped tin oxide (FTO) Fullerene, 4, 65 structure of, 5 Fumed alumina, SEM photograph, 423, 463 Functional behavior, 332 Furfural, molecular structure, 432 G Gage factor, 271, 288 Gas diffusion layer (GDL), 104, 113 Gas phase impregnation, 397 Gas residence time, 401 GC. See Green composite (GC) GDL. See Gas diffusion layer (GDL) Gel, 472 General effective media (GEM) model, 198 Generic epoxide, structure, 163 Gibbs free energy, 410 Glass ceramics, 386 coating, 494 Glass fiber, 15, 335 coefficient of thermal expansion (CTE), 16 composite, 203, 288 density of, 15 softening point of, 17 tensile modulus, 16 vs. carbon fiber, kevlar fiber and carbon steel, 15

Glass-forming additives, 422 Glass transition temperature, 161, 162, 226, 241, 265 3-Glycidyloxypropyl trimethoxysilane, molecular structure, 347 GNP. See Graphite nanoplatelets Granular activated carbon, 82 Granulated blast furnace slag, 369 Graphene, 264, 289 definition of, 5 electronic properties, 5 fiber, 13 zero energy bandgap, 5 Graphene nanoribbon (GNR), 5 Graphene oxide, 13 Graphite, 1, 103 degree of crystallinity, 3 density of, 1, 482 electrical conductivity, 1 energy and momentum of, electrons and holes in, 6 energy band structure, 5–7 exfoliation of, 8 degree of expansion, 8 exfoliated graphite (EG), 8 expansion phenomenon, 8 structure of cell wall, 10 film, 308 glassy state, 1 graphitization, 3 heaters, 400 intercalation of, 7 Daumas-Herold model, 8 structure of, graphite intercalation compound, 8 interplanar spacing, 1 lattice vibrations of, 13 layered crystal structure, 1 mat, 400 noncrystalline state, 1 oxidation resistance, 4 powder, 353 rod, 399 structure of, 1, 2 thermal conductivity, 1 turbostratic carbon, 1 van der Waals bonding, 1

670 Index

Graphite-bromine intercalation (lamellar) compounds interlayer ordering in, 8 Graphite nanoplatelets (GNP), 9 SEM image of, 10 Graphite oxide, 12 electrical conductivity, 12 structural model of, 12 Graphite-potassium intercalation compound structure of stage-1, 7 Graphitization, 3, 44, 94, 389 catalyst, 417 temperature, 409 Graphitized fibers, 391 Gravel/sand ratio, 351 Gray cast iron, 415 Green composite (GC), 394 H HA. See Hydroxyapatite (HA) Hafnium oxychloride octahydrate, 449 Halloysite nanotube (HNT), 226 SEM image, 227 Halpin-Tsai theory, 219 Hazard monitoring, 379 Heat dissipation, 302 Heat-treatment temperature, 410 HER. See Hydrogen evolution reaction (HER) Herringbone structure, 58 Heterogeneous distribution, 258 Hexamethylenetetramine [(CH2)6N4] chemical representation, 513 3D representation, 513 molecular structure of, 513 High-efficiency particulate arrestance (HEPA) filter, 78 High-heat-treatment-temperature (HTT) carbon fiber, 47 Highly porous continuous carbon fiber, 197 High-modulus carbon fibers, 46 standard-modulus carbon fiber and, 46 High-resolution X-ray computed microtomography, 404 High-strength (HT) fiber, 406 High-temperature consolidation, 397

HIPIC. See Hot isostatic pressure impregnation carbonization (HIPIC) HNT. See Halloysite nanotube (HNT) Hobart mixer, 362 Honeycomb sheet, 204 Hot isostatic pressure impregnation carbonization (HIPIC), 388, 396 Hot pressing, 388, 397 HT fiber. See High-strength (HT) fiber Humidity, 269 Hybrid C/C composites, silicon carbide in matrix, 447–449 C/C-SiC fabrication, 447 properties of, 449 C-SiC hybrid matrix, microstructure of, 448 porous C/C preform, pyrolytic carbon effects, 448 porous Si-SiC, oxidation of, 449 Hybrid composite, 132, 201–204, 286, 287 degree of transverse contact, 202 fabrication of, 202 gage factor, 201 intraply hybrid, 202 laminated hybrid, 202 mixtures of fillers, 203 Hybrid matrices, 525 and silicon borocarbide, 527 silicon carbide, 525 titanium silicon carbide and, 527 zirconium boride, 526 and tantalum carbide, 527 zirconium carbide, 525 zirconium oxide, 526 Hybrid reinforcement, 527 carbon fibers and carbon nanotubes, 530 and silicon carbide fibers, 527–528, 530 and silicon carbide whiskers, 528 Hydrated magnesium silicate, 378 Hydraulic cement, primary constituents, 333 Hydrazine, molecular structure of, 558 Hydrogenated butadiene-acrylonitrile (HNBR) elastomer, 296 Hydrogen evolution reaction (HER), 150

Index 671

Hydroxyapatite (HA), 120, 525 composite matrix, 525 Hygrothermal aging, 250 Hypersonic aircraft, 439 I IFSS. See Interfacial shear strength (IFSS) ILSS. See Interlaminar shear strength (ILSS) Imide functional group, 165 Impedance, 277 Impregnation, 125 Infrared thermography (IRT), 408, 504 Injection molding process, 210 In-plane shear modulus, 219 Intelligent transportation system technology, 381 Intercalate, 7 Interfacial layer on, carbon fibers, 470 effects on, oxidation resistance of composite, 470 pyrocarbon (PyC), 470 SiCN, 470 Interfacial shear strength (IFSS), 233 Interlaminar interface, 181–189 contact electrical resistivity, 184–189 curing pressure, effect of, 184 humidity, effect of, 184 impact, effect of, 189 measuring methodology, 187 temperature, effect of, 185–187 thermal damage, effect of, 188 through-thickness compression, effect of, 189 stress, effect of, 182 structure, 181–182 Interlaminar shear strength (ILSS), 225, 387 Intermediate graphitizations, 394 Intermediate-heat-treatment-temperature (IHT) carbon fiber, 47 Internal friction, 433 Interplanar spacing, 408 Intersurface adhesion, 243 Ionic conduction, 352 Ionomer, 113, 235 Iron-matrix composites, 559 Iron nanoparticles, 298

Iron oxide, 362 composite matrix, 524 Irreversible damage, 279 Irreversible disturbance, 272 Irreversible resistance, 283 changes, 271 IRT. See Infrared thermography 3-Isocyanatopropyl triethoxysilane, molecular structure, 228 Isopropanol, molecular structure, 529 Isotropic material, 268 Isotropic pitch, 30 K Kaolin-based ceramics, 384 Kaolinite, 383 structural model, 384 Kerosene decomposition, apparent activation energy, 403 Kevlar fiber, 15, 298 coefficient of thermal expansion (CTE), 16 density of, 15 service temperature of, 17 tensile modulus, 16 vs. carbon fiber, glass fiber, and carbon steel, 15 Kiln sintering, 333 Knudsen diffusion, 403 KOH. See Potassium hydroxide (KOH) L Ladder polymer, 41 Lanthanum hafnate coating, 494 Lanthanum hafnium oxide coating, 495 Lanthanum oxide, 507 Laser beam machining (LBM), 497 Laser joining, 251 Latex/cement mass ratio, 338, 341 conductivity ratio of cement paste, effect on, 342 flexural strength of cement pastes, effect on, 342 flexural toughness of cement pastes, effect on, 342 Lattice composite, 476 Layered composites, 531

672 Index

Layer-to-layer angle-interlock preform, 392 LBM. See Laser beam machining (LBM) Leading-edge panel large hole, 388 LIC. See Li-ion capacitor (LIC) Lightning resistance, 263 Li-ion capacitor (LIC), 98 Lime, 336 Lime-pozzolana cement, 378 Linear wear rate, 448 Liquid crystal structure of, 29 thermotropic, 29 vs. crystalline solid and ordinary liquid, 29 Liquid magnesium, 540 Liquid metal infiltration, 475, 534–535 Liquid metal transfer agent (LMTA) technique, 538 Liquid phase impregnation (LPI), 388, 394–395 Liquid silicon infiltration (LSI), 393, 473, 484 Liquid-vapor phase transformation, 312 Liquid zirconium, 473 Lithium aluminosilicate, 386 Lithium-manganese oxide, 121 Lithium nitrate, 119 Longitudinal electrical resistivity, 364 Longitudinal flexural loading, 240 Longitudinal flexural strength, 402 Longitudinal resistance, 288 Longitudinal resistivity, 279, 286 Loss tangent, 346 Low-drying shrinkage, 378 Low-heat-treatment-temperature carbon fiber, 47 LPI. See Liquid phase impregnation (LPI) LSI. See Liquid silicon infiltration (LSI) M Macropores, 81 Magnesium alloys, 550 Magnesium aluminum silicate (MAS), 465 Magnesium diboride (MgB2), 478 Magnesium-matrix composite, 550 carbon fibers, coatings on, 550 aluminum oxide coating, 552

silicon dioxide coating, 551 titanium dioxide coating, 551 titanium nitride coating, 550 zirconium oxide coating, 553 magnesium alloys, 550 mechanical properties, 554 thermal expansion, 553 Magnesium oxide-matrix composites, 522 Magnetic nanoparticles, 290 Magnetic permeability, 290 Maleimide, molecular structure, 165 Manganese dioxide (MnO2), 121 MAS. See Magnesium aluminum silicate (MAS) Mats, 93 for electrical conductivity, 94 for electrochemical applications, 97 fabrication, 94 for friction materials, 95 mechanical properties, 95 for thermoelectricity, 95 MCVI. See Microwave heating (MCVI) MDA. See 4,4′-methylenedianiline (MDA) Measured (apparent) volume electrical resistivity, variation with time before and after voltage polarity switching for cement paste, 357 Mechanical energy dissipation, 238, 433 Mechanical fastening, 251 Mechanical interlocking, 124 Melt-assisted spinning method, 38 Melting temperature, 169, 311 Melt spinning method, 38 MEMS. See Microelectromechanical systems (MEMS) Mesophase pitch, 29, 389 carbon yield, 29 heterogeneous mixture of, 30 method of production, 30 as precursor, 29 processing of, 29 softening points, 33 spinning of, 31, 32 uses, 32 Mesophase-pitch-based carbon, 452

Index 673

cross-sectional microstructure of, 23 fibers, 391 mechanical properties of, 19 thermoelectric power of, 51 Mesopores, 81 Metal coatings, 537 rule of mixtures (ROM), 537 sodium process, 537 Metal-matrix composites, 532 fabrication of, 533 carbon preform, 536 diffusion bonding, 534 liquid metal infiltration, 534 physical vapor deposition, 536 powder metallurgy, 533 semisolid hot pressing, 536 shaping, 537 squeeze casting, 534 stir casting, 535 thermal spraying, 535 thermal degradation after composite fabrication, 542 during composite fabrication, 542–543 water degradation, 544 Metal (aluminum or copper) meshes, 264 Metal-organic framework (MOF), 120 Methacrylic acid, molecular structure of, 42 Methane, decomposition reaction, 68 Methocel A15-LV, 338 Methylcellulose, 338 molecular structure, 340 Methylcellulose and silica fume, combined use of vs. latex, 346 N-Methyl-4,4′-diaminodiphenylsulfone, molecular structure, 165 4,4′-methylenedianiline (MDA), 163 molecular structure, 166 Methylsilane (CH3-SiH3) molecular structure of, 531 N-Methyl-4,4′-methylenedianiline, molecular structure, 164 Methyltrichlorosilane, 407 molecular structure, 408 Methyltrichlorosilane (MTS), 447

MFCs. See Microbial fuel cells (MFCs) Microbial fuel cells (MFCs), 97 Microcracking, 434 Microcracks, 391 Microdroplet (microbond) test, 236 Microelectromechanical systems (MEMS), 464 Microelectronics, 302 Micropores, 81 Microporous precursor fiber, 40 Microscale composites, 195–197 Microwave absorbers, 300 Microwave absorption, 258 Microwave-assisted pyrolysis, 405 Microwave heating (MCVI), 400 Mitsubishi K13D fiber, 18 MnO2. See Manganese dioxide (MnO2) MnZn ferrite, 302 Modeling of electromechanical behavior, 289 Modified composites flexural modulus, 225 MOF. See Metal-organic framework (MOF) Molding methods, continuous fiber polymermatrix composite fabrication, 206–211 Molybdenum, 557 Molybdenum 2-ethylhexanoate, structure, 523 Monte Carlo method, 472 Montmorillonite, 461 Mortar, 333, 338, 343, 346, 350, 358, 363, 378, 382 Mortar with as-received short carbon fiber, silica fume, and methylcellulose drying shrinkage strain vs. curing age, 345 Mortar with ozone-treated short carbon fiber, silica fume, and methylcellulose drying shrinkage strain vs. curing age, 345 MTS. See Methyltrichlorosilane (MTS) Mullite coating, 494, 495 Mullite-matrix composites, 523–524 Multidirectional laminate, fiber lay-up configuration, 180 Multilamina composite, 280 Multilayer coating, 496 Multilayer cracking, 433 Multiwalled carbon nanotubes (MWCNTs), 52 polyaniline-matrix composites, 290 SEM photograph of, 54

674 Index

N Nafion, 235, 261 Nanobioelectronics, 145 Nanofibers, 63 Nanofibers dispersion methods in cement, 336–348 carbon surface treatment, effect of, 343–348 degree of dispersion, effect of, 341–343 dispersion methods, 338–340 Nanographite, 82 Nanoindentation, 430 Nanoscale filamentous carbons structures of, 58 Nanoscale interlaminar fillers, 228 Nanotube assemblies, 88 Nanotubes dispersion methods in cement, 336–348 carbon surface treatment, effect of, 343–348 degree of dispersion, effect of, 341–343 dispersion methods, 338–340 Nanowire, 296 Naphthalene, molecular structure of, 78 Needled carbon fiber, 440 Neomesophase pitch, 31 Nerve tissue engineering, 145 Network formation, 256 Neural interfaces, 145 Nickel-alumina meta-composites, 290 Nickel-coated short carbon fibers, 258 Nickel-coated SWCNT, 264 Nickel-matrix composites, 562 Nickel nanofiber, 63, 301 schematic illustration of, skin depth, 63 Nickel nitrate hexahydrate, 454 Nitric acid treatment, 343 Nitride-matrix composites, 505 Nitriding, 486 Nonconductivity, 288 Nondestructive evaluation, 332 Nonporous fiber composites, 300 Nuclear fusion reactors, 439 Nuclear power plants, 372 Nylon, 127

O Oblique resistance, 280, 282, 369 Offshore oil rig activities, 380 Optimum latex content, 338 Organic additive, 338 Organic zirconium precursor, 418 Organobentonite, 462 Organoborosilazane polymer solution, 422 Orthosilicate ion, 334 Oxidation protection, 117, 133, 410, 411, 415, 424–428, 494, 496, 503, 512 Oxidation resistance, 65, 116, 249, 310, 385, 405, 419, 421, 423, 427, 436, 461, 463, 470, 479, 487, 490, 495, 502, 509, 516 Oxide-matrix composites, 517 Oxyacetylene torch, 249, 414 Ozone surface treatment, 343 P PAA. See Polyacrylic acid (PAA); See also Polyamic acid (PAA); Polyarylacetylene (PAA) Pack cementation, 411 PAN. See Polyacrylonitrile (PAN) Parallel-plate capacitor, 290 geometry, 292 Particle size, 325 Passive damping, 243 PDDA. See Poly(diallyldimethylammonium chloride (PDDA) PDI. See 1,4-phenylene diisocyanate (PDI) PEALD. See Plasma enhanced atomic layer deposition (PEALD) PECVD. See Plasma enhanced chemical vapor deposition (PECVD) PEEK. See Polyetheretherketone (PEEK) PEI. See Polyetherimide (PEI) PEKK. See Poly(ether-ketone-ketone) (PEKK) PEMs. See Proton exchange membranes (PEMs) Percolation threshold, 295, 337 Perform needling, 492 Perhydropolysilazane, molecular structure of, 506 Permittivity, 293, 296 PES. See Polyethersulfone (PES)

Index 675

Petroleum pitch, 394 Phenanthrene, molecular structure, 78 Phenol-formaldehyde resin impregnation, 440 Phenolic matrix, 229 Phenolic resin, 389 powder, 405 Phenol, molecular structure, 80 1,4-phenylene diisocyanate (PDI), 115 Physical activation method, 83 Physical vapor deposition (PVD), 536 PI. See Polyimide (PI) Piezoelectric material, 243 Piezoresistive effect, 279, 280 Piezoresistive material, 267 Piezoresistive strain sensor, 268 Piezoresistivity, 267, 268, 270, 364 in composites with continuous carbon fibers, 270 in composites with discontinuous carbon fillers, 268 concept, 267 PIP. See Preceramic polymer infiltration and pyrolysis (PIP) Pitch based carbon fibers mechanical properties of, 18 thermal conductivity, 27 composition of, 29 content, 28 fabrication of carbon fibers, 28–34 impregnation, 392 infusiblization, 29 molten form of, 29 softening point, 33 stabilization/ infusiblization, 28 tensile strength of, 33 thermoplastic polymer, 29 Plain cement paste, 376 Plain mortar, drying shrinkage strain vs. curing age, 345 Plasma enhanced atomic layer deposition (PEALD), 117 Plasma enhanced chemical vapor deposition (PECVD), 437 Plastic-elastic fracture toughness, 220

Plastic viscosity, 378 PLD. See Pulsed laser deposition (PLD) Poisson’s effect, 430 Poisson’s ratio, 134, 219, 267, 268 Polarity reversal, 277 Polarization, during DC resistance measurement, 277 Polarized light optical microscopy, 408 Polyacrylic acid (PAA), 119 Polyacrylonitrile (PAN), 112, 300 carbon fibers, 257, 258, 296, 303 color changing in, stabilization process, 35 degree of crystallinity, 27 density, 21 diameter, 21 electrical resistivity, 21 grades of Toray, 45 mechanical properties of, 18 polymerization reaction, 26 SEM photograph of, side view, 22 tensile modulus, 21 tensile strength, 21 thermoelectric power of, 52 chemical steps in, conversion of PAN to carbon, 36 fabrication of carbon fibers, 34–44 Polyamic acid (PAA), 236 Polyamide 66, 253 structure of, 253 Polyamide 6, mer of, 168 Polyaniline (PANI), 52, 258, 266, 296 coating, 296 Polyaniline-coated fiber, 301 Polyaniline-matrix composites, 290 Polyarylacetylene (PAA), 390 Polycarbonate (PC) mer of, 168 Polycarbosilane, 418, 487 Polycrystalline graphite, 140 Poly(diallyldimethylammonium chloride (PDDA), 245 structure of, 245 Polyester, 127 Polyester polyol, molecular structure, 165

676 Index

Polyetheretherketone (PEEK), 161 matrix composite, 132 mer of, 168 Polyetherimide (PEI), 161 mer of, 169 Poly(ether-ketone-ketone) (PEKK), 250 Polyethersulfone (PES) film, 161, 249, 301 matrix composites, 268 direct-current (DC) electrical resistivity of, 200 electrical resistivity, 199 EMI shielding effectiveness of, 200 Polyethylene (PE), 44 staggered conformation, 167 Polyethylene glycol (PEG), 38 Poly(3-hexylthiophene), 331 Polyimide (PI), 161 Polymer-based membranes, 261 Polymer-matrix composites, 130, 257, 279, 288, 294, 302, 331 concepts of mechanical properties, 218–220 with discontinuous carbon fillers carbon black composites, mechanical properties, 237 CNT/CNF composites, mechanical properties, 233–236 composites with both short carbon fiber and CNTs, mechanical properties, 236 short carbon fiber composites, mechanical properties, 230–233 dynamic mechanical properties, 237–243 fatigue behavior, 237–238 viscoelastic behavior, 238–243 environmental degradation, 250 friction and wear behavior, 243–246 continuous carbon fiber composites, 245 interface between unbonded continuous carbon fiber composites, 246 short carbon fiber composites, 244–245 hybrid composites, 251–255 matrix hybridization, 252–253 noncarbon filler, use of, 254 polymeric/metallic interlayer, use of, 254

reinforcement hybridization, 251–252 joining, 251 recycling and upcycling, 250 static mechanical properties, 220–237 continuous carbon fiber polymer-matrix composites, 221–230 polymer-matrix composites with discontinuous carbon fillers, 230–237 thermal expansion, 247–249 types, 161–169 amorphous vs. semicrystalline polymers, 166 epoxy, 163 polymers other than epoxy, 163–165 thermoplastic polymers, example of, 167–169 thermoset and thermoplastic polymers, 161–162 Polymers, 258 glass transition and melting, 169–173 importance to composite processing, 169–170 impregnation, 471 matrix, 256, 265 Poly(methyl methacrylate) (PMMA), 300 matrix composite, 257, 309 structure of, 57 Polymorph α−SiC (6H-SiC), 485 Poly(3-octylthiophene) (P3OT), 330 Poly(organocarbosilanes), 487 Poly(1,4-phenylene diisocyanate) (PPDI), 115 Polyphenylene oxide (PPO), mer of, 168 Polyphenylene sulfide (PPS), 309 mer of, 168 Polyphenyl sulfide (PPS), 161 Poly(p-phenylene benzobisoxazole) (PBO), 44 Poly(p-phenylene benzobisthiazole) (PBZT), 44 Polypropylene (PP), 235 molecular structure, 167 Polypropylene/ polyethylene (PP/PE) blends, 258 Polypyrrole, 259, 260 Polysilazane, 486 Polystyrene (PS), 331 mer, structure of, 57

Index 677

Polysulfone mer of, 168 Polytetrafluoroethylene (PTFE), 92, 232 Poly(trifluoroethyl methacrylate), 265 Poly(2,2,2-trifluoroethyl methacrylate), 265 Poly(trimethylene terephthalate) (PTT) structure of, 230 Polyureasilazane, 92 Polyurethane, 258 Polyvinyl butyral, molecular structure of, 529 Polyvinyl chloride (PVC) mer of, 167 Polyvinylidene fluoride (PVDF), 106, 120, 153, 231 matrix composites, 266 Porous carbon fiber, 300 Portland cement, 333 types, 334 Positive temperature coefficient (PTC) effect, 265 Potassium dichromate, 346 Potassium hydroxide (KOH), 151 Potassium permanganate, 121 Potassium titanium hexafluoride, 541 structure of, 541 Potassium zirconium hexafluoride (K2ZrF6), 541 Potential energy, 265 Pothole repair, 358 Powder metallurgy (PM), 533 admixture method, 533 coating of filler method, 533 reinforcement particles/fibers, 533 formation of neck between, metal particles, 533 variations of, method, 533 Pozzolanic reaction, 336 Pozzolans advantages, 336 calcium hydroxide, reaction with, 336 cementitious value, 336 PP. See Polypropylene (PP) PPDI. See Poly(1,4-phenylene diisocyanate) (PPDI) PP/PEvolume ratio, 258 PPS. See Polyphenyl sulfide (PPS)

Preceramic polymer infiltration and pyrolysis (PIP), 447 Predensification, 404 Preform, 536 machining of, 537 shaping, 537 Premesophase pitch, 31 Pressure gradient method (PCVI), 401 Prestabilization treatments, 42 Propane (C3H8), 481 Propylene glycol molecular structure of, 194 Propylene, molecular structure, 435 Proton exchange membranes (PEMs), 98, 235 Prussian blue, 122 Pseudocapacitor, 151 Pseudoplastic fracture behavior, 409 PTFE. See Polytetrafluoroethylene (PTFE) Pulled-out fiber, 343 Pulsed electric current sintering (PECS), 545 Pulsed laser deposition (PLD), 425 Pultrusion process, 207, 209 PVD. See Physical vapor deposition PVDF. See Polyvinylidene fluoride (PVDF) Pyrocarbon (PyC), 470 deposition, 393 rate, 403 infiltration multiscale model, 404 Pyrocarbon microstructures, 404 Pyrolysis, 17, 390, 471 Pyrolytic carbon, 397 interfacial layer, 415 matrix layer-by-layer, 417 Q Quaternary ammonium cation, structure, 461 R Radiation heating, 358 Ragone plot, 98 Raman peak intensity ratio, 65 Raman scattering, 13 Random walk technique, 404 Reaction shrinkage, 43

678 Index

Reaction sintering, 413 Reactive gas infiltration, 475 Reactive liquid infiltration, 473–475 disadvantage, 473 liquid silicon infiltration (LSI), 473 Reactive thermoplastic pultrusion, 207 Recycling, 133, 250 Reduced graphene oxide (RGO), 106, 120 Regenerative medicine, 145 Relative dielectric constant, 357, 376 strain effect, 376 Renewable energy, 312 Residual flexural modulus, 433 Resin impregnation, 427 Resin infusion molding, 206 Resin transfer molding (RTM) process, 131, 210, 227 Resistance associated with damage, 281 Resistance measurement, 281, 285 Resistance of surface receiving impact vs. impact energy, 285 Resistive heating, 399 Resistivity, 256, 265, 279 relative humidity, effect of, 352 Resonant frequency, 283 Reversible resistance, 268 Reversible strain, 279 RL. See Rough laminar (RL) Room occupancy, 379 Rough laminar (RL), 409 microstructure, 399 RTM. See Resin transfer molding (RTM) Rule of mixtures, 218 S Sandblasting, 230 Sandwich composite, 204 SBR. See Styrene-butadiene copolymer (SBR) Scandium sorosilicate coating, 495 Secondary reinforcement effect, 128 Seebeck effect, 352 Seebeck voltage, 321 Selected laser sintering (SLS) method, 405 Self-heating, 382 Self-lubricious film-like debris, 436

Self-sensing, 289 of damage in hybrid composites, 286–289 of strain and damage, 273, 279 in composites with continuous carbon fiber, 279 Semiconductor-semiconductor interfaces, 266 Semiconductor wafers, 354 Semisolid hot pressing method, 536 Sensing characteristics, one-lamina carbon fiber epoxy-matrix composite sensor, 287 Sensing effectiveness, 287 Sensors, 2D array of, 189 Shape-memory polymer (SMP), 232 shape-memory effect, 232 Shear bond strength, 363 Short carbon fiber composites, 129, 195–197, 509, 518 addition of glass, 518 addition of, magnesium oxide, 520 alumina particles, 518 boron nitride, 519 carbon fiber length, 519 forming mullite, during sintering, 519 friction and wear behavior, 520 hot-pressing carbon fibers, 518 Short carbon fibers cement mortar, double percolation, 350 cement paste, percolation in, 350 dispersion in cement below percolation threshold, 337 dispersion methods in cement, 336–348 carbon surface treatment, effect of, 343–348 degree of dispersion, effect of, 341–343 dispersion methods, 338–340 nanoparticles, use of, 338 organic admixtures, use of, 338 sonication, use of, 340 surfactant, use of, 338–339 ozone treatment, 343 vs. CNF, 346 Short pitch-based carbon fiber, 362

Index 679

SiBCN. See Silicoboron carbonitride ceramic (SiBCN) SiC. See Silicon carbide (SiC) Signal-to-noise ratio, 369 Silica, 76 Silica fume, 335, 336, 338 alkylsilane-treated, 346 cement paste (p-type), 353 Silica-matrix composites, 521 fused silicon dioxide, 521 silicon dioxide aerogel, 522 Silica nanofiber, 103 Silica nanoparticles, 114, 338 Silicoboron carbonitride ceramic (SiBCN), 116 Silicon-based ceramics, 413 Silicon borocarbonitride, 516 Silicon carbide (SiC), 140, 482 as abrasive, 483 coating, 495 consisting of zirconium carbide and, 496 composition, 483 density of, 482 elastic modulus, 483 hydrothermal corrosion, 485 melting temperature, 482 monolithic production, 483 nanofibers, 453 self-healing ability, 485 type of, 483 whisker, 446 Silicon carbonitride, 515 Silicon dioxide, 336 Silicone-matrix composites, 299 Silicone rubber composite, 249 Silicon hafnium borocarbonitride, 517 Silicon nitride nanofibers, 453 Silicon nitride nanoparticles, 244 Silicon nitride nanowires, 492 Silicon nitride (Si3N4) particles, 310 Silver-matrix composites, 557 as brazing materials, 558 effect of graphite flakes, 558 fabrication of, 557 thermal conductivity of, 557 Silver nanoparticles, 288

Silver nanowires, 203, 229, 296 Single carbon fiber apparent tensile modulus and apparent electrical resistivity measurement specimen configuration, 174 Single-lamina composite, 280 Single-walled carbon nanotubes (SWCNTs), 52 structures of, 58 Sintered silicon carbide (SSiC), 483 Sintering, 384 of solids, 475 Skutterudite, 478 SLS method. See Selected laser sintering (SLS) method Slurry casting method, 535 Slurry infiltration (SI), 472–473 alumina sol, 472 gel, 472 isopropyl alcohol slurry, 473 sol, 472 xerogel, 472 Smooth laminar (SL) microstructure, 394 SMP. See Shape-memory polymer (SMP) Sodium acetate molecular structure, 385 Sodium carboxymethylcellulose, 337 Sodium dodecyl sulfate, molecular structure of, 558 Sodium hypophosphite, structure of, 51 Sodium metasilicate-activated calcium aluminate, 379 Sol, 472 Solar cells, 154 Solid-state diffusion, 425 Solution coating method, 539–542 Solvent extraction, 390 Solvothermal treatment, 421 Sonication, 340 Spark plasma sintering (SPS), 545 Specific capacitance, 121 Specific heat, 359 Specimen-contact interface, 292 Spray pyrolysis, 76 Squeeze casting, 534–535 Stainless steel fiber cement, 353

680 Index

Standard-modulus carbon fibers high-modulus carbon fiber and, 46 mechanical properties of, 46 Steatite, 378 Steel fiber cement paste (n-type), 353 Steel rebar, 382 Steel reinforcement, 371 Stiffness, 162 Stir casting, 535 Storage modulus, 239, 364 Strain energy release rate, 220 Strain-sensing, 288 ability, piezoresistivity-based, 354 Strain-sensing effectiveness, 280, 355 Strain/stress sensing, 288 Stress-graphitization, 397 Stress intensity factor, 220 Stress-strain curve, 432 Stretchable electronics, 145 Strong fiber-matrix bonding, 409 Structural vibration monitoring, 379 Styrene-butadiene copolymer (SBR), 153, 338 Styrene, molecular structure, 340 Sucrose, molecular structure of, 488 Sulfate-aluminate cement paste, 361 Sulfoaluminate cement, 376 Sulfonated tetrafluoroethylene-based fluoropolymer-copolymer, 261 Supercapacitors, 151, 259, 290, 291 Supercritical fluid, 395 Supersonic plasma spraying, 414 Surface electrical resistance, 371 Surface fibers, 283 Surface resistance, 271, 278, 280–283, 369 measurement, 280, 281, 286 Surfactants, classification, 338 T Tantalum carbide, 407 Tantalum pentoxide, 407 TEC. See Thermoelectrochemical cell (TEC) Tellurium, 320, 321 particles, 325, 330 TEM. See Transmission electron microscopy (TEM)

Temperature, 269, 277 Tensile fatigue, 288 Tensile stress-strain curve, 41 Tension-tension fatigue evolution of damage, 282 TEOS. See Tetraethoxysilane (TEOS); See also Tetraethyl orthosilicate (TEOS) Tetrabutyl titanate, 551 molecular structure of, 551 Tetraethoxysilane (TEOS), 228 Tetraethyl orthosilicate (TEOS), 118, 420 molecular structure of, 76 Tetrahydrofuran (THF), 33 Thermal conductivity, 161, 302, 307, 308, 310 of continuous carbon fiber polymer-matrix composites, 302–304 of continuous carbon fiber polymer-matrix composites in through-thickness direction, 305–309 of polymer-matrix composites with discontinuous carbon fillers, 309–312 Thermal energy, 265 Thermal expansion, 125 Thermal fatigue resistance, 426 Thermally desized PAN-based fiber, 354 Thermal oxidation, 170 Thermal radiator panels, 439 Thermal resistance (K/W), 305 Thermal spraying method, 535 Thermoelectric behavior, 312 of continuous carbon fiber polymer-matrix composites, 313 of polymer-matrix composites with discontinuous carbon fillers, 330 Thermoelectric effect, 330 Thermoelectric energy, 312 Thermoelectric power, 320, 324 Thermoelectrochemical cell (TEC), 98 Thermogravimetric analysis (TGA), 66 Thermo-oxidative stabilization, 41 Thermoplastic-matrix composites, 250 advantages, 161 disadvantages, 162 Thermoplastic polymer, elastic modulus

Index 681

glass transition and melting temperature, effect of, 170 Thermoplastic polymer matrix, 256 Thermosetting resins, 397 Thiophene, molecular structure, 70 Three-dimensional percolation model, 348 Three-point bending, 369 TiB whisker, 446 TiN. See Titanium nitride (TiN) Tin-lead alloy particles, 263 Tin-matrix composites, 560 contact angle, 560 friction and wear behavior, 561 soldering, 560 thermal conductivity, 561 thermal expansion, 561 Tissue engineering, 145 Titanium butoxide, 551 Titanium ethoxide Ti(OC2H5)4, 540 molecular structure of, 540 Titanium-matrix composites, 559 Titanium nitride (TiN), 156 Titanium tetraisopropoxide [TTIP, Ti(OC4H9)4], molecular structure of, 480 TMA. See Trimethylaluminum (TMA) Toughness, 162 Traffic monitoring, 381 Transfer molding process, 209 Transformers, 354 Transition interlocking structure, 426 Transmission electron microscopy (TEM), 408 Transparent conductive films, 145 Trans-1,4-polyisoprene (TPI) polymer structure of, 232 Transverse electrical resistivity, 364 Transverse fiber modulus, 224 Transverse modulus, 219 Transverse resistivity, 286 Triaxial stress state, 437 Tributyl borate, molecular structure, 421 Tricalcium aluminate, 333 Tricalcium silicate, 333 Triethyl phosphate, molecular structure of, 529 Trimethylaluminum (TMA), 117

Trimethyl borate, molecular structure, 385 Triple percolation, 351 Tunneling, 198 Turbostratic carbon fibers, 1, 24 Two-probe method, 356, 445 Two-step stabilization, 33 Type I carbon fiber. See High-heat-treatmenttemperature (HTT) carbon fiber Type II carbon fiber. See Intermediate-heattreatment-temperature (IHT) carbon fiber U 0˚ Ultimate tensile strain, 221 Ultrasonic probe, 340 Ultrasonic welding, 251 Uniaxial compression, 376 Uniaxial tensile loading, 269 Uniaxial tension, 280 Unidirectional carbon fiber epoxy-matrix composite flexural stress-strain curves, 223 Unmodified carbon fiber, 258 Unmodified composites, flexural modulus, 225 Urethane, 127 V VACNFs. See Vertically aligned CNFs (VACNFs) VACNTs. See Vertically aligned CNTs (VACNTs) Vacuum-assisted resin transfer molding (VARTM), 227 Vacuum bag molding, 206, 208 Vacuum forming process, 211, 212 Vacuum furnace, 420 Vacuum impregnating, 396 Vapor grown carbon fiber, 259 Vaporization, 264 VARTM. See Vacuum-assisted resin transfer molding (VARTM) Vertically aligned carbon fiber array composites, 520 Vertically aligned CNFs (VACNFs), 101 Vertically aligned CNTs (VACNTs), 101 Vibration damping, 238, 364 ability, 335

682 Index

Villari effect, 113 Viscoelastic material stress-strain relationship, graphical representation, 239 Viscose-based activated carbon fiber (ACF), 300 Volume electrical resistivity, 372 measurement method, involving four-probe method, 176 Volume fraction effect, 128 Vulcanization, 258 W Waterborne polyurethane, 296 Water-reducing agent, 334 Waviness, 280 Weighing-in-motion (WIM), 380 Well cementing, 378 Wet spinning method, 38, 39 Whiskerized fabric preform, 416 WIM. See Weighing-in-motion (WIM) Wood fibers short carbon fibers, use with, 252 Worm, 8 Woven carbon fiber polymer-matrix composites, 220 Woven fiber composites, 195 Woven fiber fabrics, 195 bending of one fiber over another, 196 carbon fiber fabric, 433 cross-sectional view of fabric layers, 196 schematic illustration of, fiber tows woven together, 196

X Xerogel, 472 X-ray compton backscattering radiography, 408 X-ray computerized microtomography (CMT), 404 X-ray diffraction, 408 Y Yarns, 98 fabrication, 98 mechanical behavior, 99 for microelectrodes, 100 Young’s modulus, 542 Ytterbium oxide, 507 Yttrium oxide, 428, 507 Yttrium silicate coating, 494, 495 Z Zigzag orientation, 65 Zirconium boride, 526 and tantalum carbide, 527 Zirconium carbide (ZrC), 477, 525 crystal structure of, 478 as matrix, 480 Zirconium diboride (ZrB2), 119, 419 Zirconium oxide, 526 Zirconium oxychloride (ZrOCl2), 542 molecular structure of, 542 Zirconium tetrachloride, structure, 414 ZrB2. See Zirconium diboride (ZrB2) ZT value, 328 Z value, 327 Z yarn, 392