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Metadata of the chapter that will be visualized in SpringerLink Book Title Eco-friendly Polymer Nanocomposites Series Title Chapter Title Multifunctionalized Carbon Nanotubes Polymer Composites: Properties and Applications Copyright Year 2015 Copyright HolderName Springer India Author Family Name Julkapli Particle Given Name Nurhidayatullaili Muhd Prefix Suffix Division Nanotechnology & Catalysis Research Centre (NANOCAT), IPS Building Organization University Malaya Address 50603, Kuala Lumpur, Malaysia Email Author Family Name Bagheri Particle Given Name Samira Prefix Suffix Division Nanotechnology & Catalysis Research Centre (NANOCAT), IPS Building Organization University Malaya Address 50603, Kuala Lumpur, Malaysia Email Corresponding Author Family Name Sapuan Particle Given Name S. M. Prefix Suffix Abstract Division Department of Mechanical and Manufacturing Engineering Organization Universiti Putra Malaysia Address 43400 UPM, Serdang, Selangor, Malaysia Email [email protected] Carbon nanotubes (CNTs) is a rigid rod-like nanoscale material produced from carbon in powder, liquid, or gel form via acid or chemical hydrolysis. Due to its unique and exceptional renewability, biodegradability, mechanical, physicochemical properties, and abundance, the incorporation associated with a small quantity of CNTs to polymeric matrices enhance the mechanical and thermal resistance, and also stability of the latter by several orders of magnitude. Moreover, NCC-derived carbon materials are of no serious threat to the environment, providing further impetus for the development and applications of this green and renewable biomaterial for lightweight and degradable composites. Surface functionalization of CNTs remains the focus of CNTs research in tailoring its properties for dispersion in hydrophilic and hydrophobic media. Through functionalization, the attachment of appropriate chemical functionalities between conjugated sp2 of CNTs and polymeric matrix is established. It is thus of utmost importance that the tools and protocols for imaging CNTs in a complex matrix and quantify its reinforcement, antimicrobial, stability, hydrophilicity, and biodegradability are be developed. Keywords (separated by '-') CNTs - Composites - Polymer - Functionalization and applications Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 1/61 Time: 2:52 pm 4 Nurhidayatullaili Muhd Julkapli, Samira Bagheri and S.M. Sapuan 5 19 Abstract Carbon nanotubes (CNTs) is a rigid rod-like nanoscale material produced from carbon in powder, liquid, or gel form via acid or chemical hydrolysis. Due to its unique and exceptional renewability, biodegradability, mechanical, physicochemical properties, and abundance, the incorporation associated with a small quantity of CNTs to polymeric matrices enhance the mechanical and thermal resistance, and also stability of the latter by several orders of magnitude. Moreover, NCC-derived carbon materials are of no serious threat to the environment, providing further impetus for the development and applications of this green and renewable biomaterial for lightweight and degradable composites. Surface functionalization of CNTs remains the focus of CNTs research in tailoring its properties for dispersion in hydrophilic and hydrophobic media. Through functionalization, the attachment of appropriate chemical functionalities between conjugated sp2 of CNTs and polymeric matrix is established. It is thus of utmost importance that the tools and protocols for imaging CNTs in a complex matrix and quantify its reinforcement, antimicrobial, stability, hydrophilicity, and biodegradability are be developed. 20 Keywords CNTs 21 1 Introduction 22 1.1 Polymeric Nanocomposites: Advantages and Limitation 9 10 11 12 13 14 15 16 17 18 23 24 PR OO D 8 TE 7 EC 6
Composites
Polymer
Functionalization and applications OR R 2 F 3 Multifunctionalized Carbon Nanotubes Polymer Composites: Properties and Applications 1 Polymer composites are made up of a polymeric matrix with some physically distinct distributed phases called reinforcements, or fillers (Richard and Giannelis UN C Author Proof Layout: T1 Standard Unicode N.M. Julkapli
S. Bagheri Nanotechnology & Catalysis Research Centre (NANOCAT), IPS Building, University Malaya, 50603 Kuala Lumpur, Malaysia S.M. Sapuan (&) Department of Mechanical and Manufacturing Engineering, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia e-mail: [email protected] © Springer India 2015 V.K. Thakur and M.K. Thakur (eds.), Eco-friendly Polymer Nanocomposites, Advanced Structured Materials 75, DOI 10.1007/978-81-322-2470-9_6 1 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 2/61 Time: 2:52 pm 30 31 32 33 34 35 36 37 38 39 40 41 42 43 F PR OO 29 D 28 TE 27 2001; Zheng-Ming et al. 2003; Paul et al. 2007; Rohan and Darrin 2007; Xiaofeng et al. 2011). The reinforcing fillers combined with the polymeric matrix result in preferred qualities, such as high stiffness, strength, flame redundancy, scratch/wear resistance, toughness, thermal/electrical conductivity, electromagnetic shielding, coefficient thermal expansion, wear, and damping resistances (Zheng-Ming et al. 2003; Rohan et al. 2007; Lin et al. 2012a, b). The polymeric nanocomposites consist of a polymer with nanoparticles or nanofillers dispersed in its matrix (Paul et al. 2007; Thakur et al. 2012). It is expected that the transition from micro to nanoparticles increase the surface area-to-volume ratio (Thakur et al. 2014a, b). This in turn results in a prominent increment of the behavior of the atoms on the surface of the particles. It affects the properties of the particles when they react with other particles (Yuan-Qing et al. 2008). Due to the higher specific surface area of nanoparticles, the interaction with other particles within the mixture became more intense (Dubois and Alexandre 2006). This consequently results in positive properties, such as high temperature capability, resistance against corrosion, noise damping, low in cost/manufacturer, ductile, high specific stiffness and strength, high thermal conductivity, and low coefficient of thermal expansion (Fig. 1). Another advantage of polymer nanocomposites is that it could be fabricated via rapid and precise manufacturing methods, such as injection molding, compression EC 26 OR R 25 N.M. Julkapli et al. UN C Author Proof 2 Fig. 1 Advantages and disadvantages of polymeric nanocomposites Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 3/61 Time: 2:52 pm 3 69 2 CNTs: General View 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 70 71 72 73 74 75 76 77 78 79 80 PR OO 49 D 48 TE 47 EC 46 OR R 45 F 68 molding, vacuum bag molding, contact molding, and resin transfer molding (Peter and Richard 2002; Hua and Brinson 2005). Therefore, polymeric nanocomposites are posited as appropriate options in overcoming the inherent restrictions of microcomposite and monolithic, while posing preparation challenges related to the control of elemental composition and stoichiometry in the nanocluster phase. In the development of polymer nanocomposites, there are several challenges and limitations. For example, polymeric nanocomposites require controllable mixing/ compounding, stabilization of the dispersion, and orientation of the dispersed phase. Despite the fact that the modulus of polymeric nanocomposites increases with the increasing nanofiller content, toughness, and thus it impacts the strength which decreases when the materials became more brittle (Kiliaris and Papaspyrides 2010; Xiao-Lin et al. 2004; Reddy et al. 2008). The viscosities of polymeric nanocomposites also increase with the nanofiller content, which render manufacturing difficult (Adams and Charles 2001). Furthermore, a highly viscous flow of polymer melts induced large forces or cause short shots during extrusion and injection molding. In other words, the effect of nanofiller on the polymer properties differs from predicted using the thermodynamic studies for reduced particle size filler (Gary and Dimitris 2008). Studies and modeling using continuum mechanics revealed that the enhanced properties of nanocomposites strongly depend on particular features of the nanofiller system, particularly its content, aspect ratio, and the ratio of filler mechanical properties to those of the matrix. Furthermore, uniform dispersion of fillers (micro/nano) particles/fibers within the polymer matrix is limited due to the formation of agglomerates (Singha et al. 2009a, b; Yuan-Qing et al. 2008; Thakur et al. 2012). Agglomeration induced defects that limit the mechanical performance of the polymeric composite materials (Gary and Dimitris 2008; Thakur et al. 2014a, b, c). 44 Carbon nanotubes (CNTs) were discovered in 1991, and since then many studies were dedicated to it and its related nanomaterials due to its superior electronic, chemical, and mechanical properties (Li et al. 1996; Micheal et al. 2002; Min-Feng et al. 2000a, b; Philip et al. 2000). The general structure of CNTs is depicted as a rolled up sheet of a planar-hexagonal arrangement of carbon atoms dispersed in a honeycomb lattice (Micheal et al. 2002). There are two major categories of CNTs; single-walled (SWCNTs) and multiwalled (MWCNTs). UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … 2.1 CNTs: Properties CNTs exhibited unique mechanical, thermal, and field emission properties and electrical conductivity (Min-Feng et al. 2000a, b) (Table 1). It is claimed that CNTs have an elastic modulus that is higher than carbon fibers, and is five times stronger Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 4/61 Time: 2:52 pm Author Proof 4 N.M. Julkapli et al. Table 1 List on properties and characterization of CNTs Testing/analysis Results References Stiffness Observation the amplitude of thermal vibration inside the transmission electron microscopy A stress–strain measurement utilizing a nanostressing stage operating in the scanning electron microscope 1.8–1.25 TPa Min-Feng et al. (2000a, b) 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 101 2800 °C Electrical conductivity twice higher than diamond and 1000 times higher than Cu wire TE D High-temperature differential scanning calorimetric analysis Outer shell of MWCNTs (11–63 GPa) Fracture strains (12 %) Modulus (270–950 GPa) Strength is 10–100 times more than the strongest steel 1 TPa Min-Feng et al. (2000b) and Demczyk et al. (2002) Treacy et al. (1996) and Jian (1997) Savas et al. (2000) and Hone et al. (1999) than carbon fibers. Its strength is determined by the number of defects, bundles of SWCNTs, and interlayer interactions within MWCNTs (Philip et al. 2000). The structural defects, together with twists or bends, considerably influence the mechanical strength of the CNT. It is shown that the CNTs absorb near-infrared light at wavelengths that are optically transparent to native tissues (Kenji et al. 2000). This allows selective drug delivery that is capable of sufficient heating and killing the target cell. In addition to the mechanical behavior, CNTs also possess very high intrinsic electrical conductivity. The electrical conductivity of CNTs is in the range of 107–108 S m−1, which is comparable to metals (Li et al. 1996). The room temperature conductivity of metallic SWCNTs was found to be 105–106 S m−1, and for CNTs, which is a semiconductor, it is about 10 S m−1. Its electrical conductivity assisted in imparting conductivity in remarkably insulating materials (Min-Feng et al. 2000a, b). Certain theoretical studies on the electronic properties of SWCNTs pointed out that CNTs shells depend on which helicity could be metallic or semiconducting (Tang et al. 2001). This was analyzed due to the weak control on generation; more than 30 % of SWCNTs formed are metallic, while the rest are semiconductors. The axial thermal conductivity of individual, perfect CNTs were showed to be as high as 3300 W m−1 K−1 (Brigitte et al. 2000). Due to these factors and also their superior electrical and thermal properties, lots of consideration have been dedicated to the use of CNTs as reinforcement in polymeric composite systems (Li et al. 1996). EC 83 Thermal/ electrical stability OR R 82 A stress–stains curve UN C 81 Elastic modulus PR OO Tensile strength F Properties Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 5/61 Time: 2:52 pm 107 108 109 110 111 112 113 114 115 116 117 118 119 120 121 122 123 124 125 126 127 128 129 130 131 132 133 134 135 136 137 138 139 140 141 142 143 144 F PR OO 106 D 105 One of the most intriguing problems in the synthesis of CNTs is to understand its microscopic growth mechanism and determine ways of controlling it (Journet et al. 1995). Currently, experimental techniques have been developed, and CNTs could be produced with various methods and very flexible environments (from higher than 3000 °C of arc discharge, to laser ablation to as low as 500 °C of chemical vapor deposition methods to control the growth of CNTs (Table 2). The optimum pressure of the arc-discharge method of up to 500 Torr resulted in more than 75 % conversion of CNTs in large quantities (Hutchisona et al. 2001). In addition to the aforementioned main generation methods, there are other parameters to these routes, such as ball milling, cold water, SiC decomposition, graphene scrolling, and flame synthesis (Hwa-Jeong et al. 2005; Zhu et al. 2005; Pierard et al. 2001; Li et al. 1999). Due to its unique quasi one-dimensional structures, CNTs have different chirality, diameters, and layers, which were in turn brought about from different growth conditions and behaviors (Scott et al. 2001). For example, hollow tubes of CNTs, with a C range between 2 and 50 nm in diameter, are produced by a mixture of benzene and H2 decomposition using arc-discharge apparatus at low pressures of argon (100 Torr) (Journet et al. 1995). Furthermore, the addition of catalyst to the synthesis of CNTs plays an important role in its nucleation and sustained growth (Stig et al. 2004; Chris et al. 2000). A noteworthy aspect is the emergence on nonmetal catalyst; these might well replace metallic catalyst system due to their potential of yielding high-purity samples, and compatibility with silicon technology (Hwa-Jeong et al. 2005). Meanwhile, CNTs with a fully interconnected two-dimensional ring network has been grown by low-temperature chemical vapor deposition prepared from nanochannel network template in porous anodic alumina (Stig et al. 2004; Chris et al. 2000). In this case, CNTs strictly grow in a both-tip mechanism; with the ends open and growing forward in both directions by the incorporation of C clusters (Fig. 2). Meanwhile, MWCNTs have 2–50 walls or concentric tubes prepared by the deposition of carbon evaporation from the anode for condensation on the cathode (Chris et al. 2000). Therefore, different growth mechanisms were proposed to explain the underlying initiating process and dynamical growth, which focuses on the metal catalystassisted growth. In this case, the precipitation of diffusion of C atoms at the catalyst’s surface is believed to precipitate the continued growth of CNTs (Pierard et al. 2001; Li et al. 1999). However, these proposed mechanisms are still highly controversial, due to the lack of experimental proofs and inability of explaining the growth behavior. In the last few years, great advances have been made regarding SWCNTs separation, based on metallicity. Positive developments were made in controlling and optimizing the generation of CNTs, as well as its separation and purification via chirality and metallicity (Hongjie et al. 2002; Rodney et al. 2002). Therefore, SWCNTs were formed as a small amount of metal particle placed on a dimple TE 104 EC 103 5 2.2 CNTs: Synthesis Process OR R 102 UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 6/61 Time: 2:52 pm Author Proof 6 N.M. Julkapli et al. Table 2 The synthesis methods on production of CNTs Advantages Disadvantages Arc discharge The arc ignited between two electrodes of graphite in an H2 gas The arcing evaporates the C and while it cools and condenses that some of the product forms as filamentous C on the cathode Direction of intense pulse of laser light on a C surface in a stream of He gas Mass production of CNTs and fullerenes Multimorphology shoots productions The CVD process in that volatile precursors utilized to provide a C feed source to a catalyst particle or pore at elevated temperature around 350–1000 °C, heated flow of CO, pressure between 1 and 10 atm Require several purification steps High temperature process Scott et al. (2001) D Not suitable for mass production Modification process parameters needed to control SWCNTs diameter distribution and yield Stig et al. (2004) and Chris et al. (2000) 145 146 147 UN C OR R Chemical vapor deposition (CVD) EC The evaporated material condenses to yield fullerenes Combination of a metal catalyst in the C target results in the formation of SWCNTs with a tiny diameter distribution and high SWCNTs yield and diameter distribution could be varied by controlling the process parameters An extensive method which also shows multivariable process can adjust in a several manner like plasma enhanced CVD, thermochemical CVD, aerogel supported, high pressure CO disproportionation, alcohol catalytic CVD, aerosol assisted CVD, and hybrid laser assisted thermal CVD Mass production Hutchisona et al. (2001) TE Laser ablation Production of both SWCNTs and MWCNTs References F Description PR OO Synthesis methods cathode and a mixture of argon and methane atmosphere utilized during arc discharge (Hutchisona et al. 2001). For example, 2 at.% Co-containing anode utilized in the arc-discharge apparatus under the atmosphere results in an 80 % selectivity of Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 7/61 Time: 2:52 pm 7 PR OO F Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … Fig. 2 In situ HRTEM image sequence of the growing CNTs (Scale bar = 5 nm). Images (a–h) show one cycle in the elongation/contraction process (Stig et al. 2004) 152 2.3 CNTs: Applications 154 155 156 157 158 159 160 TE EC 153 The CNTs have exposed completely new paths intended for establishing novel functional materials. Thus, some applications seek to exploit CNTs with respect to different fields (Table 3). The combination of CNTs with some macromolecules improves the conductivity of the material, representing one avenue of application (Brigitte et al. 2000; Demczyk et al. 2002). The large environmental window and the electrochemical stability draw essential values onto CNTs (Jian 1997). Additionally, the extension of the functional techniques for two-dimensional carbon, including grapheme, is a growing area in semiconductor applications. OR R 150 Table 3 List on applications of CNTs corresponding to its characteristics UN C 149 D 151 SWCNTs. Then, the synthesis of SWCNTs via evaporation of a hot (1200 °C) transition metal containing C target by the laser ablation technique is followed by the condensation on a cold finger, yielding up to 80 % purity at 50 kg day−1 (Shigeo et al. 2002; Flahaut et al. 2000). 148 Applications of CNTs Characteristics of CNTs Structural applications High tensile strength fibers Fire resistance properties Electromagnetic properties Parallel carbon sheets Electroacoustic potential properties Fast oscillators Semiconductor properties Field emission properties Artificial muscles Loudspeakers Air/water filtration Electronic devices Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 8/61 Time: 2:52 pm 3 CNTs: In Polymeric Composites F 161 N.M. Julkapli et al. 189 3.1 CNTs: In Synthetic Polymeric Composites 190 3.1.1 CNTs: In Thermoset Polymeric Composites 191 Thermoset resin is a petrochemical in a viscous state or soft solid, which changes irreversibly straight into an infusible, insoluble polymer system via curing (Pickering et al. 2000; Wim and Richard 2004; Makki et al. 2005; Torresa et al. 2000). The curing process of thermosets could be induced via radiation or heat. The actual curing procedure converts the resin into a rubber or plastic through crosslinking (Wim and Richard 2004). Adding energy and catalysts results in the 167 168 169 170 171 172 173 174 175 176 177 178 179 180 181 182 183 184 185 186 187 192 193 194 195 196 D 166 TE 165 EC 164 OR R 163 PR OO 188 Since surface characteristics influence its proinflammatory effect, embedding CNTs in polymeric materials modifies the surface environment. This, in turn, could modify its toxicity, thus representing a useful strategy in reducing adverse health effects of industrially produced CNTs (Joseph et al. 2005; Andrews and Weisenberger 2004; Huisheng 2008; Peng et al. 2008). Furthermore, there are great challenges and opportunities expected for the CNTs as nanoscopic reinforcement in polymer matrices (Andrews and Weisenberger 2004). These opportunities include CNTs with a small number of defects per unit length possessing 27,500 times higher specific surface area per gram according to the equivalent volume fraction of typical carbon fiber, and a high aspect ratio, mostly exhibiting great tensile, thermal, and electrical properties (Huisheng 2008). In addition to the economic advantages caused by combining expensive CNTs and cheap polymer, it is also possible where a synergy presents itself between the CNTs and polymeric materials (Breuer and Uttandaraman 2004). This, in turn, brought about the simple rule of mixture, which fully utilize CNTs properties in producing a composite system with promising properties. Furthermore, due to their hollow nature, CNTs can be opened and filled with various materials such as biological molecules, which in turn generate technological opportunities (Chenyang et al. 2003; Petra et al. 2002; Myounggu et al. 2008). This combination addresses the challenges in producing homogeneous dispersion and strong interfacial interactions, improving surface grafting/functionalization. To tailor and optimize the properties of CNT-filled polymer composites, it is necessary to disperse the CNTs homogeneously with the sustenance of strong interaction and adhesion of composite components via several proposed methods (Table 4). Finally, nanoreinforcements using biodegradable polymers possess a substantial possibility of the structure of eco-friendly green materials regarding future applications (Joseph et al. 2005). 162 UN C Author Proof 8 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 9/61 Time: 2:52 pm Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … 9 Table 4 Mainly used methods with commercial viability in preparation of CNTs-filled polymer composites Advantages Disadvantages References Solution mixing Simplest and most widely used methods CNTS and polymer mixed with a suitable solvent, evaporated in control conditions Acceptable for wide range of polymer Obtain a good dispersion with ultrasonic agitation methods Acceptable for polymer with solution mixing approach problem Methods involved melting of the polymer to form viscous liquid followed by blending with CNTs Dispersion of CNTs improved by shear mixing CNTs dispersion into the monomer matrix in the presence or absence of solvent which followed by standard methods of polymerization Enables the grafting of polymer molecules on CNTs Better dispersion coefficients Better interactions between CNTs and polymeric matrix Process deal with insoluble and thermally unstable polymer Compatibility issue between functionlized CNTs and polymer matrix Agglomeration of CNTs takes place after evaporation process Zhaoxia et al. (2001) and Zdenko et al. (2010) Less efficient than solution mixing due to the high viscosity of thermoplastic polymer Hindrance in achieving uniform dispersion of CNTs Wenzhong et al. (2003) and Haggenmuellera et al. (2000) PR OO D Limited number of polymer used Seung et al. (2003) and Fenga et al. (2003) 198 199 200 201 202 203 204 205 molecular chains being able to react at chemically active sites, linked into a rigid three-dimensional structure. The cross-linking procedure forms a molecule with a much larger molecular weight, leading to a material with a much higher melting point. Throughout the reaction, the molecular weight increased to a point so that the melting point exceeds the ambient temperature, and the material forms a solid material (Toressa et al. 2000). The CNT-filled thermoset polymer composites have been fabricated and studied with different kinds of thermosets, such as epoxides, polyester, and polyimide resin. Most of the mechanical, conductivity, and thermal stability of the thermoset resin increases with the addition of low content CNTs. UN C 197 OR R EC In situ polymerization TE Melt processing F Preparation methods Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 10/61 Time: 2:52 pm N.M. Julkapli et al. CNTs: In Epoxides Polymeric Composites 207 The reinforcement of CNTs into epoxy improved mechanical properties, such as strength, stiffness, and durability (Huang et al. 2014a, b, c; Battisti et al. 2014a, b; De Borbon et al. 2014). Furthermore, MWCNTs with epoxy coatings increase the adhesion strength of the matrix, and exhibit hydrophobicity, low water intake, and corrosion resistance, flame retardant, and antioxidation properties (Koreyam et al. 2014; Grabowski et al. 2014). CNT-filled epoxy composites comprised most of studies utilizing the in situ polymerization method, where the CNTs were first dispersed in the resin and cured with a hardener (Korayem et al. 2014). Meanwhile, there are some studies that prepare epoxy composites by this method, utilizing carboxylated end-cap SWCNTs and an esterification reaction to fabricate composites with enhanced tensile modulus (Guo et al. 2014). It is worthy pointing out that as polymerization moves along, the viscosity is enhanced (Gardea and Lagoudas 2014; Wang et al. 2014a, b, c). Thus, the addition of CNTs into epoxy resin increases the mechanical properties, but only to a point. For example, monotonic increased with hardness was observed to up to a factor of 3.5 by loading of 2 wt% of SWNT into the epoxy matrix (Wang et al. 2014a, b, c; Bal and Saha 2014). Furthermore, the measured fracture energy increased from 133 to 223 J m−2 with the addition of 0.5 wt% of CNTs. In order to transfer the superior properties of the epoxy matrix, the functionalization of as-prepared CNTs is crucial for realizing proper dispersion and strong interfacial bonding (Fig. 3) (Kuzhir et al. 2013; Rajendra et al. 2013; Li et al. 2013a, b, c, d, e; Florian et al. 2003). CNT’s electrical conductivity-filled epoxy nanocomposites, with less than 0.5 wt % of CNTs, were improved by several orders of magnitude (Jiang et al. 2013a, b; Russ et al. 2013; Prolongo et al. 2013, He et al. 2013; Safdari and Al-Haik 2013). Furthermore, thermal conductivity of epoxy matrix at room temperature increased by 300 % on 3 wt% SWCNTs loading, and an additional increase of 10 % once they are magnetically aligned (Li et al. 2013a, b, c, d, e). Similar observations were found on epoxy nanocomposites with 1 wt% raw laser oven SWCNTs, and recorded a 125 % thermal conductivity enhancement. In addition, the CNT’s alignment plays a key role in improving the transport properties of CNT-filled epoxy composites (He et al. 2013). Compared to its non-aligned counterpart, 10 % increment in thermal conductivity was recorded with aligned MWCNTs. Moreover, the ultra-low electrical percolation threshold of the 0.0025 wt% in aligned CNTfilled epoxy composites were correspondingly recorded (Russ et al. 2013). This affect the aspect ratio of CNT-filled polymer composite vis-à-vis the electrical shielding properties. Some studies focused on the electrical conductivity properties of CNT-filled epoxy nanocomposites with respect to the aspect ratio and percolation threshold of CNTs. It is found that there is an eight times decrease in the threshold concentration in MWCNT-filled epoxy composites as its length increased from 1 to 50 µm (He et al. 2013). Meanwhile, the minimum percolation threshold concentration of MWCNT-filled epoxy was recorded at 0.0021 wt% of MWCNTs (Safdari and Al-Haik 2013). Furthermore, there are some reports on the effect of surface functionalization of CNTs toward the electrical conductivity of the 213 214 215 216 217 218 219 220 221 222 223 224 225 226 227 228 229 230 231 232 233 234 235 236 237 238 239 240 241 242 243 244 245 246 247 248 249 PR OO 212 D 211 TE 210 EC 209 OR R 208 F 206 UN C Author Proof 10 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 11/61 Time: 2:52 pm 11 OR R EC TE D PR OO F Fig. 3 TEM images of functionalized CNTs. Epoxides covers the surface of the CNTs which indicates an improved interaction (a). CNTs improve the fracture toughness by bridging pores and microcracks in the epoxies (b and c). Telescopic pull-outs substantiate the evidence of improved interactions (d and e) (Florian et al. 2013) UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 12/61 Time: 2:52 pm N.M. Julkapli et al. 259 CNTs: In Polyester Polymeric Composites 260 The CNT-filled unsaturated polyester composites with styrene have extensive usage in industrial applications included structural (Jung and Park 2013), automotive, (Seyhana et al. 2007a, b, c) aerospace (Liang et al. 2009), and others. Conventionally, the composites were fabricated through three-roll ill and sonication technique, which fabricated CNTs with and without NH2 functional groups and polyester. The CNT-filled polyester suspension demonstrated a shear loss behavior, while the polyester resin combination behaves in the manner of a Newtonian fluid. Improvements within the character of the rheology of the CNTs/polyester suspension checked like a function of the level of energy, introduced via ultrasonic horn mixing and associated with microscopic observations. However, the reported improvement on mechanical and thermal properties of CNT-filled polyester composites is considerably lower than the expectation due to difficult alignment of CNTs, weak dispersion, and poor interface between polyester matrix and CNTs, which are usually associated with geometrical properties of CNTs, polyester properties, and fabrication methods (Liao et al. 2011; Hossain et al. 2011; Agnihotri and Kar 2007). To overcome these obstacles, various efforts included ultrasonication, surface treatment, shear mixing, bi-tri-axial rolling, extrusion, and combination process, all of which were designed to properly accomplish excellent dispersion of CNTs in polyester (Hossain et al. 2011). Furthermore, several methods were suggested for managing CNT alignment in polyester by utilizing shear, elongation, and melt processing, as well as magnetic field or electrical spinning (Matthew and Virginia 2009; Qiao et al. 2006). Furthermore, the self-polymerization and styrene evaporation at high temperatures are main issues that need to be accounted for whenever a thermoset polyester resin was blended together with CNTs by utilizing the three-roll milling and sonication technique. It is surmized that the three-roll milling technique is more suitable for dispersing CNTs in polyester resin blends compared to other techniques such as direct mixing and sonication (Matthew and Virginia 2009). Another study prepared CNTs/polyester composites by shear mixing with no solvents. In this case, additional energetic mixing of the condition generated greater dispersion at both the nanoscopic and microscopic levels. The results demonstrate that the dispersion depends on the high shear conditions on the structure and nature of nanofilaments 256 257 261 262 263 264 265 266 267 268 269 270 271 272 273 274 275 276 277 278 279 280 281 282 283 284 285 286 287 288 289 290 291 PR OO 255 D 254 TE 253 EC 252 OR R 251 F 258 nanocomposites. It is found that for nanocomposites, the incorporation of octadecylated and acid functionalized MWCNTs in the epoxy resin, reducing the electrical conductivity (Abu et al. 2006; Jeena et al. 2010). Therefore, it is very important to improve the modification reagent or condition of CNTs to minimize the degradation of electrical properties. A noteworthy enhancement in the mechanical and electrical conductivity of CNT-filled epoxy composites lead to the development of conductive materials for electronics, automotive shielding, electrostatic dissipation, conductive coating, multilayer printed circuits, and electromagnetic inference. 250 UN C Author Proof 12 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 13/61 Time: 2:52 pm 13 306 CNTs: In Polyimides Polymeric Composites 307 Polyimides are broadly utilized in the manufacture of aircraft assemblies, packaging materials, microelectronic devices, interlayer dielectrics, and circuit boards (Zhang et al. 2010; Cui et al. 2013; Ko et al. 2014; Jiang et al. 2014a, b). This is due to its special structure, flexibility, good dielectric properties, great glass transition temperature, excellent thermal stability, radiation resistance, and thermal and mechanical characteristics (Wu et al. 2013a, b, c). The electrostatic charge is accumulated on the surface of polyimides, due to its insulating nature, which causes local heating, and consequently leads to premature material degradation. Therefore, the promising mechanical strength, thermal stability, and surface resistivity of Polyimide could be realized by the addition of CNTs as filler (Jia et al. 2012). Polyimide/CNTs composites can be prepared using various fabrication techniques, such as polymerization, wet casting, and efficient solution. It is suggested that in situ polymerization is one the most suitable fabrication technique of CNT-filled polyimides composite, which also results in the introduction of certain level of electrical conductivity despite lower loadings of CNTs (Wang et al. 2014a, b, c). There are some reports on the synthesis of SWCNTreinforced polyamide composites via the sonication of in situ polymerization of diamine and dianhydride (Chen et al. 2011; Schlea et al. 2012). Other studies have fabricated CNT-filled polyimides composites by in situ polymerization, utilizing 4,4′-oxydianilline, MWCNTs, and pyromellitics dianhydride, continued with casting, evaporation, and also thermal imidization (Xiaowen et al. 2006; Hyang et al. 2007). The incorporation of 3 wt% MWCNTs improved the mechanical features of polyimide due to the presence of a robust interfacial interaction between the CNTs and polymer matrix (Hyang et al. 2007). It is also pointed out that the tensile strength increased from 102 MPa for neat polyimide, to 134 MPa for the 6.98 wt% MWCNTs/polymides composites (Xiaowen et al. 2006). Furthermore, pretreatment of CNTs in solvent released enough CNTs, which resulted in the percolation of 298 299 300 301 302 303 304 308 309 310 311 312 313 314 315 316 317 318 319 320 321 322 323 324 325 326 327 328 329 330 331 332 333 PR OO 297 D 296 TE 295 EC 294 OR R 293 F 305 (Seyhana et al. 2007a, b, c). The most effective dispersion is realized by demonstrating the minimum percolation threshold, which did not correspond to the most energetic mixing conditions. Moreover, lower nanofilament concentrations resulted in a much better dispersion, which demonstrates superior mechanical performance (Qiao et al. 2007). With regards to electrical resistivity properties, the quality of the CNTs dispersion within the polyester matrix was studied using optical microscopy (Cao et al. 2003). The results showed that polyester matrix is suitable for the preparation of electrically conductive thermosetting nanocomposites at low CNT concentrations. Moreover, surface functionalization of CNTs influenced the final properties of the composites. Thus, they are focused on enhancing the CNTs/polyester master batches without styrene through various kinds of functional groups to obtain the desired mechanical properties and microstructure of composites (Seyhana et al. 2009; Hilmi et al. 2010; Esteban et al. 2013; Ziyan et al. 2014). 292 UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 14/61 Time: 2:52 pm N.M. Julkapli et al. 364 3.1.2 CNTs: In Thermoplastic Polymeric Composites 365 The CNT-filled thermoplastic composites have been effectively introduced into an extensive range of applications formerly owned by thermoset composites (Ortengren 2000; Kanagaraj 2010; Nie and Fisher 2013; Zaminpayma 2014; Pang et al. 2014; Kulathunga and Ang 2014). Generally, thermoplastic possess high toughness, larger impact resistance, and ease of shaping and recycling compared to thermoset. However, the use of thermoplastic as a matrix of CNTs composites is traditionally limited due to impregnation difficulties and high temperatures (Nie and Fisher 2013). The processing methods included Fulcrum thermoplastic composites technology, comingled thermoplastic fabrics, powder/sheath fibres bundles, wet processing method, direct reinforcement fabrication technology powder preimpregnation, filament winding, and film stacking (Panamoottil et al. 2013; Gao 340 341 342 343 344 345 346 347 348 349 350 351 352 353 354 355 356 357 358 359 360 361 362 366 367 368 369 370 371 372 373 374 375 PR OO 339 D 338 TE 337 EC 336 OR R 335 F 363 solvents into the network. This, in turn, forms a large amount of entanglements between CNTs and the polymer molecular chains (Zhang 2011; Pei et al. 2011). CNT-filled with polyamide could be fabricated via the wet casting technique (Tang et al. 2010a, b; Lu et al. 2011; Ribeiro et al. 2012a, b). In this case, both CNTs and polyimide matrices are soluble in certain organic solvents; allow close mixing of solutions, and subsequent fabrication of the composites (Lu et al. 2011). Moreover, in situ polymerization, with the dispersion of the CNTs, leads to a composite with good electrical, mechanical, optical, and thermal properties (Tang et al. 2010a, b). Furthermore, an effectual solution process (Lu et al. 2011) could prepare the polyimides/MWCNTs nanocomposites. Through this method, the MWCNTs were well dispersed, and their structures remained similar in the final resulting nanocomposites. The electrical conductivity of polyimides is improved by more than 11 orders of magnitudes to 10−4 S cm−1 at the percolation threshold by the addition of 0.15 % vol CNTs (Tsai et al. 2010). Moreover, the nanocomposites containing 10 wt% of MWCNTs resulted in the dielectric constant reaching 60, which are about 17 times of 3.5 for pure polyimide (Thuau et al. 2009). The electrical resistivity of the nanocomposites surface was reduced from 1.28 × 1015 ohm cm−2 for neat polyimide, to 7.5 × 106 ohm cm−2 by the addition of 6.98 wt% of MWCNTs (Myung et al. 2010; Sun et al. 2008). The frequency behavior of specific admittance of 0.05 vol% of CNTs-filled polyimides composites determined that its conductivity properties follow a percolation-like power law, with a comparatively low percolation threshold (Tzeng et al. 2008; Guo et al. 2009; Zha et al. 2013). The measurement of the current-voltage demonstrated that the composites displayed a nonohmic behavior, representing a quantum tunneling conduction procedure (Itoh et al. 2008). Thus, it is concluded that the conductivity of the composites results from the formation of conducting pathways to the polyimides by CNTs (Bong et al. 2006; Yang et al. 2007; Kim et al. 2007; Li and Bai 2011). Therefore, based on the concentration of CNTs, it is possible to modify the conductivity of the composite (Shigeta et al. 2006; Ogasawara et al. 2004). 334 UN C Author Proof 14 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 15/61 Time: 2:52 pm 15 384 CNTs: In Polyacrylic/Polymethylacrylic Polymeric Composites 385 Studies using melt-processed CNTs-filled polymethylmethacrylate polymer composites have been quite limited. The particular inclination of CNTs to form agglomerates may be minimized by the suitable application of shear throughout melt mixing (Chen and Lin 2010; Nie et al. 2012). Therefore, some studies applied a combined solvent casting and melt processing to produce polymethylmethacrylate-containing SWCNTs. They press little pieces of cast films between warm plates, and subsequently breaking the resulting film all over again into little pieces, and repeated the process many times (Nie et al. 2012). The particular film acquired by this melt processing technique had more homogenous CNTs distribution than the cast film, and led to superior mechanical properties. Other studies used a miniature mixer-molder to produce small quantities (approximately 0.4 g) of welldispersed mixtures of the CNTs in polymethylmethacrylate. The well-dispersed mixture was then compressed into thin films for the purpose of investigating the dynamic mechanical properties, with a significant improvement in storage modulus (Vicente et al. 2009). It has also been recorded that CNT-filled polyacrylic acid composite film generated by the electrophoretic deposition technique in polyacrylic acid solution is utilized as electrodes for capacitive deionization (Antolin-Ceron et al. 2008). In this case, polyacrylic acid serves as the matrix to incorporate CNTs and cation-exchange polymer. The unit cell, according to the CNT-filled polyacrylic acid composite film electrode demonstrated an 83 % NaCl removal, with excellent regeneration ability, meaning that it is 51 % higher than the cell based on pure CNTs electrodes (Chen and Lin 2010). Furthermore, binary CNT-filled polyacrylic composite system was introduced in the belief that a miscible polyacrylic blends attract host materials where CNTs could be inserted, since this kind of mixtures has a degree of mixing down to the molecular level (Nie et al. 2012). For example, CNTs contain composite materials films, which were obtained after evaporating the solvent used to prepare solutions of the four types of binary polymer blends of poly[ethylene-co-(acrylic acid)]. The evidence of H-bond formation was verified for the composite materials (AntolinCeron et al. 2008). The Young’s moduli and crystallinity of the CNTs-filled poly [ethylene-co-(acrylic acid)] composites were improved compared to single polyacrylic. 382 386 387 388 389 390 391 392 393 394 395 396 397 398 399 400 401 402 403 404 405 406 407 408 409 410 411 412 413 414 415 416 PR OO 381 D 380 TE 379 EC 378 OR R 377 F 383 et al. 2013; Huang et al. 2013). The processing of CNT-filled thermoplastic leads to different mechanisms of residual stress formation, especially crystallization shrinkage in semicrystalline thermoplastics (Gao et al. 2013). This great impact resistance and large volume production potential make CNT-filled thermoplastic composites attractive as structural materials in ground and rail vehicles, mass transit, aircraft, and military structures. They have outstanding potential to preserve the integrity in case of impact, due to their catastrophic failure resistance (Huang et al. 2013). 376 UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 16/61 Time: 2:52 pm N.M. Julkapli et al. CNTs: In Polyethylene Polymeric Composites 418 448 Currently, polyethylene, as high-strength matrix composites, is widely used for protective systems, due to its flexibility, high Young’s Modulus, good impact resistance, and lightness (Pollanen et al. 2011; Raja et al. 2013a, b; Maizatulnisa et al. 2013; Sedláková et al. 2014a, b). It is reported that CNT-filled polyethylene composites enhance dynamic stab-resistance compared with plain polyethylene (Haznedar et al. 2013; Ma et al. 2014a, b). During mechanical testing, polyethylene maintains the position and orientation of the CNTs and distributed the load due to the impact among CNT fillers (Kanagaraj et al. 2011; Sulong and Park 2011; Yesil and Bayram 2011). In this case, the weak CNT-to-polyethylene adhesion is required to allow the composite to undergo maximum deformation. Polyethylene also protects the CNTs from environmental factors, such as decreased impact resistance under conditions of high humidity and the decrease of mechanical behaviour due to the photocatalytic degradation caused by ultraviolet radiations (Kim et al. 2010; Mehta et al. 2011; Sulong et al. 2011). Certain studies focused on the impact of CNT’s diameter and temperature on the interaction energy of CNT-filled polyethylene composites; and at low temperatures, a large radius CNT displays the toughest interaction energy with the polyethylene matrix (Hida et al. 2012; Ibrahim et al. 2012; Xie et al. 2013; Hao et al. 2013). Additionally, the studies also indicated a direct relationship between interaction energy and mechanical properties, which render CNT-filled polyethylene a promising candidate for ultra-strong lightweight materials. Meanwhile, some reports focused on the temperature-dependent electrical behaviour of MWCNTs/high density polyethylene (HDPE) composites prepared by solution precipitation. The electrical intensity for MWNT/HDPE composites can reach 104 by 5.4 wt% loading of MWCNTs (Ibrahim et al. 2012). Furthermore, the addition of neat CNTs improved the gas permeability properties of the polyethylene composites (Xie et al. 2013). For example, in the composite membranes, organic vapour are much more permeable than permanent gases, permeability of hexane and toluene is higher about two orders of magnitude than permanent gas permeability (Mhlanga et al. 2013a, b; Zhao et al. 2013; Li et al. 2013a, b, c, d, e). The CNT-filled polyethylene membranes results offer perspectives for vapor/gas separation applications. 449 CNTs: In Polypropylene Polymeric Composites 450 Surface properties of CNTs induce chemical interactions between CNTs and polypropylene, which in turn improve the mechanical behaviour of the composites (Girei et al. 2012; Pascual et al. 2012; Kim et al. 2013a, b, c). With that in mind, the interface between CNTs and polypropylene was simulated using contact elements. It is recorded that the length of CNTs significantly affects the reinforcement phenomenon of the polypropylene composites (Sulong et al. 2013; Wu et al. 2013a, b, c). Indeed, to increase the surface properties of CNT-filled polypropylene composites, some studies focused on the surface functionalization of CNTs. For 424 425 426 427 428 429 430 431 432 433 434 435 436 437 438 439 440 441 442 443 444 445 446 447 451 452 453 454 455 456 457 PR OO 423 D 422 TE 421 EC 420 OR R 419 F 417 UN C Author Proof 16 AQ1 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 17/61 Time: 2:52 pm 17 D PR OO F Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … 460 461 462 463 464 465 466 467 468 469 470 471 472 473 474 475 example, butyllithium, which is functionalized by MWCNTs, developed in a manner that can covalently bond to chlorinated polypropylene (Yazdani-Pedram et al. 2013). By adding 0.6 vol% MWCNTs, the modulus improved by three orders of magnitude, and both toughness and tensile strength were enhanced by 4 times (from 27 to 108 J g−1), and 3.8 times (from 13 to 49 MPa), respectively (Zhou et al. 2012). The micrograph on the break surface showed that while CNTs have been pulled out from the polypropylene matrix, its outer wall remained in the polypropylene matrix (Fig. 4). Moreover, the polypropylene’s percolation threshold reinforced CNT composites being prepared by diluting a master batch with different kinds of polypropylene, varying from 1.1 to 2.0 vol%. Only poor van der Waals forces are present between the different concentric tubes of MWCNTs; whereas, the outer tubes are covalently attached to the polypropylene matrix (Georgiev et al. 2011; Pötschke et al. 2011; Ma et al. 2014a, b). Furthermore, better CNT-filled polypropylene composite system was obtained by ultrasonic treatment, demonstrating superior storage modulus, viscosity, electrical, and mechanical properties (Yang et al. 2013; Zhang et al. 2014; Huang et al. 2014a, b, c). The lower fractal dimension of CNT and higher backbone fractal dimension result in comparatively better dispersions (Zhong et al. 2014). OR R 459 UN C 458 EC TE Fig. 4 TEM images of nanotube–polymer composites which show the buckled CNTs. The ends of the nanotubes, embedded in the polymer matrix. a Buckled nanotube bridging a micro-crack in the composite. b A close up of a buckled region which indicates the narrowing of the inner diameter and the arrow shows the change the inter-shell spacing. c CNTs with thin walls where single buckles were typical. d A buckled nanotube with 18 % tensile strain in the outer wall. e A fractured CNT (Bower et al. 1999) Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 18/61 Time: 2:52 pm N.M. Julkapli et al. CNTs: In Polystyrene Polymeric Composites 477 494 The MWCNT-filled polystyrene nanocomposites were prepared by solution evaporation method after sonication. By adding 1 wt% of MWCNTs to polystyrene, the elastic modulus and break stress increased by 36–42 and 25 %, respectively. The verification of the external load transfers to nanotubes was efficiently achieved by tensile tests and in situ transmission electron microscopy, showing that nucleation of cracks takes place at low-density area of CNTs, and after that, propagates along the poor CNT-polystyrene interfaces or relatively low CNT density regions (Kumar Sachdev et al. 2013; Tang et al. 2014). When the crack dimension exceeds 800 nm, CNTs start to break and/or even remove itself from the polystyrene matrix. Increased CNT concentrations result in a significant decrease in both tensile strength and elongation at break. Furthermore, with excess content of CNTs, decrease in fluidity with increasing CNT loading becomes an impediment to the formation of a uniform microstructure (Suemori et al. 2013). The super hydrophobic aligned layer of polystyrene nanotubes layer showed strong adhesion to water (Tang et al. 2014). This, in turn, disclosed the fact that aligned CNTs structure could not only improve hydrophobicity, but also give rise to a high adhesion force. The CNTs incorporated into the polystyrene matrix are applicable to the tire industry (Kumar Sachdev et al. 2013). 495 CNTs: In Polyvinyl Chloride Polymeric Composites 496 The effective application of CNTs in polyvinyl chloride is based on the improvement of electrical conductivity and mechanical properties, and its capability of dispersing homogeneously in the polyvinyl chloride matrix (Suemori et al. 2013). However, homogenous dispersion of CNTs is difficult due to the van der Waals interactions between the CNTS, consequently leading to the formation of agglomerations (Song et al. 2013). In this respect, the melt-mixing method is the preferred method of fabricating CNT-filled polyvinyl chloride (Farsheh et al. 2011; Aljaafari et al. 2012). The MWCNT-filled polyvinyl chloride mixed matrix membrane is suitable for gas separation applications, as well as an indicator electrode in potentiometric titrations (Abu-Abdeen 2012). In addition, it was determined that the dispersion of CNTs and morphology changes from CNT breakages are closely related to the electrical conductivity of the composites (Suemori et al. 2013). Therefore, a large morphological change in CNTs occurs at a specific processing time, and a significant decrease in the electrical conductivity of polyvinyl chloride was reinforced by CNT composites (Song et al. 2013). For example, a meaningful increase of electrical and mechanical properties was observed in the composites with about 1–2 wt% CNT contents sintered at 200 °C after being milled for 20 min (Mamunya et al. 2008). The actual concentration dependence of the thermophysical and electrical behaviour of composites depends on polyvinyl chloride filled with MWCNTs discovered that the great anisotropy of the MWCNTs and the actual presence 483 484 485 486 487 488 489 490 491 492 493 497 498 499 500 501 502 503 504 505 506 507 508 509 510 511 512 513 514 515 516 PR OO 482 D 481 TE 480 EC 479 OR R 478 F 476 UN C Author Proof 18 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 19/61 Time: 2:52 pm 19 535 3.1.3 CNTs: In Elastomer Polymeric Composites 523 524 525 526 527 528 529 530 531 532 533 536 537 538 539 540 541 542 543 544 545 546 547 548 549 550 551 552 553 554 555 PR OO 522 D 521 TE 520 The introduction of CNTs to the collection of possible fillers provides new opportunities to tailor the behavior of elastomers through blending with comparatively small volume fractions of CNTs. These kinds of enhancements rely on good alignment and dispersion of the CNTs and excellent bonding of composite components (Sementsov et al. 2010; Raja et al. 2013a, b). Issues with bonding and alignment might be good for optimally improving the composites behavior which could possibly be detrimental to improving elastomeric mechanical properties (Singha and Thakur 2008a, b, c, d; Shi et al. 2013). Generally, the applications of elastomeric need the significant deformation extensibility and resilience of the elastomer. After incorporation of CNTs, as highly rigid fillers in elastomers, it typically needs to improve the stiffness of overall large-strain deformation behavior of composites (Cadambi and Ghassemieh 2012). Besides, this approach is likewise maintaining the key features of large strain-to-break behavior as well as large strain resilient of composites. Additionally, if stiffness improvement mainly consequences from unbending of the waviness of CNTs as opposed to axial straining of the CNTs, depends on good bonding and shear lag load transfer from the elastomer to the CNTs, the stiffness improvement will not be lost with large strains (Le et al. 2014). EC 519 OR R 518 F 534 associated with segregated structure of MWCNTs within the polyvinyl chloride permitted the attainment of very low value of the electrical percolation threshold of 0.00047 (Zhou et al. 2010). The improvement of thermal conductivity in CNTs volume content was attained following a minimum value. Thus, the addition of CNTs influenced the heat flow through the composite (Aljaafari et al. 2012). The experimental values obtained for poly(vinyl chloride)/CNT composites were utilized to estimate the thermal conductivity of the CNT fillers (Suemori et al. 2013). Furthermore, the addition of CNT affected the thermal properties of polyvinyl chloride. The suspension polyvinyl chloride and the MWCNTs within the concentration range of 0.01 and 0.05 wt% resulted in a lower glass transition temperatures, and an obvious relationship between the frequency, CNT content, and the glass transition temperature was determined (Sterzynski et al. 2010; Jin and Matuana 2010). By increasing the charging frequency, the glass transition temperature improved by about 3 °C via frequencies f = 1 Hz and f = 10 Hz, and 9 °C by f = 1000 Hz, respectively (Sterzynski et al. 2010). The maximum glass transition temperature was realized when the CNT concentrations are at 0.01–0.02 wt%. This might be due to the multiple response of CNTs distribution on the temperaturedependent chain mobility of polyvinyl chloride (Jin and Matuana 2010). 517 UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … CNTs: In Polyisoprene Polymeric Composites Currently, the polyisoprene vulcanized offers many attributes of great interest at a technological perspective, included damping, mechanical, age and heat resistance, Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 20/61 Time: 2:52 pm N.M. Julkapli et al. 578 CNTs: In Polybutadiene Polymeric Composites 579 Elastomer polybutadiene copolymers composed of different ratios of styrene and butadiene, influencing strongly their macroscopic properties. The polybutadiene composites using CNTs show higher enhancement in the electrical properties that can interrelate within the framework of percolation theory (Zhou et al. 2005). The electrical percolation for polybutadiene often observed in the greater CNTs content around between 2 and 14 wt% (Speltini et al. 2013). The application range of polybutadiene once suitably reinforced with CNTs can extend to a variety of products such as sensors/actuators, materials with electromagnetic shielding properties, vapor and infrared sensor, and capacitors. In advanced approach, the CNT is incorporated to a 50:50 blend of styrene– butadiene rubber and butadiene rubber solution (Das et al. 2008; Mari and Schaller 2009; Yu et al. 2011). The predispersed CNTs in ethanol is formed and after that the CNT-alcohol suspension is mixed with the polybutadiene at elevated temperature. CNTs-filled polybutadiene nanocomposites prepared by a technique which show meaningfully improved physical behavior already at very low concentrations of the CNTs (Mari and Schaller 2009). The particular high ratio of the CNTs enabled the formation of a conductive percolating network in the composites at concentrations lower than 2 wt%. By the presence of CNTs, as opposed to the electrical conduction properties, the thermal conductivity of the composites not 562 563 564 565 566 567 568 569 570 571 572 573 574 575 576 580 581 582 583 584 585 586 587 588 589 590 591 592 593 594 595 596 597 PR OO 561 D 560 TE 559 EC 558 OR R 557 F 577 dynamic fatigue resistance, compression set, low temperature flexibility, electrical and swelling resistance properties (Galimberti et al. 2013). The addition of CNTs as filler achieved the level and range of properties in polyisoprene to offer a suitable amount of reinforcement such as tear resistance, tensile strength, and abrasion resistance. To have a high degree of reinforcement, the quantity of CNTs filler loading has elevated significantly which is difficult to improve these types of attributes in order to same optimal level (Yu et al. 2012). In advance, vulcanization of CNTs-filled polyisoprene composites transforms predominantly the polyisoprene into elastic or hard Ebonite-like state. This procedure is termed as curing or “crosslinking.” It involved the association of macromolecules through the reactive sites. In addition, in irradiated CNTs-filled polyisoprene composites by powerful radiation, H2 atoms of the chain, chiefly groups of methylene proportional to double bonds are ejected and radical sites are formed and combined into C–C cross-links. However, the radiation cross-linking efficiency of polyisoprene is insignificant, because of the loose packing of polyisoprene molecules with the cis structure and the groups of methyl (Yu et al. 2013a, b). Polyisoprene is known to form carbon–carbon cross-links under pressure at controllable process parameters. The results of the cross-linking and inclusion of CNTs into polyisoprene studied by in situ thermal conductivity and tensile test revealed that Polyisoprene reinforced MWCNTs composite showed an increment in stiffness with growing MWCNTs content, retained stiffness to large strains, but with the increase in MWCNTs content the failure strains decreased (Yu et al. 2013a, b). 556 UN C Author Proof 20 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 21/61 Time: 2:52 pm 21 603 CNTs: In Nitrile Rubber Polymeric Composites 604 The nitrile butadiene rubber is a random copolymer of acrylonitrile and butadiene. Melt mixing of nitrile rubber with CNTs is described using a two-step process; internal mixer and two-roll mild which fond a powerful dependency of the surface resistivity of the composites on processing parameters (Perez et al. 2009; Likozar 2010; Boonbumrung et al. 2013). The CNTs-filled nitrile rubber composites were prepared by blending in a two-roll mill. The CNTs dispersion in nitrile rubber regularly began with treatment of CNTs in organic solvent ultrasonically; included toluene and ethanol followed by adding of the ethanol dispersion to the nitrile rubber compounds. In this case, it should be consider that beside the homogeneous dispersion of the CNTs in the nitrile rubber matrix, the vulcanization might have a significant effect on the final composite properties (Likozar 2010). For the filler network developed by the CNTs above, the percolation threshold will probably be interpenetrating the network of cross-linked nitrile rubber (Perez et al. 2009) (Figure 5). Undoubtedly, it is represented as a good potential for the conceptualization of CNTs-filled nitrile rubber for many reasons included, nitrile rubber degradation process occurred meanwhile the melt mixing procedure results in the formation of free-radicals on chains of polymer (Fang et al. 2011). This, in turn, increases the 607 608 609 610 611 612 613 614 615 616 617 618 619 620 621 PR OO 606 D 605 TE 601 EC 600 OR R 599 F 602 influenced meaningfully. The dynamic mechanical analysis designates that the CNTs incorporation affects the glass transition (Tg) behavior of polybutadiene by reducing the height of the tan δ peak significantly (Yu et al. 2011). As mentioned earlier Tg the storage modulus has been improved after incorporating a small amount of CNTs (Das et al. 2008). 598 UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … Fig. 5 Schematic description of CNT/polymer composites, which prepare by using nitrile rubber technology Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 22/61 Time: 2:52 pm N.M. Julkapli et al. 634 CNTs: In Silicon Rubber Polymeric Composites 635 648 Silicone rubber-based material owns great mechanical elasticity as it certainly has 100 % tensile strain without showing any structural failure. The study on silicone rubber elastomers filled with SWCNTs shows a remarkable improvement in preliminary stiffness with small fractions of SWCNTs (Liu et al. 2013a, b, c). Though the improvement in stiffness is lost after just 10–20 % strain where the tangent stiffness of the nanocomposites returns to that of the parent elastomer because of debonding of the CNTs from the silicon matrix; the tensile strain-to-break found to decline meaningfully with growth in volume fraction of the CNTs (Li et al. 2011; Zhang et al. 2011). Furthermore, introduction of infra red light assisted the actuating mechanism of the silicon rubber (Tarawneh and Ahmad 2012). The actuating aspect of the mechanical properties contributed to the resilient and reversible behavior required for a superior candidate of improving the mechanical behavior of silicon rubber by means of incorporation of small amount of CNTs (Tarawneh and Ahmad 2012). 649 CNTs: In Polyurethane Polymeric Composites 650 Elastomer polyurethanes are multiblock copolymers keeping the common replicate unit structure (AmBn)p (Liu et al. 2013a, b, c; Gupta et al. 2013; Yu et al. 2013a, b; Gu et al. 2014). As a result of modifications within the individual block features, including the chemical identity and molecular weight; polyurethanes fabricate to be soft or hard (Raja et al. 2014; Jiang et al. 2014a, b). The CNTs-filled polyurethane composites fabricated either via melt mixing, dispersion of CNTs in the solvent, and the dissolution of the polyurethane in the same solvent, followed by solvent evaporation or the reaction of the monomers or pre-polyurethane in the presence of dispersed CNTs (Gupta et al. 2013; Liu et al. 2013a, b, c). The former has not been tried; most probably due to weakly melting material has less tendency to disperse CNTs, since the latter technique is only industrially practical (Fonseca et al. 2013; 628 629 630 631 632 636 637 638 639 640 641 642 643 644 645 646 647 651 652 653 654 655 656 657 658 659 660 PR OO 627 D 626 TE 625 EC 624 OR R 623 F 633 affinity between acrylonitrile and CNTs components, which consequently give no important effect of poisoning by CNTs on vulcanization procedure. It is highlighted that, degradation process of polymer in terms of thermo-oxidative and/or thermomechanical happens during the melt blending results in the covalent grafting nitrile runner on the surface of CNTs (Verge et al. 2010). For example, the stiffness of the nitrile rubber matrix increases the use of CNTs as filler that has a large specific surface area. This is due to the large surface area to a more developed CNTs–CNTs networks, which in consequence generate strong hysteresis under dynamic operating conditions (Yue et al. 2006). The stiffness also imparted by a certain mass of CNTs and clearly observed once the CNTs aggregates. This effect attributed to the hydrodynamic effect, which is an analog to the effects of CNTs on the viscosity of the nitrile rubber (Perez et al. 2009). 622 UN C Author Proof 22 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 23/61 Time: 2:52 pm 23 673 3.2 CNTs: In Biopolymer System 667 668 669 670 671 674 675 676 677 678 679 680 681 682 683 684 685 686 687 688 689 690 691 692 693 694 695 696 697 698 PR OO 666 D 665 Different types of biopolymers-based materials have been used in a number of applications either as the polymer matrix or as the reinforcement due to their enormous advantages (Thakur and Thakur 2014a, b, c; Thakur et al. 2014c, d, e, f). The biopolymer or biodegradable plastics are polymeric materials which degrade in one-step through metabolism of the organism occuring naturally (Parvinzadeh et al. 2013; Singha and Thakur 2008a, b, c, d). In suitable temperature, O2 availability, and moisture, biodegradation of polymer is induced into disintegration or fragmentation with no toxicity. Generally, biopolymer is divided into three main categories as listed in Fig. 6. However, most of the biopolymers-based materials show relatively weak barrier and mechanical behavior, which presently limit their industrial utilization for the targeted applications (Zhang et al. 2012; Yang et al. 2014; Thakur et al. 2010a, b). In particular, low-heat distortion temperature, brittleness, high vapor and gas permeability, weak resistance to protected processing operation have powerfully limit its applications (Singha and Thakur 2009a, b, c, d, e; Alimohammadi et al. 2013). Thus, biopolymers have been filled with CNTs nanoparticles for improving their required properties, whereas retaining the biodegradability in a reasonably economic ways. The incorporation of CNTs into the biopolymer system is achieved predominantly by adsorption and/or chemical binding. An ideal method should assist the interactions of the biopolymer toward CNTs within its environment. TE 664 EC 663 OR R 662 F 672 Zheng et al. 2013). The latter technique accustomed to generate MWCNTs-filled polyurethane composites. In this attempt, isophorone diisocyanate in an organic solvent reacted with poly(tetramethylene oxide, after that this mixture emulsified in H2O, and dispersed CNTs added. The ethylenediamine just added as a chain extender to react with the terminal groups of isocyanate (Gurunathan et al. 2013; Loos et al. 2013a, b; Tijing et al. 2013). As an indicative of an excellent CNTs dispersion, the percolation threshold is extremely low, approximately 0.1 wt% (Loos et al. 2013a, b). In a comparable approach, the CNTs dispersed in the liquid soft segment, and after that in a single step the reaction is completed (Yu and Li 2012; Yan et al. 2012). This mixture is added at one time to the methylene diisocyanate, isocyanate, and chain extender, 1,4-butanediol (Wu et al. 2012; Raja et al. 2011). 661 UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … 3.2.1 CNTs: In Cellulose Polymeric Composites The CNTs-filled cellulose nanocomposites prepared with various fabrication techniques included phase inversion, vacuum filtration, and flash freezing (Li et al. 2013a, b, c, d, e; Qi et al. 2013a, b, c; El Badawi et al. 2014). The CNTs-filled Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 24/61 Time: 2:52 pm N.M. Julkapli et al. TE D PR OO F Author Proof 24 Fig. 6 Categories of biopolymer based on the origin of raw materials and their manufacturing process 702 703 704 705 706 707 708 709 710 711 712 713 714 715 716 717 718 719 EC 701 cellulose nanocomposites membrane are prepared by phase inversion using acetone as solvent and 20 wt% deionized water as nonsolvent. It revealed that permeation rate found to improve by 54 % with a minimal decrease in salt retention (6 %) for the membrane with only 0.01 wt% of CNTs (Callone et al. 2008). Further addition of CNTs caused a reduction in permeation rate, which attributed to the decreased porosity and surface area (Nadagouda and Varma 2008). Another fabrication of CNTs-filled cellulose composites is done by the flash freezing and lyophilization process using wet-gel precursors. The fabricated composites exhibited both a nanostructured solid network with specific surface area between 140 and 160 m2 g−1 and nanoporous network (Fugetsu et al. 2008). The Young’s modulus of the composites tuned to reach 90 MPa with conductivity about 2.3 × 10−4 to 2.2 × 10−2 S cm−1 (Loos and Manas-Zloczower 2013). In consequence, composite materials consisting of CNTs combined with cellulose paper have developed, and found that the composite is able of shielding electromagnetic interference over the examined range of 15–40 GHz, mainly in the range of 30–40 GHz, with absorption as the critical shielding mechanism (Wang et al. 2012; Won et al. 2013). It is also found in other studies that both normal flexible paper and conducting CNTs demonstrated in the composite systems with a controllable volume resistivity within a range of 1.35–540 Ohm cm (Tanaka et al. 2013). It is also documented that the composites are physically strong and yet highly flexible (Wang et al. 2012). Approximately 10 wt% CNT is needed to attain composite paper with 20-dB far-field EMI SE. In OR R 700 UN C 699 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 25/61 Time: 2:52 pm 25 739 3.2.2 CNTs: In Chitosan Polymeric Composites 740 Chitosan is the only cationic biopolymer that has the solution sensitivity of positive charged NH2 groups in its molecular chains (Yu et al. 2014). Thus, it possesses beneficial properties included biodegradability, biocompatibility, and adsorption capacity (Shawky et al. 2012; Nitayaphat and Jintakosol 2014; Popuri et al. 2014). It has many vital biological applications in immunity, tissue engineering, catalyst support, permeable membranes, biological carrier, and drug delivery. In addition, besides excellent electrical and mechanical properties, CNTs have described to be biocompatible with chitosan matrix (Popuri et al. 2014). When compared to chitosan, the composites composed of 2 wt% MWCNTs show more doubled Young’s modulus and tensile strength (Shin et al. 2006). The micrograph analysis shows that the produced composites have a three-dimensional network with lamellar structure and macrospores (Spinks et al. 2006). This makes CNTs-filled chitosan composites as suitable candidates for the well-defined microchannel porous structure, biodegradable and biocompatible support for culture growth (Wu and Yan 2013). It is recorded that the composites have a promising adsorption properties (Salehi et al. 2012). Thus, the composite systems could offer exclusive properties as a composite in removal of heavy metal ions and treatment of wastewater (Zheng et al. 2008; Lu et al. 2009). For example, the maximum adsorption capacity 0.393 mg g−1 of silver ions (Ag+) adsorbed only 0.01 wt% of CNTs in chitosan composites. It is also found that the maximum monolayer adsorption of copper ions (Cu2+) of CNTsfilled chitosan composites recorded at 454.55 mg g−1 (Zheng et al. 2008). Modulated release of dexamethasone from CNTs-filled chitosan recorded to be faster than 726 727 728 729 730 731 732 733 734 735 736 737 741 742 743 744 745 746 747 748 749 750 751 752 753 754 755 756 757 758 759 760 761 PR OO 725 D 724 TE 723 EC 722 OR R 721 F 738 another case, the composite electrodes generated by CNTs vacuum filtration, followed by rebuilding of cellulose dissolved 1-ethyl-3-methylimidazolium acetate, which is an ionic liquid, for the oxidation process of glucose oxide (Qi et al. 2013a, b, c; Kim et al. 2013a, b, c). The result shows that direct electron transfer between glucose oxide and composite electrodes is achieved. It is also found that the glucose oxide immobilized on the composite electrodes retained catalytic oxidation of the glucose (Qi et al. 2013a, b, c). A similar result is obtained using bacterial cellulose as a matrix for the CNTs filler; it revealed that ultra-strong, transparent, and highly conductive CNTs-filled bacterial cellulose is obtained with a good biocompatibility for direct electron transfer to glucose oxide (Kim et al. 2013a, b, c). The electrical conductive properties of CNTs-filled cellulose also used as a water sensor. The composites demonstrated high sensitivity and fast response with an electrical resistance change of 5500–500 % with CNTs loading up to 2–10 wt% (Koga et al. 2013). Thus, CNTs/cellulose composite systems have high potential to use in H2O/ CH2OH solution fraction process. In another study, a good alignment and dispersion of MWCNTs in cellulose is attained by dissolution in an ionic liquid and subsequent grinding and spinning (Lin et al. 2011a, b, c; Peng et al. 2013). This simple technique of preparing regenerated-cellulose/MWCNTs composite fibers can result in the carbon fibers production from a renewable resource (Peng et al. 2013). 720 UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 26/61 Time: 2:52 pm N.M. Julkapli et al. 770 3.2.3 CNTs: In Collagen Polymeric Composites 771 Incorporation of CNTs into the collagen matrix leads to a considerable improvement of mechanical behavior, thermal stability, and infrared emissivity (Roy et al. 2010; Ribeiro et al. 2012a, b; Mao et al. 2014). The choice of CNTs for reinforcement of collagen has motivated by two considerations. First, according the viscoelastic and calorimetric analysis, collagen is thermodynamically immiscible, thus it is a promising matrix to wrap the CNTs surface (Roy et al. 2010). Second, the probable worthy adhesion between collagen and CNTs combined with the selfassembly capabilities of collagen can result in the alignment of CNTs in the polymer matrix, improving the mechanical behavior at low loading level (PourAkbar Saffar et al. 2009). Besides, CNTs are striking for being used in fillerreinforced composite materials because of their high aspect ratio, combined with good electrical properties. Thus, this material possesses potential applications in some fields such as biomedicine, biosensor, medical devices, tissue engineering, and substrates for electrical stimulation of cells, transducers, and infrared camouflage (Mao et al. 2014). Most probably, the composites materials including the collagen matrix with implanted CNT are prepared by blending solubilized and polymerization (Cho and Borgens 2010). It is shown that the mixture of SWCNTs with collagen supports smooth muscle cell growth; with mouse fibroblast has effectively grown on CNTs (Lee et al. 2010). Furthermore, constructs containing 201 wt% CNTs demonstrated delayed gel compaction, relative to lower concentrations that compacted at the same rate as pure collagen control (Boccaccini and Gerhardt 2010). Under the micrograph analysis, the collagen/CNTs composites formed rigid fibril bundles, which polarized the growth and differentiation of human embryonic stem cell. The conductivity of collagen increased uniformly with increasing CNTs content from 0.8 to 4.0 wt% and displayed modest frequency dependence, suggesting that the electrical percolation threshold had not been reached in the CNTs-filled collagen composites (Cho and Borgens 2010). Furthermore, there is some report on the improvement of the mechanical behavior of SWCNTs-filled collagen composites. It is found that a dramatic toughness (700 %), Young modulus (260 %), tensile strength (300 %) could expect with the classical rule of mixture between CNTs and collagen matrix (Chahine et al. 2008). 768 772 773 774 775 776 777 778 779 780 781 782 783 784 785 786 787 788 789 790 791 792 793 794 795 796 797 798 799 800 801 802 PR OO 767 D 766 TE 765 EC 764 OR R 763 F 769 unfilled chitosan film. In this case, the produced composites have very low selfstanding ability and density that makes it having a very worthy penetrability and process ability (Babaei and Babazadeh 2011). The CNTs-filled chitosan composites did not cause significant cytotoxic effects on the tissue culture plate. Thus, manipulation of CNTs/chitosan composites gave a positive signal for scaffold and living cell applications (Sahithi et al. 2010; Takahashi et al. 2009). However, at high densities, the CNTs in chitosan composites might exert inhibitory effects by inducing apoptosis (Takahashi et al. 2009). 762 UN C Author Proof 26 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 27/61 Time: 2:52 pm 27 4 Functionalized CNTs: In Polymeric System F 803 829 4.1 CNTs: Covalent Functionalization 809 810 811 812 813 814 815 816 817 818 819 820 821 822 823 824 825 826 827 830 831 832 833 834 835 836 837 838 839 840 841 D 808 TE 807 EC 806 OR R 805 PR OO 828 In principle, the outer wall of pristine CNTs conceived as chemically inert. However, this is not always desirable for applications in polymeric composite systems. Indeed, the surface energy of CNTs significantly different form that of the polymer matrices thus makes CNTs may not have chemical affinity to organic matrices (Song et al. 2010; Ntim et al. 2011). Therefore, the dispersion of CNTs into matrices becomes the biggest obstacle in practice. In addition, the seamless surface of CNTs cannot provide physical interaction within the interface of CNTs and polymer matrices (Abe et al. 2011a, b; Kotchey et al. 2013). The nature of the dispersion problem for CNTs is different from other conventional filler (Song et al. 2010). This is due to its small diameter in nanometer scale with high aspect ratio and thus possessing large surface area (Vijay et al. 2011; Abe et al. 2011a, b). A typical molecular dynamic stimulation theoretically attributed the aggregation of CNTs to the solvation interaction causes the H atoms of H2O molecules point to the surface of CNTs. This leads to greater interaction of H2O molecules around CNT surface than in the bulk H2O. The orientated H2O molecules give rise to the energy of those molecules around CNTs and force CNTs aggregate into bundles to minimize the system energy rise (Lei and Ju 2010). Indeed, the commercialized CNTs supplied in the form of heavily entangled bundles, resulting in inherent difficulties in dispersion. For this reason, further modifications on properties of CNTs in a controlled manner through several functionalization routes have thought to make the CNTs chemically active. For example, amine functionalized CNTs is completely dispersed in the polymer matrix in comparison to unmodified CNTs. The functionalization can mean in lattice doping, intercalation, molecule/particle adsorption, encapsulation, or even other nonexplored modifications (Lei and Ju 2010; Prajapati et al. 2011). 804 One of the major obstacles in the processing of CNTs is their inherent poor solubility in organic and aqueous solvents. It is thought that the formation of covalent links significantly multiplies the solubility of CNTs in a variety of solvents at the same time assures the structural integrity of the CNTs skeleton. This, consecutively, modifies the intrinsic physical properties and polydispersity of the CNTs caused by the modification of the sp2 C skeleton. Direct covalent sidewall functionalization is coupled with a change of hybridization from sp2 to sp3 and a simultaneous loss of the p-conjugation system (Wang et al. 2010; Lee et al. 2013). The end caps of CNTs consist of highly curved fullerene-like hemispheres, which are hence highly reactive, when compared with the sidewalls (Wang et al. 2010). Such modification of CNTs together with their low reactivity impedes the chemical functionalization and the characterization of the corresponding reaction products with high-chemical UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 28/61 Time: 2:52 pm N.M. Julkapli et al. 854 4.1.1 CNTs: Carboxylation Functionalization 855 The conventional covalent functionalization strategy of CNTs, most commonly initiated through the carboxylation procedure by chemical acid oxidation treatment including HNO3, H2SO4 or a combination of them. Powerful oxidation agents such as KMnO4, ozone, reactive plasma tend to open the CNTs tubes, and consequently create oxygenated functional groups like COOH, COH, OH, and ester, which function to bind various types of chemical moieties onto the ends and defect location of CNTs. These functional groups have rich chemistry and the CNTs can be used as originators for further chemical reactions, such as silanation and polymer grafting (Battigelli et al. 2013a, b; Liu et al. 2014a, b, c, d, e). For instance, the oxidation of MWCNTs with HNO3/H2O2 and HNO3/H2SO4 leaded into some COOH groups on CNTs, which improved their stability in H2O at room temperature for over 100 days (de Lannoy et al. 2013a, b; Frohlich et al. 2013; Li et al. 2013a, b, c, d, e). Consequently, the water-stable CNTs easily embedded in watersoluble polymer contained poly(vinyl alcohol), providing CNTs-filled polymer composites the homogeneous dispersion of CNTs. Oxidized CNTs well show an exceptional stability in other solvents including caprolactam, which is applied in the production of polyamide (Frohlich et al. 2013). Study on carboxylation of CNTs has shown a considerable enhancement in interfacial bonding between CNTs and polymer matrices, which consecutively triggered stronger CNTs-polymer interaction, leading to improvement of Young’s modulus and mechanical strength (Hashimi et al. 2012; Shi et al. 2009). Conversely, dramatic amounts of induced defects throughout functionalization hamper the intrinsic mobility of carriers along CNTs, which is not desirable in any case (Naeimi et al. 2009; Liu et al. 2011; Zhong et al. 2011). The carboxylation technique not only functionalizes the CNTs exterior with COOH groups, but also leaves behind unfavorable structures, thus hampering their potential for practical purposes (Zhong et al. 2011). This in turn compromises the mechanical properties of CNTs. Moreover; the concentrated acids or strong oxidants often used for CNTs functionalization are environmental unfriendly (Liu et al. 2011). 848 849 850 851 852 856 857 858 859 860 861 862 863 864 865 866 867 868 869 870 871 872 873 874 875 876 877 878 879 880 881 882 883 PR OO 847 D 846 TE 845 EC 844 OR R 843 F 853 reactivity (Lee et al. 2013). Further, this covalent bond considerably develops the interfacial contact between matrix and filler that enables a stress (Yi et al. 2010). It is supposed that the solubility of CNTs is enhanced with modification and fine-tune on physical properties of CNTs. The modification is supposed to improve the compatibility between CNTs and the foreign matrix and makes available the direct grafting with little or no structural damage to CNTs available (Lee et al. 2013). Overall, covalent functionalization of CNTs has diverse mechanical and electrical attributes caused by the intervention of the attached moieties and the modification of the structural p-network (Wang et al. 2010). This structural alteration occurred at the termini of the tubes and/or at the sidewalls. Moreover, the direct sidewall functionalization associated with rehybrization of one or more sp2 C atc of C network into a sp3 configuration and concurrent loss of conjugation (Lee et al. 2013). 842 UN C Author Proof 28 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 29/61 Time: 2:52 pm 29 4.1.2 CNTs: Amidation Functionalization 885 898 Polymer molecules can further graft on the surface of CNTs in the presence of NH2 functional groups. This grafting method carried out either by grafting from or grafting to technique (Table 5). Conversely, at some point in the functionalization reaction, chiefly along with the damaging ultrasonic process, a large number of defects unavoidably formed on the CNTs sidewalls (Abe et al. 2011a, b; Singh et al. 2012; Ng and Manickam 2013; Li et al. 2013a, b, c, d, e; Jiang et al. 2013a, b). In some circumstances, CNTs fragmented into smaller chunks and altered the C hybridization from sp2 to sp3 (Singh et al. 2012; Ng and Manickam 2013). These detrimental effects bring about severe degradation in mechanical properties of CNTs besides disruption of π electron system in CNTs (Li et al. 2013a, b, c, d, e). The disruption of H electrons is disadvantageous to transport properties of CNTs caused by the defect sites scattered electrons and photons that are responsible for electrical and thermal conductions of CNTs (Ng and Manickam 2013). 899 4.1.3 CNTs: Halogenation Functionalization 891 892 893 894 895 896 897 900 901 902 903 PR OO 890 D 889 TE 888 The fluorination of CNTs becomes prevalent for early investigation of the covalent functionalization due to the fact that CNTs sidewalls are expected to be inert (Karousis et al. 2010; Li et al. 2012). The fluorinated CNTs have C-F bonds that are easily broken than those in alkyl fluorides, and therefore providing substitution sites EC 887 Table 5 Polymer grafting methods of amidation functionalized CNTs Items Grafting from technique Grafting to technique References Synthesis methods The initial immobilization of NH2 initiators onto the CNTs surface, followed by in-situ polymerization with the formation of polymer molecules attached to CNTs High grafting density Attachment of already functionalized polymer molecules to the functionalized CNTs surface via appropriate chemical reactions Chen and Hseih (2010) High grafting selectivity Commercially available polymers containing reactive groups can be utilized Low product density Jiang et al. (2010) Advantages OR R 886 F 884 UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … Disadvantages Polymer matrix Process needs a strict control of the amounts of initiator and substrate Poly(methyl methacrylate) Poly(n-butyl methacrylate) Poly(ethylene glycol) Poly epoxypolyamidoamine Coto et al. (2011) Jain et al. (2011) and Mases et al. (2011) Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 30/61 Time: 2:52 pm N.M. Julkapli et al. for additional functionalization, successfully replacements of the fluorine atoms by NH2, CH3, and OH groups have been achieved (Xu et al. 2013). 906 4.1.4 CNTs: Acylation Functionalization 907 921 The acylation of CNTs is a hopeful strategy to not only advance its dispersion, but also offer a method for creating microscopic interlinks (Heidari et al. 2013; Saidi 2013; Ye et al. 2011). Overall, acylation of CNTs improves the reactivity, enhances the specificity, and provides an avenue for additional chemical modification of CNTs; Considerable achievements have been made improving various functionalities of CNTs-filled polymer composites, generally not possible for each of the components independently (Saidi 2013). The approach is conceptualized based on CNTs chemistry via direct Friedel-Craft acylation technique, which has higher operational simplicity (Ye et al. 2011). This is not only a mild and a substitute path to functionalize CNTs, this approach also has previously shown to be less-detrimental and/or nondestructive reaction form for the proficient dispersion and functionalization of CNTs (Heidari et al. 2013). Consequently, CNT damage from severe chemical treatments including oxidation and sonication can avoid largely. Hence, greatest improvement in properties can be expected from enhanced dispersion stability on top of a chemical affinity with matrices (Saidi 2013). 922 4.2 CNTs: Noncovalent Functionalization 913 914 915 916 917 918 919 920 923 924 925 926 927 928 929 930 931 932 933 934 935 936 937 938 939 940 941 PR OO 912 D 911 TE 910 EC 909 The suggested application of CNTs in polymeric composite systems has reduced because of their functional insolubility in aqueous and organic solvents (Chen et al. 2013a, b; Wu et al. 2013a, b, c; Yan et al. 2014; Battisti et al. 2014a, b). Because of their high polarizability and flat surface, CNTs, specifically SWCNTs, produced bundles and ropes characteristics (Wu et al. 2013a, b, c). Hence, numerous CNTs line up in parallel to each other through a high van der Waals attraction (0.5 eV mm−1) (Yan et al. 2014). Besides, CNTs obtained as mixtures that demonstrate different chiralities, diameter, and length, in which non-CNTs carbon and metal catalyst represent in the ultimate CNTs product (Battisti et al. 2014a, b). A number of these limitations can be conquered by controlling defect and sidewall functionalization of CNTs. Yet the most prominent effect on this functionalization is that the natural conductivity of the CNTs is destroyed (Werengowska-Ciecwierz et al. 2014). A substitute approach for maintaining the inherent electronic and mechanical characteristics of CNTs is based on the noncovalent or super-molecular alteration of CNTs (Liu et al. 2014a, b, c, d, e). Such interactions, chiefly involve hydrophobic, van der Waals, and electrostatic forces, and necessitate the physical adsorption of suitable molecules onto the sidewalls of the CNTs (Wu et al. 2013a, b, c; Yan et al. 2014). Noncovalent functionalization is attained by polymer wrapping, adsorption of surfactants or small aromatic molecules, and interaction OR R 908 F 905 904 UN C Author Proof 30 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 31/61 Time: 2:52 pm 31 951 4.2.1 Oxidized Functionalization CNTs 952 At the primitive stage, nearly all noncovalent functionalization of CNTs focused on sorting out and dispersing them by chemical oxidation in acidic media, where the acid not only breaks up any residual metal catalyst but also eliminates the CNT caps, leaving behind COOH residue (Yin et al. 2014; Jerez et al. 2014). The oxidized CNTs are easily dispersible in a variety of NH-R organic solvents, under the impact of an ultrasonic force field (Lertrojanachusit et al. 2013; Parveen et al. 2013). In a following work, treating MWCNTs by sonication in H2O caused the implementation of O-containing functionalities (OH, C–O–C and COOH) and no considerable harm to the basic CNTs structure (Vanyorek et al. 2014; Parodi et al. 2014). The production of functional groups is reflected in the withdrawal of –CHn groups existing on the pristine CNTs and the presence of H bonding between the CNTs and the aqueous medium (Wang et al. 2014a, b, c; Sato et al. 2013). Previously, soluble and oxidized SWCNTs arranged by supramolecular attachment of functionalized organic crown ethers (2-aminomethyl-18-crown-6). The obtained CNTs yielded concentrations of dissolved products in H2O and CH2OH. The composition of produced CNTs reflected in noncovalent, zwitterionic chemical interaction involving COOH groups and NH2 moieties (Masinga et al. 2013). The advanced oxidized functionalization of CNTs required a vast ultrasonic treatment in a mixture of concentrated HNO3 and H2SO4 (Kim et al. 2013a, b, c). Such extreme conditions bring about the opening of the CNTs caps in addition to the formation of holes in the sidewalls (Vanyorek et a. 2014). This is persisted by an oxidative etching along the CNTs wall with the simultaneous discharge of CO2. The ultimate products are CNTs with fragment length of 100–300 nm, whose ends and sidewalls decorated with an elevated density of diverse O2 containing groups (Wang et al. 2014a, b, c). 948 949 953 954 955 956 957 958 959 960 961 962 963 964 965 966 967 968 969 970 971 972 973 974 975 976 977 978 979 980 PR OO 947 D 946 TE 945 EC 944 OR R 943 F 950 with porphyrins or biomolecules (Li et al. 2014; Sedláková et al. 2014a, b). Moreover, the major benefit of noncovalent functionalization is that it does not break the conjugated system of CNTs sidewalls, and as a result, it does not influence the final structural properties of the matter. The noncovalent functionalization of CNTs can do much to maintain their preferred properties, while enhancing the solubility rather remarkably (Werengowska-Ciecwierz et al. 2014). The noncovalent entities interact with the sidewalls of CNTs via π–π stacking interactions, and consequently opening up the track for the noncovalent functionalization of CNTs (Yan et al. 2014). 942 UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … 4.2.2 Small Molecules Functionalized CNTs The interaction between CNTs and a series of small molecules involving cyclohexane, cyclohexene, cyclohexadiene, and benzene is studied in gas phase and confirmed that p–p interactions are essential for the adsorption on CNTs (Nxumalo Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 32/61 Time: 2:52 pm N.M. Julkapli et al. 998 4.2.3 Derivatives Functionalized CNTs 999 The adsorption of multiple derivatives, replaced with groups with different electronic properties and volume size onto the sidewalls of cut SWCNTs, expected to make better p–p bond interactions controlling the adsorption process (Table 6). This procedure along with an electron donor–acceptor charge transfer interacts between the aromatic adsorbents and the SWCNTs sidewall, which technicality causes a considerable change in the electrical dipole moment along its primary axis. This shift alters the local electrostatic potential in the CNTs, modifies its conductance with elevated threshold voltage current flows (Tan et al. 2011; Martin et al. 2009). Functionalization of CNTs by means of derivatives with positive or negative charge like nitrogenated bases, alkyl ammonium ion, through p–p interaction carried on by the assembling of the energy/electron donor molecules complementary electrostatics, axial coordination or crown ether-alkyl ammonium ion interactions, in order (Martin et al. 2009). This brought astable donor–acceptor system with maximum preservation of the mechanical and electronic characteristics of CNTs. To the best our knowledge, self-assembly via ammonium ion-crown ether derivatives is held as one of the most potent methods as it proposes a high level of directionality with binding energies up to 50–200 kJ mol−1 (Feng and Chen 2006). 987 988 989 990 991 992 993 994 995 996 1000 1001 1002 1003 1004 1005 1006 1007 1008 1009 1010 1011 1012 1013 1014 1015 1016 1017 1018 1019 PR OO 986 D 985 TE 984 EC 983 OR R 982 F 997 et al. 2013). It is discovered that the CNTs and small molecule interactions in this series regulated by coupling of the p-electrons of the molecules in the electronic psystem of the CNTs (Liu et al. 2013a, b, c; Mhlanga et al. 2013a, b). Undeniably, the coupling of p-electrons involving CNTs and aromatic molecules is noticed as an effective way to solubilize individual CNTs, which consecutively controls electronic properties (Song et al. 2012). In addition, the solubility of CNTs with biological elements is definitely more appropriate by introducing and incorporating tiny biomolecules (Pang et al. 2010). The biomolecules for noncovalent functionalization of CNTs involve simple saccharides, enzyme, protein, DNA, and others. A range of biomaterials consisting of n-decyl-β-Dmaltoside, ϒ-cyclodextrin, n-cyclodextrin, chitosan, pullulan, and phospholipid-dextran have been employed for noncovalent functionalization of CNTs (Braga et al. 2014; Lu et al. 2014; Ahmad et al. 2013). They have assisted the process for the reason that such biomolecules have nearly no light adsorption in UV-Vis wavelength region, in order to that the CNTs polymeric composites can be characterized by photochemical and are mostly biocompatible and appropriate for many medicinal purposes (Xu et al. 2010; Bai et al. 2010; Krause et al. 2010). 981 UN C Author Proof 32 4.2.4 Polymer Functionalized CNTs Polymers, particularly conjugated polymers, have proved to serve as exceptional wrapping materials for the noncovalent functionalization of CNTs due to π–π stacking and van der Waals interactions between the conjugated polymer chains Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 33/61 Time: 2:52 pm Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … 33 Table 6 List of derivatives functionalized CNTs with its advantages and potential applications Advantages Potential applications References Chromophore Reversible and repeatable conductance change over a long period of time Excellent solubility in H2O Transparent solution of CNTs High single nanotube chiral index Nucleophilically be substituted by primary/secondary NH2 Allow immobilization of the biopolymer on the CNTs surface Mitigation of toxicity Integrated nano photodetector Sanip et al. (2009) N-succinimidyl1pyrenebutanoate 1023 1024 1025 1026 1027 1028 1029 1030 1031 1032 1033 1034 1035 OR R 1022 Protein detector/sensor Ghasemi et al. (2014) Active coating materials Bandaru and Voelcker (2012) Sevilla et al. (2014) Donor acceptor hybrid Template for immobilization of electroactive unit on CNTs surface Ehli et al. (2008) having aromatic rings and surface of CNTs within. The physical adsorption of polymer on the CNTs surface reduced the surface tension of CNTs that successfully averted the aggregation of CNTs (Adhikari et al. 2014). The success of this method relied deeply on the properties of polymer and medium chemistry. There are two types of polymers used, nonionic and cationic polymer (Table 7). In addition to achievable enhancement in the mechanical and electrical properties of polymers, the functionalization with CNTs regarded as a useful approach for integrating CNTs into polymer-based devices (Liu et al. 2014a, b, c, d, e; Chehata et al. 2014). For noncovalently functionalized CNTs with polymers, quite a lot of strategies have been taken on and involved physical mixing in solution, in situ polymerization of monomers in the presence of CNTs, surfactant-assisted processing of composites and chemical functionalization (Roy et al. 2014). For instance, polymers such as poly(m-phenylene-co-2,5-dioctoxy-p-phenylenevinylene) were employed to wrap around CNTs in organic solvent contained CHCl3. Polymers which hold a polar side chain, including poly(vinyl pyrrolidone) or poly(styrene silfonate) gave stable solutions of SWCNTs-filled polymer complexes in H2O medium (Ten et al. 2014; UN C 1021 Matsuoka et al. (2014) TE Pyrenetetrathiafulvalene Pyrenepyropheophorbide Interface biocompatibility with living cells Detect the dynamic secretion of biomolecules Able to transform sunlight into electrical/chemical energy Formation of flexible and medium length chains Favor a facile interaction with CNTs surface EC N-acetyl-Dglucosamine 1020 Semiconductor D Glycodendrimers PR OO Ammonium amphiphiles F Derivatives Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 34/61 Time: 2:52 pm N.M. Julkapli et al. Table 7 List of polymer functionalized CNTs with different types and potential applications Types Advantages References Polymeric amphiphiles Polyvinylpyrrolidone A stable composites materials High glass transition temperature Elastic modulus 30 and higher in relative to native sample Water soluble Increase the hydrophilicity of CNTs Positively charged polyelectrolytes Formation of strong interface via electrostatic interactions Systematic and molecularly controlled organization of CNTs Stable CNTs formation Efficiency of macromolecular dispersion Promising electronic interactions in CNTs bundles Formation of uniform coating (1.0–1.5 thick) Good solubility in organic solvents obtained by covalent/ionic attachment of long chain aliphatic NH2 onto COOH groups Able to fold around the graphitic surface of CNTs Good dispersion in aqueous solutions by noncovalent interactions The size and morphology of coated CNTs can control by peptide–peptide interactions Highly ordered structure Han et al. (2014) EC TE Polystyrene sulfonate + Polydiallyldimethylammonium chloride N-ethyl-4-vinylpyridinum bromide-co-4-vinylpyridine PR OO Polydiallyldimethylammonium chloride D Polystyrene sulfonate Biopolymer OR R Polyethylene glycol Polypeptide F Polymer UN C Author Proof 34 Lee and Cui (2011) Huaming et al. (2005) Vladimir et al. (2005) Nozomi et al. (2007) Davide et al. (2003) (continued) Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 35/61 Time: 2:52 pm Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … 35 Table 7 (continued) Advantages Polar part of the lipids could participate in the selective immobilization of histidine-tagged protein through metal ion chelates The lipid membrane found to maintain its fluidity and mobility of lipid molecules Effective in dispersing CNTs in H2O A stable solution Slow structure rearrangement Aligned parallel to the CNTs surface with a high degree of orientation order 1041 1042 1043 1044 1045 1046 1047 1048 1049 1050 1051 1052 1053 1054 1055 1056 1057 1058 1059 1060 1061 TE 1040 EC 1039 OR R 1038 Cyrille et al. (2003) Davide et al. (2004) He et al. 2014). While surfactants may be effective in the solubilization of CNTs, they proven permeable plasma membranes (Primo et al. 2013; Mallakpour and Zadehnazari 2013; Rath et al. 2013). They are toxic for biological purpose, hence imperfect for biomedical applications (Chen et al. 2013a, b; Fisher et al. 2013; de Lannoy et al. 2013a, b; Amirilargani et al. 2013). To defeat the imperfections, biopolymer functionalized CNTs have persistently studied. CNTs liquid crystal phase creation and selective chiral SWCNTs enrichment assisted by biopolymer uncovered that biopolymer is a promising agent of high quality on surface functionalization of CNTs (Battigelli et al. 2013a, b; Albuerne et al. 2013; Loos et al. 2013a, b; Wei et al. 2005). Now widely available, large-scale production and low-price polysaccharides including chitosan, gelling gum, hydraulic acid, and others have realized to be easier and commercially acceptable; therefore making a high-concentration CNTs in a single dispersion becomes more convenient. For instance, physical purification of CNTs by chitosan functionalization has been endorsed to be easy processing and also is efficient. Besides, the CNT-H2O interface direction, the ordered organization of lipid derivatives onto CNTs by supra molecular self-assembly by biopolymers on the CNT surface has noticed to be of tremendous effect on CNTs dispersion (Hordy et al. 2013). Gum Arabia, the primeval biopolymer dispersant presented to stabilize SWCNTs (Yulong et al. 2006; Rajdip et al. 2002; Nadia et al. 2005). The dispersion can concentrate into suspension of SWCNTs concentration as much as 150 mg mL−1; the most favorable concentration of SWCNTs (Rajdip et al. 2002). The hyaluronic acid functionalized CNTs at high concentration of 10 mg mL−1 demonstrated anisotropic birefringence phenomenon, representing the liquid crystal part of biopolymer functionalized CNTs. Aligning CNTs throughout a liquid crystal phase of CNTs by polysaccharide has improved as well. UN C 1037 D Oligonucleotides 1036 References F Types Single-chain lipid PR OO Polymer Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 36/61 Time: 2:52 pm N.M. Julkapli et al. 5 CNTs/Polymer: Applications 1063 5.1 Structural Applications 1069 1070 1071 1072 1073 1074 1075 1076 1077 1078 1079 1080 1081 1082 1083 1084 1085 1086 1087 1088 1089 1090 1091 1092 1093 1094 1095 1096 1097 1098 1099 1100 1101 1102 PR OO 1068 D 1067 TE 1066 The structural characteristics of CNTs-filled polymer composites are very imperative in automotive, aerospace, paint, protectors, and other (Hyang et al. 2007). As mechanical properties play a crucial role in structural purposes, load transfer from the polymer matrix to CNTs filler grows to be essential. Load transfer between polymer matrix and CNTs is subject to the interfacial shear stress between the composite components (Kumar Sachdev et al. 2013). To make the reinforcement efficient, it is required that the CNTs must be adequately long and the interface between CNTs and polymer matrix is strong (Xiaowen et al. 2006). Since CNTs has some surface defects, including changeable diameter and bend/twist as a result of nonhexagonal defects, along CNTs, mechanical interlocking do play a role in CNTs to polymer interface (Hyang et al. 2007). The outstanding mechanical characteristics of CNTs are proposed that incorporation of very little amounts of CNTs into the polymer matrix initiated structural materials application with considerably higher strength and modulus. For instance, the addition of 1 wt% of MWCNTs in the polystyrene by solution evaporation procedure brought about 36–42 and almost 25 % enhancement in tensile modulus and tensile strength, in order (Suemori et al. 2013). Whereas, the improvement in indentation resistance was recorded up to 3.5 times by supplementing 2 wt% SWCNTs in epoxy resin (Shi et al. 2009; Huaming et al. 2005). Some studies observed a major enhancement in modulus and hardness (1.8 times and 1.6 times) with the integration of 1 wt% MWCNTs in polyvinyl alcohol (Song et al. 2013). Homogeneous dispersion and alignment of CNTs had a considerable result in mechanical properties of CNTs-filled polymer composites particularly in the structural applications (Kanagaraj et al. 2011). It is reported that by enhancing the dispersion of CNTs through the in situ polymerization, great mechanical strength of CNTs-filled polymer composites could employ to make some high-end sporting goods as well as tennis rackets, baseball bat, and consequently delivering excellent performance (Hida et al. 2012). The mechanical property study of CNTs-filled polymer is also described by morphology studies (Girei et al. 2012). For example, pullout process proposes that effective load transfer arises from the polymer matrix to the outer layer of CNTs, caused by the sturdy covalent bonding within its interfacial region (Shi et al. 2009). This observation anticipated that the efficiency of property improvement relies on the form of CNTs, processing technique, and compatibility between CNTs and polymeric matrix (Pascual et al. 2012). Additionally, the modulus and strength of composites mainly traded for high fracture toughness. In contrast with traditional polymer composites containing micron-scale fillers, the integration of nanoscale CNTs into a polymer system causes the very tiny distance between the fillers; these characteristics of composites can largely modified even at an exceedingly low content of filler (Li et al. 2011). Even though chemical functionalization of CNTs EC 1065 OR R 1064 F 1062 UN C Author Proof 36 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 37/61 Time: 2:52 pm 37 1106 5.2 Medical Application PR OO 1104 F 1105 enhanced the compatibility between CNTs and polymer, which consecutively improved the mechanical properties, but it has a worsening effect on the other properties such as electrical and thermal conductivity (Raja et al. 2014). 1103 1133 5.3 Sensor Applications 1111 1112 1113 1114 1115 1116 1117 1118 1119 1120 1121 1122 1123 1124 1125 1126 1127 1128 1129 1130 1131 1134 1135 1136 1137 1138 1139 TE 1110 EC 1109 OR R 1108 D 1132 The stable dispersed CNTs by biopolymer set up into biomedical purposes as well as tissue engineering and drug delivery system (Yu and Li 2012). For the bioactivity of biopolymer, their composites with CNTs offer exceptional sensing performance (Liu et al. 2014a, b, c, d, e). The biomimetic actuation founded on CNTsfilled biopolymer devices have as well initially proved to be of large and fast actuation displacement under low voltage electrical stimulation (Chahine et al. 2008). The CNTs, and in particular SWCNTs, with surface area as high as 2600 m2 g−1 is very appropriate for acting as a drug carrier for biomedical purposes. For instance, CNTs has presented as a template for hosting bioactive peptides to the immune system (Davide et al. 2003). In this case, B cell epitope of the foot and mouth disease virus covalently adhered to the NH2 groups functionalized CNTs (Serrano et al. 2014). This, sequentially, increases the formation of peptides around CNT adopting the appropriate secondary structure because recognized by specific monoclonal and polyclonal antibodies. The function of CNTs as vaccine delivery further developed via the interaction with the complement system (Battigelli et al. 2013a, b). It is found that pristine CNT activates the complement following both classical and alternative ways to make selective adsorption of some of its protein, which consequently enhances antibody response leading to immunization with peptide-CNT conjugates (Davide et al. 2003, 2004). It also recorded that CNTs encouraged delivery of DNA or any bioactive mediator to cells. As CNTs surface functionalized to attach either electrostatically or covalently to DNA and RNA, the residual unfunctionalized and hydrophobic segment of CNTs attracted to the hydrophobic areas of the cells (Rath et al. 2013). Besides, CNTs-filled chitosan biopolymer offers localized delivery of therapeutic agents initiated by external sources (Battigelli et al. 2013a, b). 1107 UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … The CNTs-filled polymer composites used as an implantable sensor that is capable of transmitting information extracorporeally. Such a sensor made real-time date related to the physiological relevant parameters such as pH, O2 concentration, and glucose level available. In addition, the good biocompatibility with high electrical and electrochemical sensitivity assisted implantable biosensor applications (Qi et al. 2013a, b, c). The early research found that CNTs-filled polymer composites are able Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 38/61 Time: 2:52 pm N.M. Julkapli et al. 1165 5.4 Semiconductor Applications 1146 1147 1148 1149 1150 1151 1152 1153 1154 1155 1156 1157 1158 1159 1160 1161 1162 1163 1166 1167 1168 1169 1170 1171 1172 1173 1174 1175 1176 1177 1178 1179 1180 PR OO 1145 D 1144 TE 1143 EC 1142 OR R 1141 F 1164 to detect serum proteins, as well as disease markers, autoantibodies, and antibodies (Grabowski et al. 2014). An important composite biosensor is derived from CNTs-filled chitosan. The CNTs-filled chitosan composites have discovered to be an excellent biocompatibility for neutral cell growth (Spinks et al. 2006). Their suspension coated on glassy carbon electrode is capable of detecting 90 % of NaDH in less than 5 s. The stability and sensitivity of CNTs-filled chitosan composites as a biosensor allowed interference-free determination of glucose in physiological matrix (Gopalan et al. 2009). A composite of MWCNTs-filled chitosan composites employed as a matrix for capturing lactate dehydrogenase into a glassy carbon electrode to produce amperometric biosensor (Mao et al. 2014). Moreover, CNTs-filled chitosan-lactate dehydrogenase composite film demonstrats the abilities to boost the current responses, to reduce the electro-oxidation potential of β-nicotinamide adenine dinucleotide and to thwart the electrode surface fouling. It found that, the efficient biosensor for this kind of system has the sensitivity of lactate up to 0.0083 AM−1 cm−2 with response time of 3 s (Shawky et al. 2012; Popuri et al. 2014). The entrapment of acetychlolinesterase on CNTs-filled chitosan biosensor recorded that the inhibition of organophosphorous insecticide to the enzymatic activity of acetylcholinesterase, using triazophos as a model of compounds is relative to its concentrations (Zhang et al. 2012). The acetylcholinesterase could regenerate using pralidoxime iodide within 8 min. Therefore, the CNTs-filled chitosan biosensor has outstanding characteristics and performance, such as high precision and reproducibility, suitable stability and accuracy, quick response, and low detection threshold (Spinks et al. 2006). It has a potential function in the characterization of enzyme inhibitors and detection of toxic compounds against enzyme (Gopalan et al. 2009). 1140 The CNTs composites have anticipated as a potential replacement for Cu interconnects in future technologies because of its high mechanical stability, high thermal conductivity, large current ability and compatibility with present-day silicon technologies (Peter and Richard 2002). For instance, the improvement in electrical conductivity and insulating of CNTs in the polymer matrix to a high extent has accomplished with a very small loading (0.021 wt%) of CNTs. The current through CNTs is either sublinear or superlinear with voltage, in the same way as many other metallic and semiconducting nanowires/nanotubes (Gardea and Lagoudas 2014). The remarkable fact is the large current carrying capability of CNTs composites as compared to Cu as well as to superconductors and its rise with increasing diameter (Bal and Saha 2014). For example, SWCNTs composites are capable of carrying a current in the microampere random while 100 nm diameter MWCNTs composites revealed to transmit up to mili-ampere current. In reality, the current carrying capability of MWCNTs is much greater than SWCNTs, attributable to its larger conduction at outer shell (Abu et al. 2006). The boost in electrical UN C Author Proof 38 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 39/61 Time: 2:52 pm 39 1215 5.5 Thermal Conductor Application 1187 1188 1189 1190 1191 1192 1193 1194 1195 1196 1197 1198 1199 1200 1201 1202 1203 1204 1205 1206 1207 1208 1209 1210 1211 1212 1213 1216 1217 1218 1219 1220 1221 PR OO 1186 D 1185 TE 1184 EC 1183 OR R 1182 F 1214 conductivity of polymer material with CNT addition is the greatest benefit of production of CNT-filled polymer composites (Jiang et al. 2014a, b). The electrical conductivity of CNTs-filled polymer composites is subject to on many features including type of CNYs, aspect ratio, surface functionalization and CNT content (Xiaowen et al. 2006). For example, the electrical conductivity of nanocomposites rises with increasing CNTs loading up until a significant filler concentration, where a dramatic boost in conductivity recorded (Thuau et al. 2006). This critical CNTs concentration is called as electrical percolation threshold concentration (Thuau et al. 2006). At this stage, CNTs particle shapes three-dimensional conductive networks inside a polymer matrix, therefore electron tunnels from one filler to another are created and result in a high resistance presented by insulating polymer matrix. Since the creation of percolating networks is associated with both intrinsic conductivity and aspect ratio of CNTs particles, the CNTs-filled polymer composites have exhibited very low percolation threshold. This is due to the high conductivity and the aspect ratio of CNTs (Ma et al. 2014a, b). Consequently, the percolation threshold concentration and nanocomposites conductivity determined by polymer type, synthesis technique, aspect ratio of CNTs, the extrication of CNTs agglomerates, uniform spatial distribution of single CNTs and the level of alignment (Aljaafari et al. 2012). Another considerable factor, which influenced the electrical conductivity of nanocomposites is the chemical functionalization of CNTs. This is because of the interference with the extended πconjugation of CNTs and thus decreases the electrical conductivity of isolated CNTs (Qi et al. 2013a, b, c). As a result, these composite systems could be employed to protect electromagnetic interference and as electrostatic discharge components (Song et al. 2013). As a major progress in electrical conductivity monitored at very low CNT loading, this composite system found application as lightweight, economical, and highly effective shielding materials (Ramoa et al. 2013). Because of very great aspect ratio and impressive electrical properties of CNTs, some reports have revealed that ultra-low electrical percolation limit was observed with merely 0.0025 wt% in aligned CNTs-filled epoxy composites (Zeng et al. 2013). As a result, CNTs-filled polymer composites are in increasing demand in various application area such as transparent conductive coatings, electrostatic dissipation, electrostatic painting, and electromagnetic interference protecting applications (Qi et al. 2013a, b, c; Matsuoka et al. 2014). 1181 UN C Author Proof Multifunctionalized Carbon Nanotubes Polymer Composites … The thermal characteristics of polymer matrix as well altered by CNT addition including increment on glass transition, melting and thermal decomposition temperatures caused by hindered chain, and segmental mobility of the polymers (Reddy and Ramu 2008). Besides, the CNTs also influenced the crystallization speed and percentage of crystallinity by performing as nucleating agents in CNTs-filled polymer system (Table 8). Integration of 1 wt% surfactant in the role of a wetting Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 40/61 Time: 2:52 pm Author Proof 40 N.M. Julkapli et al. Table 8 Shielding properties of different kinds of CNTs-filled polymer composites Shielding properties (dB) References 7.5 vol% MWCNTs-filled polypropylene 7 wt% MWCNTs-filled polystyrene 20 wt% MWCNTs polyurethane 40 wt% Polymethyl methacrylic 35 Lopez Manchadoa et al. (2006) Guoxing et al. (2010) Hsu-Chiang et al. (2006) Fangming et al. (2003) PR OO 20 17 27 F CNTs-filled polymer composite systems 1237 6 Conclusion 1227 1228 1229 1230 1231 1232 1233 1234 1235 1238 1239 1240 1241 1242 1243 1244 1245 1246 1247 1248 1249 1250 TE 1226 EC 1225 OR R 1224 The study on CNT-filled polymer nanocomposite surmized that CNTs are capable of altering the properties of polymer matrices. The great challenge in realizing the full ability of CNTs is to accomplish homogenous dispersion of CNTs with the intention that the maximum filler surface area is accessible for load-transfer between the composite constituents. The functionalization of CNTs offers a suitable route to develop dispersion and compatibility without negatively affecting the properties of the resulting composite. Three chief processing techniques of CNTfilled polymer composites involve solution, melting, and in situ polymerization. Solution blending yields high-quality composite, but melt compounding is much simpler, and offers alternatives to large-scale production. The greatest improvement in mechanical properties of CNTs-filled polymer composites is detected in the case of in situ polymerization, which forms a covalent bond between CNTs and the polymer. UN C 1223 D 1236 agent enhanced the glass transition temperature of CNTs-filled polymer composites up to 25 to 40 °C (Hone et al. 1999). Additionally, the thermal decomposition temperature of polypropylene in N2 improves by 12 °C on 2 vol% CNTs loading (Prolongo et al. 2008). These observations imply that shielding characteristics of the composites determined by numerous factors including fabrication method and purification of CNTs. It is recorded that enhancement in both properties boosts its mechanical and processing properties as well (Maizatulnisa et al. 2013). Besides, the microwaveabsorbing capacity of CNTs could utilize to heat temporary accommodation structures (Raja et al. 2013a, b). Owing to the excellent thermal conductivity of CNTs, integration of CNTs drastically enhances the thermal transport properties, which makes possible its usage as printed circuit boards, connectors, thermal interface equipments, heat sinks, and other high performance thermal management system (Ibrahim et al. 2012; Xie et al. 2013). 1222 AQ2 Layout: T1 Standard Unicode Book ID: 326800_1_En Book ISBN: 978-81-322-2469-3 Chapter No.: 6 Date: 16-5-2015 Page: 41/61 Time: 2:52 pm 1256 1257 1258 1259 1260 1261 1262 1263 1264 1265 1266 1267 1268 1269 1270 1271 1272 1273 1274 1275 1276 1277 1278 1279 1280 1281 1282 1283 1284 1285 1286 1287 1288 1289 1290 1291 1292 1293 1294 1295 1296 1297 1298 1299 1300 1301 1302 F PR OO 1255 D 1254 Abe S, Nakayama K, Hayashi D, Akasaka T, Uo M, Watari F, Takada T (2011a) Development of a novel transparent substrate coated by carbon nanotubes through covalent bonding. 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Sci Technol Adv Mater 15(1):015007 Agnihotri P, Kar KK (2007) Hybrid nanocomposites of carbon nanotubes (CNTs) grown on carbon fiber in polyester matrix with improved thermomechanical properties. In: Proceedings of the annual technical conference—ANTEC, vol 4, pp 2191–2195 Agnihotri P, Basu S, Kar KK (2011) Effect of carbon nanotube length and density on the properties of carbon nanotube-coated carbon fiber/polyester composites. Carbon 49(9):3098– 3106 Ahmad AL, Jawad ZA, Low SC, Sharif Zein SH (2013) The functionalization of betacyclodextrins on multi walled carbon nanotubes: effects of the dispersant and non aqueous media. Curr Nanosci 9(1):93–102 Albuerne J, Zenkel C, Munirasu S (2013) Functionalization and polymerization on the CNT surfaces. Curr Org Chem 17(17):1867–1879 Alimohammadi F, Parvinzadeh Gashti M, Shamei A (2013) Functional cellulose fibers via polycarboxylic acid/carbon nanotube composite coating. 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(2002), Jiang et al. (2014), Ma et al. (2014), Qi et al. (2013), Liu et al. (2013, 2014), Battigelli et al. (2013), Chen et al. (2013), de Lannoy et al. (2013), Loos et al. (2013), Mhlanga et al. (2013), Wang et al. (2014), Kim et al. (2013), Wu et al. (2013), Battisti et al. (2014), Sedláková et al. (2014), Abe et al. (2011), Li et al. (2013), Jiang et al. (2013), Ribeiro et al. (2012), Lin et al. (2011), Yu et al. (2013), Tarawneh et al. (2012), Raja et al. (2013), Kulathunga et al. (2014), Tang et al. (2010), Jung et al. (2013), Seyhana et al. (2007), Huang et al. (2014), Safdari et al. (2013), MinFeng et al. (2000), Gary et al. (2008), Adams et al. (2001), Bandaru et al. (2012), Dubois et al. (2006), Hua et al. (2005), Kiliaris et al. (2010), Shigeo et al. (2000), Rohan et al. (2007) and Richard et al. (2001)’ has been changed to ‘Raja et al. (2013a, b), Peter and Richard (2002), Jiang et al. (2014a, b), Ma et al. (2014a, b), Qi et al. (2013a–c), Liu et al. 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