Multiwall carbon nanotubes (MWCNTs) oxidized by an acid treatment were deposited on the surface of as-received commercial aramid fibers containing a surface coating ("sizing"), and fibers modified by either a chlorosulfonic treatment or a mixture of nitric and sulfuric acids. The surface of the aramid fiber activated by the chemical treatments presents increasing density of CO, COOH and OH functional groups. However, these chemical treatments reduced the tensile mechanical properties of the fibers, especially when the nitric and sulfuric acid mixture was used. Characterization of the MWCNTs deposited on the fiber surface was conducted by scanning electron microscopy, Raman spectroscopy mapping and X-ray photoelectron spectroscopy. These characterizations showed higher areal concentration and more homogeneous distribution of MWCNTs over the aramid fibers for as-received fibers and for those modified with chlorosulfonic acid, suggesting the existence of interaction between the oxidized MWCNTs and the fiber coating. The electrical resistance of the MWCNT-modified aramid yarns comprising 1000 individual fibers was in the order of M Omega/cm, which renders multifunctional properties.CONACYT-CIAM (Mexico) 188089 CONICYT (Chile) 120003 "Fondo Mixto CONACYT-Gobierno del Estado de Yucatan" 24704

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Curing effects were investigated by using the electrical response of a single carbon nanotube yarn (CNTY) embedded in an epoxy resin during the polymerization process. Two epoxy resins of different viscosities and curing temperatures were investigated, varying also the concentration of the curing agent. It is shown that the kinetics of resin curing can be followed by using the electrical response of an individual CNTY embedded in the resin. The electrical resistance of an embedded CNTY increased (~9%) after resin curing for an epoxy resin cured at 130 °C with viscosity of ~59 cP at the pouring/curing temperature (“Epon 862”), while it decreased (~ −9%) for a different epoxy cured at 60 °C, whose viscosity is about double at the corresponding curing temperature. Lowering the curing temperature from 60 °C to room temperature caused slower and smoother changes of electrical resistance over time and smaller (positive) residual resistance. Increasing the concentration of the curing agent caused a faster curing kinetics and, consequently, more abrupt changes of electrical resistance over time, with negative residual electrical resistance. Therefore, the resin viscosity and curing kinetics play a paramount role in the CNTY wicking, wetting and resin infiltration processes, which ultimately govern the electrical response of the CNTY immersed into epoxy.

Carbon nanotube yarns (CNTYs) are hierarchical fibers with outstanding electrical properties, and understating the temperature‐dependence of their electrical resistance (thermoresistivity) is essential for sensing applications and development of self‐sensing polymer composites. The cyclic thermoresistive response of individual CNTYs and the effect of embedding the yarn into a polymer are experimentally investigated herein. The effect of confining the CNTY by a thermosetting polymer is addressed by studying the thermoresistive response of CNTY/vinyl ester single‐fiber composites. Heating–cooling cycles ranging from 25 (room temperature [RT]) to 100 °C and 25 to −30 °C are applied to individual CNTYs and to CNTYs embedded into a vinyl ester polymer, while their electrical resistance is simultaneously recorded. Both the CNTY and its single‐fiber composite show a negative dependence of electrical resistance with temperature. For both temperature ranges (above and below RT), the average temperature coefficient of resistance found for individual CNTYs is ≈−9.5 × 10−4 K−1, and its magnitude decreases about ≈30% when the yarn is embedded into the vinyl ester polymer. The hysteresis rendered by the different heating and cooling pathways is small for individual CNTYs, and largely increases when the CNTY is embedded into the polymer.

The role of the physical properties of multiwall carbon nanotubes on the strain-sensing piezoresistive behavior of multiwall carbon nanotube/polymer composites is systematically studied using three types of multiwall carbon nanotubes as fillers of a brittle thermosetting (vinyl ester) and a tough thermoplastic (polypropylene) polymers under quasi-static tensile loading. Two of the three multiwall carbon nanotubes investigated have similar length, aspect ratio, structural ordering, and surface area, while the third group contains longer multiwall carbon nanotubes with higher structural ordering. The results indicate that longer multiwall carbon nanotubes with higher structural ordering yield higher piezoresistive sensitivity, and therefore are better suited as sensors of elastic and plastic strains of polymer composites. The highest gage factor achieved was approximately 24 and corresponded to the plastic zone of multiwall carbon nanotube/polypropylene composites with the longest nanotubes.

Multiwalled carbon nanotube (MWCNT)/polyethylene terephthalate (PET) composites were prepared by three processing methods: direct extrusion (DE), melt compounding followed by extrusion (MCE), and dispersion of the MWCNTs in a solvent by sonication followed by extrusion (SSE). The mechanical properties of the MWCNT/PET composites processed by MCE increased with 0.1 wt% MWCNTs with respect to the neat PET. The electrical percolation threshold of MWCNT/PET composites processed by DE and MCE was ~1 wt% and the conductivity was higher for composites processed by MCE. Raman spectroscopy and scanning electron microscopy showed that mixing the MWCNTs by melt compounding before extruding yields better dispersion of the MWCNTs within the PET matrix. The processing method assisted by a solvent resulted in matrix plasticization.

The effect of polymerization kinetics and resin viscosity on the electrical response of a single carbon nanotube yarn (CNTY) embedded in a vinyl ester resin (VER) during polymerization was investigated. To analyze the effect of the polymerization kinetics, the concentration of initiator (methyl ethyl ketone peroxide) was varied at three levels, 0.6, 0.9, and 1.2 wt.%. Styrene monomer was added to VER, to reduce the polymer viscosity and to determine its effect on the electrical response of the CNTY upon resin wetting and infiltration. Upon wetting and wicking of the CNTY by VER, a transient decrease in the CNTY electrical resistance (ca. −8%) was observed for all initiator concentrations. For longer times, this initial decrease in electrical resistance may become a monotonic decrease (up to ca. −17%) or change its trend, depending on the initiator concentration. A higher concentration of initiator showed faster and more negative electrical resistance changes, which correlate with faster gel times and higher build-up of residual stresses. An increase in styrene monomer concentration (reduced viscosity) resulted in an upward shift of the electrical resistance to less negative values. Several mechanisms, including wetting, wicking, infiltration, electronic transfer, and shrinkage, are attributed to the complex electrical response of the CNTY upon resin wetting and infiltration.

Electrical monitoring of strain and damage in multiscale hierarchical composites comprising unidirectional aramid fibers modified by multiwall carbon nanotubes and polypropylene as matrix is investigated. The key factor for electrical self-sensing in these thermoplastic composites is the formation of a multiwall carbon nanotube network, which is achieved by using two material architectures. In the first architecture, the multiwall carbon nanotubes are dispersed within the polypropylene matrix, while aramid fibers remain unmodified. The second architecture uses also multiwall carbon nanotube-modified polypropylene matrix, but the aramid fibers are also modified by depositing multiwall carbon nanotubes. Under tensile loading, the electrical response is nonlinear with strain ( ε), and the piezoresistive sensitivity was quantified by gage factors corresponding to low ( ε < 0.25%) and high ( ε > 0.3%) strain regimes. Such gage factors were 4.83 (for ε < 0.25%) and 13.2 (for ε > 0.3%) for composites containing multiwall carbon nanotubes only in the polypropylene matrix. The composites containing multiwall carbon nanotubes in the matrix and fibers presented higher piezoresistive sensitivity, with average gage factors of 9.24 ( ε < 0.25%) and 14.0 ( ε > 0.3%). The higher sensitivity to strain and damage for a specific material architecture was also evident during cyclic and constant strain loading programs and is attributed to the preferential localization of multiwall carbon nanotubes in the hierarchical composite.