Broader applications of carbon nanotubes to real-world problems have largely gone unfulfilled because of difficult material synthesis and laborious processing. We report high-performance multifunctional carbon nanotube (CNT) fibers that combine the specific strength, stiffness, and thermal conductivity of carbon fibers with the specific electrical conductivity of metals. These fibers consist of bulk-grown CNTs and are produced by high-throughput wet spinning, the same process used to produce high-performance industrial fibers. These scalable CNT fibers are positioned for high-value applications, such as aerospace electronics and field emission, and can evolve into engineered materials with broad long-term impact, from consumer electronics to long-range power transmission.O n the molecular level, carbon nanotubes (CNTs) have an outstanding combination of mechanical strength and stiffness, electrical and thermal conductivity, and low density, making them ideal multifunctional materials that combine the best properties of polymers, carbon fibers, and metals (1). However, such outstanding properties have remained elusive on a macroscopic scale. Handling CNTs with sufficient length, stiffness, and chemical inertness introduces major challenges in material processing. Here we report lightweight fibers that approach the high specific strength of polymeric and carbon fibers, while also achieving the high specific electrical conductivity of metals and the specific thermal conductivity of graphite fibers.Two distinct routes have been developed for manufacturing neat CNT fibers (2). One route employs a solid-state process wherein CNTs are either directly spun into a fiber from the synthesis reaction zone (3, 4) or from a CNT forest grown on a solid substrate (5). This approach does not lend itself to the typical easy scale-up of chemical processes, as it combines multiple steps into a single one, limiting the options for process and material optimization. Indeed, solidstate fibers have low packing and poor orientation, and include impurities within their structure (6). Despite these shortcomings, solid-state CNT fibers have delivered the best properties so far (3, 4, 7-9). The reason for this relative success is the length of the CNTs that constitute these fibers-1 mm or more (2). Longer CNTs reduce the number of CNT ends in a fiber, yielding greater strength (10) and reducing CNT junctions, which increases electrical and thermal conductivity (11). The alternate fiber production route-wet spinning-was the first method for producing CNT fibers (12). In this process, premade CNTs are dissolved or dispersed in a fluid, extruded out of a spinneret, and coagulated into a solid fiber by extracting the dispersant. Wet spinning is easily scaled to industrial levels and is indeed the route by which highperformance fibers are manufactured (including ballistic fibers such as Kevlar and Twaron and structural fibers such as Toho Tenax and Thornel carbon fibers) (13). Decoupling the synthesis of CNTs from the spinning of the fibers allo...
Translating the unique characteristics of individual single-walled carbon nanotubes into macroscopic materials such as fibres and sheets has been hindered by ineffective assembly. Fluid-phase assembly is particularly attractive, but the ability to dissolve nanotubes in solvents has eluded researchers for over a decade. Here, we show that single-walled nanotubes form true thermodynamic solutions in superacids, and report the full phase diagram, allowing the rational design of fluid-phase assembly processes. Single-walled nanotubes dissolve spontaneously in chlorosulphonic acid at weight concentrations of up to 0.5 wt%, 1,000 times higher than previously reported in other acids. At higher concentrations, they form liquid-crystal phases that can be readily processed into fibres and sheets of controlled morphology. These results lay the foundation for bottom-up assembly of nanotubes and nanorods into functional materials.
Graphene combines unique electronic properties and surprising quantum effects with outstanding thermal and mechanical properties. Many potential applications, including electronics and nanocomposites, require that graphene be dispersed and processed in a fluid phase. Here, we show that graphite spontaneously exfoliates into single-layer graphene in chlorosulphonic acid, and dissolves at isotropic concentrations as high as approximately 2 mg ml(-1), which is an order of magnitude higher than previously reported values. This occurs without the need for covalent functionalization, surfactant stabilization, or sonication, which can compromise the properties of graphene or reduce flake size. We also report spontaneous formation of liquid-crystalline phases at high concentrations ( approximately 20-30 mg ml(-1)). Transparent, conducting films are produced from these dispersions at 1,000 Omega square(-1) and approximately 80% transparency. High-concentration solutions, both isotropic and liquid crystalline, could be particularly useful for making flexible electronics as well as multifunctional fibres.
The electrospinning process was used successfully to fabricate nanofibers of poly(ethylene oxide) (PEO) in which multiwalled carbon nanotubes (MWCNT) are embedded. Initial dispersion of MWCNTs in water was achieved using amphiphiles, either as small molecules (sodium dodecyl sulfate, SDS) or as a high molecular weight, highly branched polymer (Gum Arabic). These dispersions provided separation of the MWCNTs and their individual incorporation into the PEO nanofibers by subsequent electrospinning. The focus of this work is on the development of axial orientations in these multicomponent nanofibers. A theoretical model is presented for the behavior of rodlike particles representing CNTs in electrospinning. Initially the rods are randomly oriented, but due to the sinklike flow in a wedge they are gradually oriented mainly along the stream lines, so that straight CNTs are almost oriented upon entering the electrospun jet. The degrees of orientation of polymer, surfactant, and MWCNT were studied using X-ray diffraction and transmission electron microscopy. Oriented ropes of the nanofibers were fabricated in a converging electric field by a rotating disk with a tapered edge. A high degree of alignment of PEO crystals was found in electrospun nanofibers containing only PEO, as well as PEO/SDS. The latter also exhibited a high degree of alignment of the SDS layers. The axial orientation of PEO and SDS is significantly reduced in MWCNT-containing nanofibers. Transmission electron microscopy (TEM) images indicated that the MWCNTs were embedded in the nanofibers as individual elements, mostly aligned along the fiber axis. Nevertheless, there are also many cases in which the nanotubes appear twisted, bent, or with other irregularities. Comparison of cryo-TEM images of vitrified MWCNT dispersions with TEM images of the raw nanotubes indicated that sonication during the dispersion process may be responsible for the irregularities observed in some of the nanotubes.
Highly ordered, near-single-crystal lamellar films of a triblock copolymer (polystyrene−polybutadiene−polystyrene, PS/PB/PS) were used to study the deformation mechanism of a structure of alternating glassy−rubbery layers, at different orientations of the deformation axis relative to the layer normal. Synchrotron radiation was used for simultaneous in-situ deformation and small-angle X-ray scattering measurements. These were augmented with direct imaging of the structure by transmission electron microscopy. The deformation mechanism depends on the orientation of the force with respect to the structure. Loading parallel to the lamellae results in yielding by propagation of a stable macroscopic neck. The glassy PS layers break up at the neck front, releasing the rubbery layers to achieve high strain. The morphology that develops by deformation of the structure in other directions is an ensemble of new tilt boundaries oriented along the deformation axis. The lamellar normals tilt away from the deformation axis with increasing strain, keeping the lamellar spacing essentially constant. The effect of force applied perpendicular to the lamellae is to fold the layers into a “chevron” morphology, similar to other layered systems such as smectic liquid crystals. At high strain, plastic deformation and fracture of the glassy PS hinges of the “chevron” structure leads to symmetric kink boundaries parallel to the force axis. In addition, nucleation of kink bands around defects and propagation of the kink boundaries into adjacent regions can lead to a similar morphology. The lamellar spacing remains constant during perpendicular stretching, and the tilt angle of the lamellar normal follows the macroscopic deformation in an affine manner. Stretching at 45° forms asymmetric kink boundaries parallel to the force axis. The major limbs of the kink band tilt with increasing strain so that the angle between the lamellar normal and the force axis increases from its initial value of 45°, while the lamellar period remains constant. The minor limbs tilt in the opposite direction and exhibit dilation of the lamellar spacing. Eventually the layers rupture, forming voids at the kink-boundary interfaces. The tilt angle of the major-limb lamellae, as a function of strain, is less than predicted by the affine model. This study suggests a general deformation mechanism for a lamellar structure of alternating glassy and rubbery layers. The layered structure responds to deformation, in any direction other then parallel to the layers, by creating new internal tilt-grain boundaries parallel to the deformation axis. At higher strain the layers yield and subsequently fracture at the kink-boundary interfaces. With increasing strain the lamellar stacks between the kink boundaries tilt toward the deformation axis until they are nearly parallel to it. Since the main features of this mechanism are independent of the initial orientation angle of the layers relative to the deformation axis, it is relevant also to polygranular, globally unoriented lamellar st...
The physical and structural properties of acrylamide gels have been characterized by osmotic deswelling, mechanical compression, and x‐ray scattering. These properties vary considerably with the concentration of the crosslinking agent bisacrylamide, at fixed total monomers concentration (10% wt/wt water). In particular, changes in the properties appear more prominent at a crosslinking level of about 5‐6% (wt bisacrylamide/wt monomers). The compression modulus of as‐prepared and swollen gels passes through a maximum at this level of crosslinking. The swelling pressure curves can be separated into osmotic and elastic contributions of the gel network. The elastic part exhibits similar behavior to the compression modulus. The scaling of the osmotic part with the gel concentration varies with the degree of crosslinking, changing from 2.33 to 3.09. This indicates that the solvent power of water decreases with increasing crosslinking level, towards Φ conditions. The scattering patterns from the gels have been analyzed as arising from additive contributions from a homogeneous gel matrix, and embedded heterogeneities having a higher crosslinking density. These heterogeneities become much more prominent at the same level of crosslinking about 5‐6%. Hysteresis observed in the sorption/desorption behavior of polyacrylamide gel suggests that further irreversible structural changes may occur at water activities lower than probed by osmotic deswelling. © 1992 John Wiley & Sons, Inc.
The electrospinning process was used successfully to embed single-walled carbon nanotubes (SWCNTs) in a poly(ethylene oxide) (PEO) matrix, forming composite nanofibers. Initial dispersion of SWCNTs in water was achieved by the use of an amphiphilic alternating copolymer of styrene and sodium maleate. The resulting dispersions were stable, having a dark, smooth, ink-like appearance. For electrospinning, the dispersions were mixed with PEO solution in an ethanol/water mixture. The distribution and conformation of the nanotubes in the nanofibers were studied by transmission electron microscopy (TEM). Oxygen plasma etching was used to expose the nanotubes within the nanofibers to facilitate direct observation. Nanotube alignment within the nanofibers was shown to depend strongly on the quality of the initial dispersions. Well-dispersed and separated nanotubes were embedded in a straight and aligned form, while entangled nonseparated nanotubes were incorporated as dense aggregates. X-ray diffraction demonstrated a high degree of orientation of the PEO crystals in the electrospun nanofibers with embedded SWCNTs. This result is in pronounced distinction to the detrimental effect of incorporation of multiwalled carbon nanotubes on polymer orientation in electrospun nanofibers, as reported previously.
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