Electrochemical exfoliation is a promising bulk method for producing graphene from graphite; in this method, an applied voltage drives ionic species to intercalate into graphite where they form gaseous species that expand and exfoliate individual graphene sheets. However, a number of obstacles have prevented this approach from becoming a feasible production route; the disintegration of the graphite electrode as the method progresses is the chief difficulty. Here we show that if graphite powders are contained and compressed within a permeable and expandable containment system, the graphite powders can be continuously intercalated, expanded, and exfoliated to produce graphene. Our data indicate both high yield (65%) and extraordinarily large lateral size (>30 μm) in the as-produced graphene. We also show that this process is scalable and that graphene yield efficiency depends solely on reactor geometry, graphite compression, and electrolyte transport.
Recent developments in the exfoliation, dispersion, and processing of pristine graphene (i.e., non-oxidized graphene) are described. General metrics are outlined that can be used to assess the quality and processability of various "graphene" products, as well as metrics that determine the potential for industrial scale-up. The pristine graphene production process is categorized from a chemical engineering point of view with three key steps: i) pretreatment, ii) exfoliation, and iii) separation. How pristine graphene colloidal stability is distinct from the exfoliation step and is dependent upon graphene interactions with solvents and dispersants are extensively reviewed. Finally, the challenges and opportunities of using pristine graphene as nanofillers in polymer composites, as well as as building blocks for macrostructure assemblies are summarized in the context of large-scale production.
Here, we give the first-ever report of radio frequency (RF) electromagnetic heating of polymer nanocomposite materials via direct-contact and capacitively coupled electric field applicators. Notably, RF heating allows nanocomposite materials to be resistively heated with electric fields. We highlight our novel RF heating technique for multiwalled carbon nanotube (MWCNT) thermoplastic composites and measure their broadband dielectric properties. We also demonstrate three different electric field applicator configurations and discuss their practical use in an industrial setting. We demonstrate the use of RF heating to cure an automotive-grade epoxy loaded with MWCNTs. Our results show that lap shear joints cured faster with the RF method compared with control samples cured in an oven because of the heat-transfer advantages of directly heating the epoxy composite. Finally, we implement our RF curing technique to assemble an automotive structure by locally curing an epoxy adhesive applied to a truck chassis.
Here we demonstrate an oven-free and mold-free heating route to convert preceramic polymers to silicon carbide using carbon nanomaterials as susceptors. Silicon carbide is prized for its high thermal stability and low density and could be produced via slow oven heating of polycarbosilane (PCS). We show that addition of multiwalled carbon nanotubes (MWCNT) as susceptors to polycarbosilane results in rapid and volumetric heating upon exposure to microwaves and radio frequency. We assess microwave heating of polycarbosilane-MWCNT composites; this process is capable of reaching pyrolysis temperatures, and the resulting crystal structure is cubic (-SiC). We measure dielectric properties of these composites in the radio frequency range. We cure these composites using RF, and thermogravimetric data shows that the extent of cure for these samples is around 95 %. We demonstrate the applicability of this study for 3D printing silicon carbides by successive iterations of layer deposition and rapid RF curing. We performed on the fly measurements of dielectric values of the 3D printing ink at different temperature while curing it.We have also shown that these volumetric heating methods can rapidly cure polycarbosilane fibers to make silicon carbide fibers without melting them before crosslinking.
Material
extrusion (ME) 3D printing is a revolutionary technique
for manufacturing thermoplastic parts; however, the printed parts
typically suffer from poor interlayer bonding, which causes weak tensile
strength in the build direction. Many methods have been proposed to
address the mechanical deficiencies of 3D-printed parts, but most
fall short of a production-ready solution. Here we report the use
of a dielectric barrier discharge (DBD) plasma electrode mounted concentrically
around the nozzle of an ME 3D printer for in situ welding of thermoplastic parts. This is the first report of a DBD
being used as a non-contact means to induce Joule heating in resistive
composite materials. The polymer welding process is accomplished by
coupling the DBD with the carbon nanotube-loaded interfaces between
the 3D-printed layers. The current passing through the part results
in rapid resistive heating of the nanotubes and thermal welding of
the interfaces. We show that parts printed with this method have isotropic
strength and are equivalent to their injection-molded counterparts.
Scalable production of graphene through liquid-phase exfoliation has been plagued by low yields. Although several recent studies have attempted to improve graphene exfoliation technology, the problem of separating colloidal nanosheets from unexfoliated parent material has received far less attention. Here we demonstrate a scalable method for improving nanosheet yield through a facile washing process. By probing the sedimentation of liquid-phase exfoliated slurries of graphene nanosheets and parent material, we found that a portion of exfoliated graphene is entrapped in the sediment, but can be recovered by repeatedly washing the slurry of nanosheet and parent material with additional solvent. We found this process to significantly increase the overall yield of graphene (graphene / parent material) and recover a roughly constant proportion of graphene with each wash. The cumulative amount of graphene recovered is only a function of total solvent volume. Moreover, we found this technique to be applicable to other types of nanosheets such as boron nitride nanosheets.
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