Graphene has been publicized as the game changing material of this millennium. To this day, scalable production leading to exceptional material properties has been difficult to attain. Most methods require harsh chemicals, which result in destroying the graphene surface. A method was developed, exploiting high speed elongational flow in a novel designed batch mixer; creating a distribution of pristine few to many layer graphene flakes. The method focuses on exfoliating in a molten polyamide 66 (PA66) matrix, creating a graphene reinforced polymer matrix composite (G-PMC). The process revealed that high speed elongational flow was able to create few layer graphene. Graphite exfoliation was found driven in part by diffusion, leading to intercalation of PA66 in graphite. The intercalated structure lead to increases in the hydrogen bonding domain, creating anisotropic crystal domains. The thermal stability of the G-PMC was found to be dependent to the degree of exfoliation, PA66 crystal structure and composite morphology. The aim of this research is to characterize uniquely produced graphene containing polymer matrix composites using a newly created elongational flow field. Using elongational flow, graphite will be directly exfoliated into graphene within a molten polymer.
Effective methods are needed to fabricate the next generation of high-performance graphene-reinforced polymer matrix composites (G-PMCs). In this work, a versatile and fundamental process is demonstrated to produce high-quality graphene-polymethylmethacrylate (G-PMMA) composites via in situ shear exfoliation of well-crystallized graphite particles loaded in highly-viscous liquid PMMA/acetone solutions into graphene nanoflakes using a concentric-cylinder shearing device. Unlike other methods where graphene is added externally to the polymer and mixed, our technique is a single step process where as-exfoliated graphene can bond directly with the polymer with no contamination/handling. The setup also allows for the investigation of the rheology of exfoliation and dispersion, providing process understanding in the attainment of the subsequently heat injection-molded and solidified G-PMC, essential for future manufacturing scalability, optimization, and repeatability. High PMMA/acetone concentration correlates to high mixture viscosity, which at large strain rates results in very-high shear stresses, producing a large number of mechanically-exfoliated flakes, as confirmed by liquid-phase UV–visible spectral analysis. Raman spectroscopy and other imaging evince that single- and bi-layer graphene are readily achieved. Nevertheless, a limit is reached at high mixtures viscosities where the process becomes unstable as non-Newtonian fluid behavior (e.g. viscoelastic) dominates the system. Characterization of microstructure, morphology, and properties of this new class of nanostructured composites reveals interesting trends. Observations by transmission electron microscopy, scanning electron microscopy, and helium ion microscopy of the manufactured G-PMCs show uniform distributions of unadulterated, well-bonded, discontinuous, graphene nanoflakes in a PMMA matrix, which enhances stiffness and strength via a load-transfer mechanism. Elastic modulus of 5.193 GPa and hardness of 0.265 GPa are achieved through processing at 0.7 g ml−1 of acetone/PMMA for 1% wt. starting graphite loading when injected into a sample mold at 200 °C. Mechanical properties exhibit 31% and 28.6% enhancement in elastic modulus and hardness, respectively, as measured by nano-indentation.
Polymer nanocomposites possess unique sets of properties that make them suitable for different applications, including structural and flame-retardant material, electromagnetic wave reflector, sensors, thin film transistor, flexible display, and many more. The properties of these nanocomposite are dependent on nanofiller dispersion and bonding with polymer matrix (i.e. particle-matrix interaction). Thermography is a non-destructive method that may be used to gain insight into dispersion and particle-matrix interaction. Infrared (IR) radiation emitted from these nanomaterial polymer composite depends on the emissivity of the individual components. In addition, during flash heating and cooling, different thermal conductivity of components in the nanocomposite can influence pixel intensity differently in the IR image or video being captured. We have used an economical mid wavelength IR camera Fluke RSE600 equipped with a close-up macro lens and algorithm based on MATLAB image processing toolbox to analyse dispersion, voids and thermal diffusivity of patented graphene polymer nanocomposite materials (G-PMC) in micro-scale. These G-PMCs can act as a standard material to determine the potential of our IR thermography technique due to their homogeneity and lack of impurity due to unique fabrication process. Thermal diffusivity and dispersion of nanoparticles in our G-PMCs was estimated after irradiation with a xenon flash lamp by spatially mapping transient IR radiations from different G-PMCs using the Fluke RSE600 thermal imager. Results from thermography experiments were compared with scanning electron microscope (SEM) and Raman spectroscopy results. Micro-scale thermography was able to detect millimetre scale thermal diffusivity variation in the injection molded G-PMC samples and relate it to change in dispersion of nanofillers, unlike SEM and Raman, where micro-scale measurements could not determine the reason behind millimetre scale property variation. We believe this low cost, fast, micro-scale, non-destructive technique will provide valuable insight into functional polymer nanocomposite fabrication and corresponding electrical and thermal properties.
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