We study the depth sensitivity and spatial resolution of subsurface imaging of polymer nanocomposites using second harmonic mapping in Kelvin Probe Force Microscopy (KPFM). This method allows the visualization of the clustering and percolation of buried Single Walled Carbon Nanotubes (SWCNTs) via capacitance gradient (∂C/∂z) maps. We develop a multilayered sample where thin layers of neat Polyimide (PI) (∼80 nm per layer) are sequentially spin-coated on well-dispersed SWCNT/Polyimide (PI) nanocomposite films. The multilayer nanocomposite system allows the acquisition of ∂C/∂z images of three-dimensional percolating networks of SWCNTs at different depths in the same region of the sample. We detect CNTs at a depth of ∼430 nm, and notice that the spatial resolution progressively deteriorates with increasing depth of the buried CNTs. Computational trends of ∂C/∂z vs CNT depth correlate the sensitivity and depth resolution with field penetration and spreading, and enable a possible approach to three-dimensional subsurface structure reconstruction. The results open the door to nondestructive, three-dimensional tomography and nanometrology techniques for nanocomposite applications.
High-resolution sub-surface imaging of carbon nanotube (CNT) networks within polymer nanocomposites is demonstrated through electrical characterization techniques based on dynamic atomic force microscopy (AFM). We compare three techniques implemented in the single-pass configuration: DC-biased amplitude modulated AFM (AM-AFM), electrostatic force microscopy (EFM) and Kelvin probe force microscopy (KPFM) in terms of the physics of sub-surface image formation and experimental robustness. The methods were applied to study the dispersion of sub-surface networks of single-walled nanotubes (SWNTs) in a polyimide (PI) matrix. We conclude that among these methods, the KPFM channel, which measures the capacitance gradient (∂C/∂d) at the second harmonic of electrical excitation, is the best channel to obtain high-contrast images of the CNT network embedded in the polymer matrix, without the influence of surface conditions. Additionally, we propose an analysis of the ∂C/∂d images as a tool to characterize the dispersion and connectivity of the CNTs. Through the analysis we demonstrate that these AFM-based sub-surface methods probe sufficiently deep within the SWNT composites, to resolve clustered networks that likely play a role in conductivity percolation. This opens up the possibility of dynamic AFM-based characterization of sub-surface dispersion and connectivity in nanostructured composites, two critical parameters for nanocomposite applications in sensors and energy storage devices.
Four new zinc complex derivatives of azoles and ligands were synthesized and isolated as white air-stable solids and characterized by elemental analyses, thermogravimetric analysis (TGA), infrared spectroscopy, nuclear magnetic resonance (NMR) and mass spectra. The elemental analysis, theoretical calculations and NMR show that the complexes likely have a 1:1 (M:L) stoichiometry and tetrahedral geometry. To evaluate the biological activity of the complexes and to discuss the role of metal ions and structural properties, the ligands and their metal complexes have been studied. Their antimicrobial activity was determined in vitro by agar-well diffusion and broth microdilution against nine bacterial strains and seven fungal strains with clinical relevance. In vitro assays showed that the complexes exhibited moderate antibacterial and/or antifungal activities. The antimicrobial activity was found to be more active for the metal complexes than the ligands. The metal complexes that contained copper and cobalt, respectively, displayed notable antibacterial and antifungal effects against all the tested bacterial strains. The minimum inhibitory concentration 50 (MIC 50 ) values were in the range 2454-0.7 μg mL -1 . Metal complexes were more effective at inhibiting bacteria than fungi. The results could provide a high-potential solution for antimicrobial growth resistance, for both bacteria and fungi.
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