Vijaya K. Rangari

Synthesis of Ag/CNT hybrid nanoparticles and fabrication of their Nylon-6 polymer nanocomposite fibers for antimicrobial applications

Ag-coated CNTs hybrid nanoparticles (Ag/CNTs) were prepared by ultrasonic irradiation of dimethylformamide (DMF) and silver (I) acetate precursors in the presence of CNTs. The morphology of Ag/CNTs was characterized using x-ray diffraction and transmission electron microscopy (TEM) techniques. The Nylon-6 powder and 1 wt% Ag/CNTs mixture was dispersed uniformly using a noncontact spinning technique. The dried mixture was melted in a single screw extrusion machine and then extruded through an orifice. Extruded filaments were later stretched and stabilized by sequentially passing them through a set of tension adjusters and a secondary heater. The Nylon-6/Ag/CNT hybrid polymer nanocomposite (HPNC) fibers, which were of approximately 80 microm size, were tested for their tensile properties. The failure stress and modulus of the extruded HPNC fibers (doped with 1% Ag/CNTs) was about 72.19 % and 342.62% higher than the neat extruded Nylon-6 fiber, respectively. DSC results indicated an increase in the thermal stability and crystallization for HPNC fibers. The antibacterial activity of the Ag-coated CNTs, commercial Ag, neat Nylon-6 and plain CNTs were evaluated. Ag-coated CNTs at 25 microg demonstrated good antimicrobial activity against four common bacterial pathogens as tested by the Kirby-Bauer assay. The mean diameters of the zones of inhibition were 27.9 +/- 6.72 mm, 19.4 +/- 3.64 mm, 21.9 +/- 4.33 mm, and 24.1 +/- 4.14 mm, respectively, for Staphylococcus aureus, Streptococcus pyogenes, Escherichia coli and Salmonella enterica serovar Typhimurium. By comparison, those obtained using the broad spectrum antibiotic amoxicillin-clavulanic acid were 37.7 +/- 2.13 mm, 28.6 +/- 4.27 mm, 22.6 +/- 1.27 mm, and 27.0 +/- 1.41 mm, respectively, for the same strains. The zones of inhibition obtained for Nylon-6 Ag-coated CNT powder at 25 microg were also high, ranging from 15.2 to 25.3 mm in contrast to commercial silver or neat Nylon-6, which did not inhibit the bacterial strains tested. Further, the Nylon-6 nanocomposite fibers infused with Ag/CNTs inhibited bacterial growth by 11-20%. Our results suggest that nylon nanocomposite fibers infused with Ag-coated CNTs have significant antimicrobial activity.

MANUFACTURING AND CHARACTERIZATION OF CARBON NANOTUBE/POLYETHYLENE COMPOSITES

The present study describes a method to fabricate polymer matrix nanocomposites by reinforcing multi-walled carbon nanotubes through an extrusion process. Linear low density polyethylene (LLDPE) powder and multi-walled carbon nanotubes (CNTs) are first dry mixed and extruded in the form of filaments by a single screw extrusion process. After extrusion, the filament is partially cooled by chilled air, dried, and continuously wound in a spool. The filaments are then laid in roving, stacked in a unidirectional fashion, and consolidated in a compression molding machine to come up with laminated composites. Thermo gravimetric analysis (TGA) has been performed to compare the thermal stability of as-fabricated composites with the neat polymer. The TGA result shows that the extruded composites are thermally more stable than their neat counterparts. The crystalline nature of CNTs and of as-fabricated composites were identified by X-ray diffraction (XRD) studies. The XRD results indicate that the nanocomposite materials are more crystalline than the neat systems, and the differential scanning calorimetry studies also confirmed the same trend. The scanning electron microscopy result showed that the sizes of extruded neat and nanophased filaments were about 117 and 73 µm, respectively. Tensile coupons from the consolidated panels were then extracted both in longitudinal (0◦) and in transverse (90◦) directions and tested in a Minimat Tester. It was found that with the addition of 2% by weight of CNTs in LLDPE, the tensile strength and modulus of the composite has increased by about 34 and 38%, respectively. The (0◦ )a nd (90 ◦) coupons have also demonstrated that there are directional effects in the tensile response, which is believed to have been caused by the alignment of CNTs during the extrusion process. It is our understanding that such improvement in properties is because of the increase in crystallinity of the polymer due to CNT infusion, and also due to the alignment of CNTs in the extrusion direction in the nanocomposites.

Enhanced stab resistance of armor composites with functionalized silica nanoparticles

Traditionally shear thickening fluid (STF) reinforced with Kevlar has been used to develop flexible armor. At the core of the STF-Kevlar composites is a mixture of polyethylene glycol (PEG) and silica particles. This mixture is often known as STF and is consisted of approximately 45 wt % PEG and 55 wt % silica. During rheological tests, STF shows instantaneous spike in viscosity above a critical shear rate. Fabrication of STF-Kevlar composites requires preparation of STF, dilution with ethanol, and then impregnation with Kevlar. In the current approach, nanoscale silica particles were dispersed directly into a mixture of PEG and ethanol through a sonic cavitation process. Two types of silica nanoparticles were used in the investigation: 30 nm crystalline silica and 7 nm amorphous silica. The admixture was then reinforced with Kevlar fabric to produce flexible armor composites. In the next step, silica particles are functionalized with a silane coupling agent to enhance bonding between silica and PEG. The ...

Sonochemical synthesis and rheological properties of shear thickening silica dispersions.

A sonochemical method has been developed to synthesize shear thickening fluid. This shear thickening fluid (STF) is composed of hard silicon dioxide nanoparticles and polyethylene glycol (PEG) liquid polymer. The combination of flow-able and hard components at a particular composition, results a material with remarkable rheological properties that is suitable for liquid body armor applications. In the present study nine types of STFs have been synthesized with two different types of silica nanoparticles (15 nm and 200 nm) and polyethylene glycol at various weight fractions using a high intensity ultrasonic irradiation. The resultant STF samples were tested for their rheological and thermal properties. The advantages and disadvantages of this process have been discussed.

Synthesis and Characterization of Diamond-Coated CNTs and Their Reinforcement in Nylon-6 Single Fiber

Diamond nanoparticle (DN)-coated CNTs were synthesized using a cationic surfactant-assisted sonochemical method. The as-prepared DN coated CNTs were characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). The results show that the DNs were coated on the outer wall surface of CNTs. The DN-coated CNTs were infused in Nylon-6 polymer through a melt extrusion process to form nanocomposite fibers that were tested for their tensile properties. The ultimate tensile strength is found to be 363 MPa for DN/CNTs/Nylon-6 single fibers as compared to 240 MPa for neat Nylon-6 single fibers. These results were also compared with Nylon-6 fibers infused with pristine CNTs and pristine DNs.

Nanoengineered Eggshell–Silver Tailored Copolyester Polymer Blend Film with Antimicrobial Properties

In this study, the reinforcement effect of different proportions of eggshell/silver (ES-Ag) nanomaterial on the structural and antimicrobial properties of 70/30 poly(butylene-co-adipate terephthalate)/polylactic acid (PBAT/PLA) immiscible blends was investigated. The ES-Ag was synthesized using a single step ball milling process and characterized with X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). These results confirmed the existence of silver nanoparticles (Ag NPs) in the interstitial spaces of the eggshell particles. The thin films in this study were prepared using hot melt extrusion and 3D printing for mechanical and antimicrobial testing, respectively. These films were also characterized by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), XRD, tensile testing, and antimicrobial analysis. It was found that the incorporation of ES-Ag (0.5-2.0% content) compromised the tensile properties of the blend, due to poor interaction between the matrix and the ES-Ag in the ternary systems, but thermal analysis revealed improvement in the onset of degradation temperature and char yield at 500 °C. Though film toughness was better than that of PLA, the strength was lower, yet synergistic to those of PBAT and PLA. In general, the PBAT/PLA/ES-Ag ternary system had properties intermediate to those of the pure polymers. In vitro assessment of the antimicrobial activity of these films conducted on Listeria monocytogenes and Salmonella Enteritidis bacteria revealed that the blend composite films possessed bacteriostatic effects, due to the immobilized ES-Ag nanomaterials in the blend matrix. Atomic absorption spectroscopy (AAS) analysis of water and food samples exposed to the films showed that Ag NPs were not released in distilled water and chicken breast after 72 and 168 h, respectively.

In Situ Strategy to Encapsulate Antibiotics in a Bioinspired CaCO3 Structure Enabling pH-Sensitive Drug Release Apt for Therapeutic and Imaging Applications

Herein we demonstrate a bioinspired method involving macromolecular assembly of anionic polypeptide with cationic peptide-oligomer that allows for in situ encapsulation of antibiotics like tetracycline in CaCO3 microstructure. In a single step one-pot process, the encapsulation of the drug occurs under desirable environmentally benign conditions resulting in drug loaded CaCO3 microspheres. While this tetracycline-loaded sample exhibits pH dependent in vitro drug-release profile and excellent antibacterial activity, the encapsulated drug or the dye-conjugated peptide emits fluorescence suitable for optical imaging and detection, thereby making it a multitasking material. The efficacy of tetracycline loaded calcium carbonate microspheres as pH dependent drug delivery vehicles is further substantiated by performing cell viability experiments using normal and cancer cell lines (in vitro). Interestingly, the pH-dependent drug release enables selective cytotoxicity toward cancer cell lines as compared to the normal cells, thus having the potential for further development of therapeutic applications.

Fabrication of carbon nanotubes grown woven carbon fiber/epoxy composites and their electrical and mechanical properties

Multiwall carbon nanotubes (CNTs) were directly grown on woven carbon fibers using chemical vapor deposition technique and iron acetate as a catalyst. These CNTs grown woven carbon fibers were further infused with epoxy resin to fabricate fiber reinforced nanocomposites. Both electric and mechanical properties of these composites were studied and found that the electric resistivity of composite reduced significantly as the amount of CNTs on woven carbon fiber increased. For the neat composite without CNTs, the resistivity observed was 25 Ω·m, while it was only 0.2 Ω·m for the composite with 3.3 wt. % of CNTs grown on woven carbon fiber. The flexure test results showed a 34% increase in strength and 126% increase in stiffness for 1.65 wt. % CNTs grown on woven carbon fiber.

Biomaterial-Derived Calcium Carbonate Nanoparticles for Enteric Drug Delivery

Oral drug delivery systems provide the most convenient, noninvasive, readily acceptable alternatives to parenteral systems. In the current work, eggshell-derived calcium carbonate (CaCO3) nanoparticles were used to develop enteric drug delivery system in the form of tablets. CaCO3 nanoparticles were manufactured using top-down ball-milling method and characterized by X-ray diffractometry (XRD) and transmission electron microscopy (TEM) and loaded with 5-fluorouracil as a model drug. Tablets with varying CaCO3 core and binder compositions were fabricated and coated with Eudragit S100 or Eudragit L100. Suitability for enteric delivery of the tablets was tested by oral administration to rabbits and radiography. Radiograph images showed that the tablet remained in the stomach of the rabbit for up to 3 hours. Further modifications of these biomaterial-derived nanoparticles and the coatings will enable manufacturing of stable formulations for slow or controlled release of pharmaceuticals for enteric delivery.

Synthesis and Characterization Silver, Zinc Oxide and Hybrid Silver/Zinc Oxide Nanoparticles for Antimicrobial Applications

Silver (Ag) and zinc oxide (ZnO) are well known for both antimicrobial and pro-healing properties. Here, we present a novel method to synthesize Ag and ZnO nanoparticles (NPs), as well as hybrid Ag/ZnO NPs using a custom, temperature controlled microwave assisted technique. Microwave synthesis has been shown not only to enhance the rate of chemical reactions, but also in some cases to give higher product yields over thermal heating. The as-synthesized NPs were characterized by X-ray diffraction (XRD) to study the crystalline structure, composition and purity. Transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) was used to study particle size, shape, composition and morphology. These results indicated that the as-prepared Ag NPs are spherical in shape and ~ 20 nm in sizes. The ZnO NPs are typically rod shaped and the particle sizes are ~ 20 nm in width and 100 nm in length. These NPs were tested for antibacterial and/or antifungal properties using disc diffusion assays. Results ...