Pavel Bazant

Microwave solvothermal decoration of the cellulose surface by nanostructured hybrid Ag/ZnO particles: a joint XPS, XRD and SEM study

The synthesis of hybrid silver/zinc oxide (Ag/ZnO) decoration on the cellulose surface is described. The structures were characterized with X-ray photoelectron spectroscopy (XPS) and corroborated with X-ray diffraction and scanning electron microscopy. Silver nitrate and zinc acetate dihydrate were used as soluble raw materials. Hexamethylenetetraamine was used as the precipitating and reducing agent. The surface of α-cellulose was always treated by hydrogen peroxide before synthesis with a relatively mild effect manifested in water contact angle measurement and XPS high-resolution spectra. The Ag/ZnO decoration system was identified as a true nanodispersed metal/semiconductor hybrid with a unique collective plasmonic structure observed on Ag 3d core lines for the first time. A series of experiments with a single precursor solution contributed to the characterization of the interaction of Ag+ and Zn2+ species with the surface and to the description of the reaction mechanism in the mixed precursor solution. In contrast to previous reports, a specific interaction between the cellulose substrate and Zn2+ was observed. No specific non-thermal effects of microwave heating were observed.

Low molecular weight poly(lactic acid) microparticles for controlled release of the herbicide metazachlor: preparation, morphology, and release kinetics.

The preemergence chloroacetamide herbicide metazachlor was encapsulated in biodegradable low molecular weight poly(lactic acid) micro- and submicroparticles, and its release to the water environment was investigated. Three series of particles, S, M, and L, varying in their size (from 0.6 to 8 μm) and with various initial amounts of the active agent (5%, 10%, 20%, 30% w/w) were prepared by the oil-in-water solvent evaporation technique with gelatin as biodegradable surfactant. The encapsulation efficiencies reached were about 60% and appeared to be lower for smaller particles. Generally, it was found that the rate of herbicide release decreased with increasing size of particles. After 30 days the portions of the herbicide released for its highest loading (30% w/w) were 92%, 56%, and 34% for about 0.6, 0.8, and 8 μm particles, respectively. The release rates were also lower for lower herbicide loadings. Metazachlor release from larger particles tended to be a diffusion-controlled process, while for smaller particles the kinetics was strongly influenced by an initial burst release.

The formation mechanism of iron oxide nanoparticles within the microwave-assisted solvothermal synthesis and its correlation with the structural and magnetic properties

Magnetic nanoparticles based on Fe3O4 were prepared by a facile and rapid one-pot solvothermal synthesis using FeCl3·6H2O as a source of iron ions, ethylene glycol as a solvent and NH4Ac, (NH4)2CO3, NH4HCO3 or aqueous NH3 as precipitating and nucleating agents. In contrast to previous reports we reduce the synthesis time to 30 minutes using a pressurized microwave reactor without the requirement of further post-treatments such as calcination. Dramatically reduced synthesis time prevents particle growth via Ostwald ripening thus the obtained particles have dimensions in the range of 20 to 130 nm, they are uniform in shape and exhibit magnetic properties with saturation magnetization ranging from 8 to 76 emu g(-1). The suggested method allows simple particle size and crystallinity tuning resulting in improved magnetic properties by changing the synthesis parameters, i.e. temperature and nucleating agents. Moreover, efficiency of conversion of raw material into the product is almost 100%.

Antibacterial performance of ZnO-based fillers with mesoscale structured morphology in model medical PVC composites

Three different ZnO-based antibacterial fillers having different morphologies in microscale region were prepared by the use of the microwave assisted synthesis protocol created in our laboratory with additional annealing in one case. Further, PVC composites containing 0.5-5 wt.% of ZnO based antibacterial fillers were prepared by melt mixing and characterized by scanning electron microscopy (SEM) and X-ray diffractometry (XRD). Mechanical testing showed no adverse effect on the working of polymer composites due to either of the fillers used or the applied processing conditions in comparison with the neat medical grade PVC. The surface antibacterial activity of the compounded PVC composites was assessed against Escherichia coli ATCC 8739 and Staphylococcus aureus ATCC 6538P according to ISO 22196: 2007 (E). All materials at almost all filler loading levels were efficient against both species of bacteria. The material with the most expanding morphology assuring the largest contact between filler and matrix achieved an excellent level of more than 99.9999% reduction of viable cells of E. coli in comparison to untreated PVC and performed very well against S. aureus, too. A correlation between the morphology and efficacy of the filler was observed and, as a result, a general rule was formulated which links the proneness of the microparticles to perform well against bacteria to their shape and morphology.

Hybrid nanostructured Ag/ZnO decorated powder cellulose fillers for medical plastics with enhanced surface antibacterial activity

Hybrid inorganic–organic fillers based on nanostructured silver/zinc oxide decorations on micro-cellulose carrier particles were prepared by stepwise microwave assisted hydrothermal synthesis using soluble salts as precursors of silver and zinc oxide. Hexamethylenetetramine was used as precipitating agent for zinc oxide and reducing agent for silver. The inorganics covered all available surfaces of the cellulose particles with a morphology resembling a coral reef. Prepared particulate fillers were compounded to medical grade poly(vinyl chloride) matrix. Scanning electron microscopy and powder X-ray diffractometry were used to investigate the morphology and crystalline phase structure of fillers. The scanning electron microscopy was used for morphological study of composites. With respect to prospective application, the composites were tested on electrical and antibacterial properties. A small effect of water absorption in polymer composites on their dielectric properties was observed but no adverse effect of water exposure on prepared materials was manifested. Electrical conductivity of fillers and composites was measured and no influence of water soaking of composites was found at all. The surface antibacterial activity of prepared composites was evaluated according to the standard ISO 22196. Excellent performance against Escherichia coli and very high against Staphylococcus aureus was achieved.

Light-Induced Actuation of Poly(dimethylsiloxane) Filled with Graphene Oxide Grafted with Poly(2-(trimethylsilyloxy)ethyl Methacrylate)

This study serves to combine two approaches into one single step, to achieve a significant improvement of the light-induced actuation capabilities. Graphene oxide (GO) is an inert material, from the electrical and thermal conductivity point of view, and is incompatible with the usually-used poly(dimethylsiloxane) (PDMS) matrix. During surface-modification by surface-initiated atom transfer radical polymerization, the GO was transformed into a conducting and compatible material with the PDMS showing enormous light-induced actuation capability. The GO surface-modification with poly(2-(trimethylsilyloxy)ethyl methacrylate) (PHEMATMS) chains was confirmed by transmission electron microscopy and thermogravimetric analysis, with an on-line monitoring of gasses using FTIR. The improved compatibility was elucidated using contact angle and dielectric properties measurements. The PHEMATMS shell was investigated using gel permeation chromatography and nuclear magnetic resonance. The improved electric conductivity was measured using the four-point probe method and by Raman spectroscopy. The very important mechanical properties were elucidated using dynamic mechanical analysis, and with the help of thermo-mechanic analysis for the light-induced actuation. The excellent actuation capabilities observed, with changes in the length of around 0.8% at 10% pre-strain, are very promising from the point of view of applications.

Synthesis and Effect of Hierarchically Structured Ag-ZnO Hybrid on the Surface Antibacterial Activity of a Propylene-Based Elastomer Blends

In this study, a hybrid Ag-ZnO nanostructured micro-filler was synthesized by the drop technique for used in plastic and medical industry. Furthermore, new antibacterial polymer nanocomposites comprising particles of Ag-ZnO up to 5 wt % and a blend of a thermoplastic polyolefin elastomer (TPO) with polypropylene were prepared using twin screw micro-compounder. The morphology and crystalline-phase structure of the hybrid Ag-ZnO nanostructured microparticles obtained was characterized by scanning electron microscopy and powder X-ray diffractometry. The specific surface area of this filler was investigated by means of nitrogen sorption via the Brunauer-Emmet-Teller method. A scanning electron microscope was used to conduct a morphological study of the polymer nanocomposites. Mechanical and electrical testing showed no adverse effects on the function of the polymer nanocomposites either due to the filler utilized or the given processing conditions, in comparison with the neat polymer matrix. The surface antibacterial activity of the compounded polymer nanocomposites was assessed against Escherichia coli ATCC 8739 and Staphylococcus aureus ATCC 6538P, according to ISO 22196:2007 (E). All the materials at virtually every filler-loading level were seen to be efficient against both species of bacteria.