Preparation of Gadolina Stabilized Bismuth Oxide Doped with Boron via Electrospinning Technique

In this study, boron doped and undoped poly (vinyl) alcohol/bismuth–gadolina acetate (PVA/Bi–Gd) nanofibers were prepared using electrospinning technique then calcinated at 800 °C for 2 h. The originality of this study is the addition of boron to metal acetates. The effects of boron doping were investigated in terms of solution properties, morphological changes and thermal characteristics. The characteristics of the fibers were investigated with FT-IR, XRD, SEM and BET. The addition of boron did not only increase the thermal stability of the fibers, but also their diameters, which yielded stronger fibers. XRD analyses showed that boron doping increased the peak intensities and indicated that the boron doping enhanced the crystallite size. Moreover, no shifts were noticed in diffraction angles for boron doped and undoped samples. Therefore, boron doping did not significantly alter the lattice spacing. The SEM micrograph of the fibers showed that the addition of boron resulted in the formation of cross-linked bright-surfaced fibers. The average fiber diameter for boron doped and undoped fiber mats were 204 and 123 nm, respectively. Also, grain diameters of boron doped and undoped nanocrystalline sintered powders were measured as 140 and 118 nm, respectively. The BET results showed that boron undoped and doped Bi₂O₃–La₂O₃ nanocrystalline powder ceramic structures sintered at 800 °C have surface areas of 59.72 and 39.80 m²/g, respectively.     

Synthesis and characterization of boron-doped Bi2O3 - La2O3 fiber derived nanocomposite precursor

Boron doped poly(vinyl) alcohol/ bismuth - lanthanum acetate (PVA/Bi-La) nanofibers were prepared by electrospinning using PVA as a precursor. The effect of boron doping was investigated in terms of solution properties, morphological changes and thermal characteristics. The fibers were characterized by FT-IR, XRD, SEM and BET. The addition of boron did not only increase the thermal stability of the fibers, but also their diameters, which yielded stronger fibers. XRD analyses showed that boron doping increased the peak intensities and indicated that the boron doping enhanced the crystallite size. Moreover, no shifts were noticed in diffraction angles for boron doped and undoped samples. Therefore, boron doping did not significantly alter the lattice spacing. The SEM micrograph of the fibers showed that the addition of boron resulted in the formation of cross linked bright surfaced fibers. Also, grain diameters of boron doped and undoped nanocrystalline sintered powders were measured as 170 nm and 120 nm respectively. The BET results show that boron undoped and doped Bi₂O₃-La₂O₃ nanocrystalline powder ceramic structures sintered at 800 °C have surface areas of 20.44 m²/g and 12.93 m²/g, respectively.     

Heterogeneous photodecolorization of mixture of methylene blue and bromophenol blue using CuO-nano-clinoptilolite

CuO was incorporated into nano-particles of clinoptilolite via ion exchange and calcination processes. The obtained composite (CuO-NCP) was used for the photodeclorization process of an aqueous mixture of Methylene Blue and Bromophenol Blue. All samples were characterized by FT-IR, XRD, DRS, SEM and SEM. The optimum conditions were approximated as: 7 ppm dyes, pH 5.9, catalyst dose of 0.2 g L⁻¹ and CuO loading of 4.9%. The declorization extents of 61% and 32% were respectively obtained for MB and BPB during 180 min irradiation. The degradation extent was monitored by UV–vis spectroscopy and confirmed by chemical oxygen demand (COD).     

Radiation synthesis and characterization of poly(vinyl alcohol)/poly(N-vinyl-2-pyrrolidone) based hydrogels containing silver nanoparticles

A series of PVA/PVP based hydrogels at different compositions were prepared by gamma irradiation. The gel fraction degree of swelling were investigated. Highly stable and uniformly distributed silver nanoparticles have been obtained onto hydrogel networks. The morphology and structure of (PVA/PVP) hydrogel and dispersion of the silver nanoparticles in the polymeric matrix were examined by scanning electron microscopy (SEM) and infrared spectroscopy (FT-IR), respectively. The formation of silver nanoparticles has been confirmed by ultraviolet visible (UV–vis) spectroscopy. A strong characteristic absorption peak was found to be around 420 nm for the silver nanoparticles in the hydrogel nanocomposite. The X-ray diffraction pattern confirmed the formation of silver nanoparticles with average particle size of 12 nm. The diameter distribution of silver nanoparticles was determined by dynamic light scattering DLS. Transmission electron microscope (TEM) showed almost spherical and uniform distribution of silver nanoparticles through the hydrogel network and the mean size of silver nanoparticles ranging is 23 nm. The good swelling properties and antibacterial of PVA/PVP-Ag hydrogel suggest that it can be a good candidate as wound dressing.     

ITO electrode modified by self-assembling multilayer film of polyoxometallate on poly(vinyl alcohol) nanofibers and its electrocatalytic behavior

Poly(vinyl alcohol) (PVA) nanofiber mats were collected on indium tin oxide (ITO) substrate by electrospinning method. A multilayer film composed of α-[P₂W₁₈O₆₂]⁶⁻ (abbr. P₂W₁₈), a polyoxometallate (POM) anion, and poly(diallymethylammonium chloride) (abbr. PDDA) was fabricated by layer-by-layer (LBL) self-assembly technique on the PVA/ITO electrode. The PDDA/P₂W₁₈ multilayer film could be unselectively or selectively deposited on the PVA/ITO electrode via changing the amount of PVA nanofibers on the ITO substrate. The scanning electron microscope (SEM) images showed that when the electrospun time was short the PDDA/P₂W₁₈ multilayer film was unselectively deposited on PVA nanofiber mats because the amount of PVA nanofibers was too little to cover most of the ITO substrate. However, when the electrospun time was long enough, the PDDA/P₂W₁₈ multilayer film was selectively deposited on PVA nanofiber mats because of the larger surface area and higher surface energy of PVA nanofibers in comparison with the flat ITO substrate. Growth process of the multilayer film was determined by cyclic voltammetry (CV). Electrocatalytic effects of the PDDA/P₂W₁₈ multilayer film unselectively and selectively deposited on the PVA/ITO electrode on NO₂⁻ were observed.     

Facile preparation and characterization of poly(vinyl alcohol)/chitosan/graphene oxide biocomposite nanofibers

Poly(vinyl alcohol) (PVA)/chitosan (CS)/graphene oxide (GO) biocomposite nanofibers have been successfully prepared using aqueous solution by electrospinning. CS colloidal gel in 1% acetic acid can be changed to homogeneous solution by using electron beam irradiation (EBI). The uniform distributions of GO sheets in the nanofibers were investigated by field emission scanning electron microscopy (FESEM) and Raman spectroscopy. FESEM images illustrated that the spread single GO sheet embedding into nanofibers was formed via self-assembly of GO sheet and PVA/CS chains. And the average diameters of the biocomposite nanofibers decreased (200, 173, 160 and 123 nm) with increasing the contents of GO (0.05, 0.2, 0.4 and 0.6 wt%). Raman spectra verified the presence of GO in the biocomposite nanofibrous mats. The mechanical properties of as-prepared materials related with GO contents. It revealed that the highest tensile strength was 2.78 MPa, which was 25% higher than that of neat PVA/CS nanofibers. Antibacterial test demonstrated that the addition of GO to PVA/CS nanofiber had great ability to increase inhibition zone till 8.6 mm. Overall, these features of PVA/CS/GO nanofibers which were prepared by eco-friendly solvent can be a promising candidate material in tissue engineering, wound healing and drug delivery system.     

Radiation synthesis of graphene oxide/composite hydrogels and their ability for potential dye adsorption from wastewater

A high yield of graphene oxide (GO) was chemically synthesized from graphite powder utilizing adjusted Hummer's method. The contents of acidic functional groups in GO were determined using potentiometric titration. Composite hydrogels dependent on graphene oxide/poly(2-acrylamido-2-methylpropanesulfonic acid)/polyvinyl alcohol (GO/PAMPS/PVA) were synthesized utilizing a ⁶⁰Co gamma irradiation source at different doses. The synthesized graphene oxide and composite hydrogels were portrayed via X-ray diffraction, thermogravimetric analysis, and Fourier transform infrared analysis. The morphology of composite hydrogels was characterized by scanning electron microscope. The gel % and swelling % for the prepared hydrogel demonstrated that the swelling % of hydrogel increased with raising AMPS content. Whereas the increment of GO and increasing the irradiation dose lead to a reduction in the swelling %. The influences of pH, GO percentage, initial dye concentration, the adsorbent dosage, contact time, and temperature on the adsorption of basic blue 3 dye were evaluated and the adsorption capacity was 194.6 mg/g at optimum conditions; pH = 6, GO/PAMPS/PVA composite hydrogels with 5 wt% of GO, initial dye concentration = 200 mg/L, adsorbent dose = 0.1 g, solution volume = 50 mL after 360 min at room temperature (25°C). The adsorption of dye onto the GO/PAMPS/PVA composite hydrogels follows Pseudo-second-order adsorption kinetics, fits the Freundlich adsorption isotherm model.     

Biodegradability, antimicrobial activity and properties of PVA/PVP hydrogels prepared by γ-irradiation

Polyvinyl alcohol/polyvinyl pyrrolidone (PVA/PVP) hydrogel has been prepared by using γ-irradiation technique. In the present study the conclusion on miscibility of PVA/PVP blends, confirmed qualitatively and quantitatively by using Fourier transform infrared spectroscopy and differential scanning calorimetry, respectively. PVA and PVP are found to form a thermodynamically miscible pair. The physical properties such as gel fraction and water absorption performance of the prepared hydrogels were measured, it was found that the gel fraction increases with increasing irradiation dose while the swelling of PVA/PVP blended hydrogels nearly tends to increase with increasing PVP content and reduced with enhanced irradiation doses. The hydrogel pore structure of various PVA/PVP compositions were tested with SEM. Ability of PVA/PVP hydrogels to absorb and release antimicrobial compounds was tested using amoxicillin as an antibacterial and ketoconazole as an antifungal. Antimicrobial activity of PVA/PVP hydrogels was examined using four bacteria, and four fungi. No antibacterial or antifungal activities of non-loaded PVA/PVP of various compositions were detected while the loading ones found to have antimicrobial activity. Results showed resistance of Pseudomonas aeruginosa and Candida albicans to PVA/PVP, while Bacillus subtilis was very sensitive. Biodegradation of PVA/PVP hydrogels was investigated by burial method in two types of local soils (clay and sandy soils). The highest degradation rate was found to be achieved using clay soil. Also, effect of irradiation dose on its biodegradability was tested. The results showed that the radiation prepared PVA/PVP hydrogels can be use as biomaterials.     

Preparation of a PVA/HAP composite polymer membrane for a direct ethanol fuel cell (DEFC)

A novel PVA/Hydroxyapatite (HAP) composite polymer membrane was prepared by the direct blend process and solution casting method. The characteristic properties of the PVA/HAP composite polymer membranes were investigated using thermal gravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM), micro-Raman spectroscopy and the AC impedance method. An alkaline direct ethanol fuel cell, consisting of an air cathode with MnO₂ carbon inks based on Ni-foam, an anode with PtRu black on Ni-foam, and the PVA/HAP composite polymer membrane, was assembled and investigated. It was found that the alkaline direct ethanol fuel cell comprising of a novel cheap PVA/HAP composite polymer membrane showed an improved electrochemical performance in ambient temperature and air. As a result, the maximum power density of the alkaline DEFC, using a PtRu anode based on Ni-foam (10.74 mW cm⁻²), is higher than that of DEFC using an E-TEK PtRu anode based on carbon (7.56 mW cm⁻²) in an 8M KOH + 2M C₂H₅OH solution at ambient temperature and air. These PVA/HAP composite polymer membranes are a potential candidate for alkaline DEFC applications.     

Preparation and electrochemical investigation of the polyaniline/activated carbon nanocomposite for supercapacitor applications

The polyaniline (PANI)/activated carbon (AC) nanocomposite electrodes were prepared by electropolymerization of aniline monomers on the surface of AC/polyvinyl alcohol (PVA) electrodes for supercapacitor studies. Fourier transforms infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and scanning electron microscopy (SEM) analyses were performed to characterize the structure and morphology of the nanocomposite electrodes. The electrochemical properties of the prepared nanocomposite electrodes and the supercapacitive behavior of the PANI, AC, and AC/PANI/PVA electrodes were investigated using cyclic voltammetry (CV) and galvanostatic charge/discharge measurements, respectively. Morphological studies showed that a thin film of PANI has been uniformly deposited on the porous surface of AC electrode, and an ordered arrangement of nanostructures with interlinked porous network has been made. Electrochemical measurements showed that AC particles prevent the degradation of PANI chains during charge/discharge cycles. The specific capacitance of the AC/PANI/PVA nanocomposite electrode was 338.15 F/g which is higher than that of the pristine AC electrode (0.08 F/g). This is due to the contribution of PANI chains by their pseudocapacitance (redox reaction) properties. Although the specific capacitance of PANI electrode (378.57 F/g) was greater than that of the nanocomposite electrode, the cyclic stability of the PANI electrode was lower than that of the AC/PANI/PVA nanocomposite electrode.     

A water-soluble organic-inorganic hybrid material based on polyhedral oligomeric silsesquioxane and polyvinyl alcohol

A novel series of organic-inorganic hybrid materials involving cage-like octa(3-chloroammoniumpropyl)silsesquioxane and Polyvinyl alcohol (OCAPS/PVA) were prepared via solution blending method. The obtained hybrid films were optically transparent and soluble in water. OCAPS/PVA hybrids were characterized by FT-IR, wide-angle X-ray diffraction (WAXD) scanning electronic microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), differential scanning calorimetry (DSC), thermogravimetry analysis (TGA) and tensile test. The results showed that the hydrogen bond interactions were formed between OCAPS and PVA. OCAPS could be dispersed well in PVA matrix till its content was 10 wt%, while the aggregation and crystallization of OCAPS were observed when the content was up to 15 wt%. The glass transition temperature (T _g ) of OCAPS/PVA was found to increase from 53 °C to 60 °C, and the melting temperature (T _m ) decreased from 180 °C to 171 °C with increasing OCAPS content from 0 wt% to 15 wt%. The thermal stability of PVA main chain was improved by the addition of OCAPS and the thermal residue ratio also increased. The tensile strength of OCAPS/PVA decreased from 28 MPa to 19 MPa, while the elongation at break of hybrid films increased from 121% to 175%.     

Fabrication of blend biodegradable nanofibrous nonwoven mats via multi-jet electrospinning

A series of blend biodegradable nanofibrous mats comprising poly(vinyl alcohol) (PVA) and cellulose acetate (CA) were prepared via multi-jet electrospinning. A relative high voltage (20 kV) was used to supply the power for multi-jet electrospinning. The weight ratio of PVA/CA in blend nanofibrous mats can be controlled by changing the number ratio of jets of PVA/CA. Moreover, the real composition of PVA and CA in blend nanofibrous mats was determined by immersing the blend nanofibrous mats into water to remove the PVA component. Morphology, dispersibility, and mechanical properties of blend nanofibrous mats were examined by field emission scanning electron microscopy (FE-SEM), Fourier transform infrared (FT-IR) spectroscopy, wide-angle X-ray diffraction (WAXD), and tensile test. The results showed that the blend nanofibrous mats have good dispersibility. Additionally, the mechanical properties of blend nanofibrous mats were largely influenced by the weight ratio of PVA/CA in blends. Potential applications of the blend nanofibrous mats include filters and biomedical materials.     

Microwave assisted improvement in physico-mechanical properties of poly(vinyl alcohol)/poly(ethylene imine)/gelatin blends

Blends of poly (vinyl alcohol) (PVA), poly-N-acyl ethyleneimine (PEI) and gelatin (PVA/ PEI/Gel) in the weight ratios 100/0/2, 95/5/2, 90/10/2, 85/15/2, 80/20/2 and 70/30/2 were prepared by solution casting method. The effects of poly (ethylene imine) component in the blend and microwave irradiation on the mechanical and microstructural properties have been investigated using various techniques along with Positron Annihilation Lifetime Spectroscopy (PALS). We observed tremendous improvement in mechanical properties after microwave irradiation for 60 s in 5 wt% of PEI component blend. These results are supported by the SEM data as well the optical data. The free volume data from positron results showed minimum free volume at 5 wt% of PEI after 60 s of irradiation due to cross linking through hydrogen bond formation and possible estrification among the blend components. These results correlate well the mechanical properties like tensile strength and modulus.     

Flexible dielectric ZnO-doped reduced graphene oxide bionanocomposites from solution blending for potential application in bio-related devices

Biocompatible materials with high dielectric constant and low dielectric loss have applications in bio-related electronic devices. Development of flexible materials with those properties is still a challenge. In this work, electrospun membranes and films are prepared from poly(vinyl alcohol) (PVA) and chitosan (CS) solutions, incorporated with a reduced graphene oxide-zinc oxide composite (rGO-ZnO). Blending CS with flexible PVA favors electrospinnability and mechanical properties. ZnO contributes to hinder agglomeration of conductive rGO sheets. The structural, mechanical, dielectric and electrical properties of the hybrid materials are investigated. Infrared spectroscopy reveals interaction between the filler and the polymeric components. For mats and films, the increase in rGO-ZnO content leads to lower crystallinity. The Young's modulus and stress at break values increase with increasing rGO-ZnO content. High dielectric constants (ε' = 132 to ε' = 166, at 10³ Hz), associated with low dielectric loss factor (tan δ = 0.02), are determined for the PVA/CS/rGO-ZnO films.     

Extraction of chitosan from Aspergillus niger mycelium and synthesis of hydrogels for controlled release of betahistine

Chitosan was extracted from the fungus Aspergillus niger, an alternative source of chitin that is widely available as a byproduct of the industrial production of citric acid. Chitosan with deacetylation degree (DD) of 73.6% was characterized by elemental analysis, capillary viscometry (molecular weight of 1.9 × 10⁵ g/mol), Fourier transform infrared (FTIR), nuclear magnetic resonance (¹H NMR, ¹³C NMR and ¹⁵N NMR) spectroscopies, differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Fungal chitosan was crosslinked with glutaraldehyde and glutaric acid to obtain hydrogels. Chitosan hydrogels were characterized by FTIR and by scanning electron microscopy (SEM), which showed that these materials have irregular, polydisperse, and interconnected pores. Kinetic studies of the release of betahistine from the swollen hydrogels showed a Fickian diffusion mechanism. Finally, hydrolytic degradation of chitosan hydrogels under simulated physiological conditions (pH 7.4 and 37 °C) was investigated as well as in vivo biocompatibility tests using New Zealand white rabbits as animal models.     

Preparation and hemocompatibility of electrospun O‐carboxymethyl chitosan/PVA nanofibers

Chitosan was deacetylated and carboxymethylated to prepare O‐carboxymethyl chitosan (CMC) for further electrospinning. CMC was characterized using FTIR, NMR, and chemical titration, indicating a degree of carboxymethylation of 51.4%. CMC was electrospun together with poly(vinyl alcohol) (PVA) to prepare membranes composed of nanofibers. The electrospinning conditions were optimized. The CMC/PVA membrane obtained at the conditions of 15.2 g/mL CMC 50 mL, 8 g/mL PVA 5 mL, 25 kV, and a distance of 23 cm, had nanofibers without beads, with diameters of 70–200 nm. The mats were crosslinked by glutaraldehyde before platelet adhesion measurement. The nanofibrous structure remained after crosslinking while the wettability decreased. CMC/PVA mats with higher CMC amount and fewer beads, had fewer adherent platelets and less platelets aggregation showing better hemocompatibility. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43565.     

Sorption of heavy metal ions from aqueous solution by a novel cast PVA/TiO2 nanohybrid adsorbent functionalized with amine groups

Sorption of Cd(II), Ni(II) and U(VI) ions onto a novel cast PVA/TiO₂/APTES nanohybrid adsorbent with variations in adsorbent dose, pH, contact time, initial metal concentration and temperature has been investigated. The adsorbent were characterized by SEM and FTIR analysis. BET surface area, pore diameter and pore volume of adsorbent were 35.98 m² g⁻¹, 3.08 nm and 0.059 cm³ g⁻¹, respectively. The kinetic and equilibrium data were accurately described by the double-exponential and Freundlich models for all metals. The maximum sorption capacities were 49.0, 13.1 and 36.1 mg g⁻¹ for Cd(II), Ni(II) and U(VI) ions with pH of 5.5, 5 and 4.5, respectively. Thermodynamic studies showed that the sorption process was favored at higher temperature. The adsorbent can be easily regenerated after 5 cycles of sorption–desorption.     

In situ preparation of CdS/PVA nanocomposites using gamma radiation

Films of poly(vinyl alcohol)/cadmium sulphide (PVA/CdS) nanocomposite containing various concentrations of Cd²⁺ ions were prepared using gamma radiation at different doses from 50 up to 200 kGy. The UV/VIS spectra revealed that the CdS/PVA nanocomposites showed blue shift for the absorption peak as compared with bulk CdS. As the irradiation dose increased, a gradual red shift in the wavelength accompanying with broadening of the absorption peak was observed. The estimated optical band gap energies and the calculated CdS particle sizes of (PVA/CdS) showed correlation between their values and the variable parameters (irradiation dose and Cd⁺²:S^?2 molar ratio). Transmission electron microscopy images showed that the CdS/PVA nanocomposites were dispersed as spherical CdS nanoparticles with homogeneity at either lower concentration of CdCl₂ or irradiation dose. The nano‐rod structures of CdS was accompanied with small agglomeration at either higher CdCl₂ concentration or irradiation dose. A cubic phase and mixture of cubic and hexagonal phases of the prepared CdS nanoparticles were formed at lower and higher CdCl₂ concentrations, respectively. Fourier Transform Infrared spectra confirmed the coordination of CdS nanoparticles with the hydroxyl groups of PVA matrix. POLYM. ENG. SCI., 55:2583–2590, 2015. © 2015 Society of Plastics Engineers     

Preparation and antifouling performance of thin inorganic ultrafiltration membrane via assisted sol-gel method with different composition of dual additives

A novel TiO₂ thin film was prepared on the ceramic hollow fiber by the sol-gel method using poly(vinylpyrrolidone) (PVP) and polyvinyl alcohol (PVA) as additives. SEM images verified the formation of TiO₂ layer with various thickness using different composition of titania sols. The effect of the PVP and PVA contents on the TiO₂ sol properties, the separation and the antifouling performance of the ultrafiltration membranes were investigated thoroughly. When the contents of PVP and PVA were 1.0 wt% and 0.8 wt%, respectively, the resultant membrane showed a thickness of 0.55 μm with a pure water flux of 255 L m^?2 h^?1. In addition, the adherent foulant bovine serum albumin was applied to evaluate the antifouling performance. During the three fouling-recovery cycles, the flux recovery ratio and the flux decay ratio maintained about 99% and 30%. The BSA flux and rejection were still 169 L m^?2 h^?1 and 96.9% after the cycles, indicating a superior antifouling property.     

Efficient preparation of hybrid nanocomposite coatings based on poly(vinyl alcohol) and silane coupling agent modified TiO2 nanoparticles

In the present investigation, at first, the surface of titanium dioxide (TiO₂) nanoparticles was modified with γ-aminopropyltriethoxy silane as a coupling agent. Then a new kind of poly(vinyl alcohol)/titanium dioxide (PVA/TiO₂) nanocomposites coating with different modified TiO₂ loading were prepared under ultrasonic irradiation process. Finally, these nanocomposites coating were used for fabrication of PVA/TiO₂ films via solution casting method. The resulting nanocomposites were fully characterized by Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD), thermogravimetric analysis/derivative thermal gravimetric (TGA/DTG), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and atomic force microscopy (AFM). The TEM and SEM results indicated that the surface modified nanoparticles were dispersed homogeneously in PVA matrix on nanoscale and based on obtained results a possible mechanism was proposed for ultrasonic induced nanocomposite fabrication. TGA confirmed that the heat stability of the nanocomposite was improved. UV–vis spectroscopy was employed to evaluate the absorbance and transmittance behavior of the PVA/TiO₂ nanocomposite films in the wavelength range of 200–800 nm. The results showed that this type of films could be used as a coating to shield against UV light.