Biopolymer-based nanocomposites: effect of lignin acetylation in cellulose triacetate films

We have prepared all-biopolymer nanocomposite films using lignin as a filler and cellulose triacetate (CTA) as a polymer matrix, and characterized them by several analytical methods. Three types of lignin were tested: organosolv, hydrolytic and kraft, with or without acetylation. They were used in the form of nanoparticles incorporated at 1 wt% in CTA. Self-supported films were prepared by vapor-induced phase separation at controlled temperature (35–55 °C) and relative humidity (10–70%). The efficiency of acetylation of each type of lignin was studied and discussed, as well as its effects on film structure, homogeneity and mechanical properties. The obtained results are explained in terms of intermolecular filler-matrix interaction at the nanometer scale, for which the highest mechanical resistance was reached using hydrolytic lignin in the nanocomposite.     

Tailoring of optical and electrical properties of PMMA by incorporation of Ag nanoparticles

Silver–poly(methyl methacrylate) (Ag–PMMA) nanocomposite films were prepared via ex situ chemical route by employing sodium borohydride (\(\hbox {NaBH}_{4}\)) as a reducing agent. In this study, PVP-stabilized Ag nanoparticles were prepared and mixed with PMMA solution. Optical and structural characterizations of resulting nanocomposite films were performed using UV–visible spectroscopy, transmission electron microscopy (TEM) and scanning electron microscopy (SEM). Characteristic surface plasmon resonance (SPR) peak of Ag nanoparticles was observed at about 3.04 eV (408 nm) in absorption spectra of Ag–PMMA nanocomposite films. TEM micrograph revealed that the spherical Ag nanoparticles with an average diameter of 5.4\(\,\pm \,\)2.5 nm are embedded in PMMA. In Raman spectra, besides shifting of vibrational bands, enhancement in intensity of Raman signal with incorporation of Ag nanoparticles was observed. Current (I)–voltage (V) measurements revealed that conductivity of PMMA increased with increasing concentration of Ag nanoparticles. Analysis of I–V data further disclosed that at voltage <2 V, ohmic conduction mechanism is the dominant mechanism, while at voltage >2 V Poole–Frenkel is the dominant conduction mechanism. Urbach’s energy, the measure of disorder, increased from 0.40 eV for PMMA to 1.11 eV for Ag–PMMA nanocomposite films containing 0.039 wt% of Ag nanoparticles.     

ZnO nanoparticles induced effects on nanomechanical behavior and cell viability of chitosan films

The aim of this paper is to develop novel chitosan–zinc oxide nanocomposite films for biomedical applications. The films were fabricated with 1, 5, 10 and 15% w/w of zinc oxide (ZnO) nanoparticles (NPs) incorporated with chitosan (CS) using a simple method. The prepared nanocomposite films were characterized using atomic force microscopy, Raman and X-ray diffraction studies. In addition, nano and micro mechanical properties were measured. It was found that the microhardness, nanohardness and its corresponding elastic modulus increased with the increase of ZnO NP percentage in the CS films. However, the ductility of films decreased as the percentage of ZnO NPs increased. Cell attachment and cytotoxicity of the prepared films at days two and five were evaluated in vitro using osteoblasts (OBs). It was observed that OB viability decreased in films with higher than 5% ZnO NPs. This result suggests that although ZnO NPs can improve the mechanical properties of pure CS films, only a low percentage of ZnO NPs can be applied for biomedical and bioengineering applications because of the cytotoxicity effects of these particles.     

Impedance study of PVA/PEG/LiClO<Subscript>4</Subscript>/TiO<Subscript>2</Subscript> nanocomposite solid polymer blend electrolyte

Composite solid polymeric electrolytes (CSPE) of PVA/PEG/LiClO₄ and nanocomposite solid polymeric electrolytes (NSPE) of PVA/PEG/LiClO₄/TiO₂ films were prepared via solution casting technique using water as the solvent. TiO₂ nano powder was prepared from the sulfate process and characterized by the XRD and SEM techniques. The structural interactions of the prepared films were studied by FTIR. Ionic conductivity of the prepared CSPE and NSPE films were measured using AC impedance method at a wide temperature range from 298.15 to 348.15 K in frequency range 50–100 MHz. The measured ionic conductivity results from Nyquist plot were compared with calculations results from equivalent circuit model. The temperature dependence of ionic conductivity of the prepared CSPE and NSPE films was expressed by Arrhenius model and the ionic conductivity activation energy was reported to be 0.86 and 0.89 eV respectively.     

Evaporation-induced self-assembly of organic–inorganic ordered nanocomposite thin films that mimic nacre

The present study attempts to incorporate acrylate-based polymers into ordered lamellar organic–inorganic nanocomposite thin films composed of alternating Poly(TPGDA)/ITO layers. The films were prepared by dip-coating from a homogeneous solution containing the soluble inorganic metal salts (InCl₃·4H2O and SnCl₂·2H₂O), surfactant, cross-linkers, organic monomers, and initiators, thus leading to composite lamellar nanocomposite materials through evaporation-induced self-assembly method. The final polymer/ITO nanocomposite thin film was obtained by a separate free-radical polymerization step, initiated by UV exposure. Structures and composition of the films were characterized using FTIR, XRD, UV–Vis spectrophotometer and TEM. The results indicated that the films were composed of organic and inorganic layers with orderly interlaced arrangement.     

Preparation and thermomechanical properties of Ag-PVA nanocomposite films

Metal–polymer hybrid nanocomposites have been prepared from an aqueous solution of polyvinyl alcohol (PVA) and silver nitrate (AgNO₃). The silver nanoparticles were generated in PVA matrix by the reduction of silver ions with PVA molecule at 60–70 °C over magnetic stirrer. UV–vis analysis, X-ray diffraction studies, transmission electron microscopy, scanning electron microscopy and current–voltage analysis were used to characterize the nanocomposite films prepared. The X-ray diffraction analysis reveals that silver metal is present in face centered cubic (fcc) crystal structure. Average crystallite size of silver nanocrystal is 19 nm, which increases to 22 nm on annealing the film at 150 °C in air. This result is in good agreement with the result obtained from TEM. The UV–vis spectrum shows a single peak at 433 nm, arising from the surface plasmon absorption of silver nanocolloids. This result clearly indicates that silver nanoparticles are embedded in PVA. An improvement of mechanical properties (storage modulus) was also noticed due to a modification of PVA up to 0.5 wt% of silver content. The current–voltage (I–V) characteristic of nanocomposite films shows increase in current drawn with increasing Ag-content in the films.     

Fabrication and characterization of nanostructured (Sn–Ti)O<Subscript>2</Subscript> pellets and films for liquefied petroleum gas sensing

Present paper reports the synthesis of nanostructured (Sn–Ti)O₂ via physicochemical method, its characterization and performance as liquefied petroleum gas (LPG) sensor. The synthesized material was characterized using XRD that confirmed the formation of (Sn–Ti)O₂ nanocomposite. Minimum crystallite size was found as 7 nm. The material was also investigated through SEM, DSC, FTIR, PL and UV–Vis spectrophotometer. Further, the pellet, thick and thin films were fabricated for the sensing analysis. Pellets (9 mm diameter, 4 mm thickness) of (Sn–Ti)O₂ nanocomposite were made by hydraulic pressing machine by applying uniaxial pressure of 616 MPa, thick films (thickness ~2 µm) were made by screen printing technique and thin films were prepared using a Photo resist spinner unit. Further at room temperature, the pellet and films were exposed to LPG in a gas chamber under controlled conditions at room temperature and variations in resistance with the concentrations of LPG were observed. The maximum value of sensitivity of solid state pellet, thick and thin films based sensors were found 7, 9 and 39 for 5 vol% of LPG, respectively. Sensing characteristics were found to be reproducible, after 6 months of their fabrication, indicating the stability of the sensors.     

Enhancement of the optical and mechanical properties of chitosan using Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles

In this work, the optical and mechanical properties of Fe₂O₃ nanoparticles (NPs)/chitosan nanocomposite films have been investigated. Nanocomposite films of different weight ratios of Fe₂O₃ NPs/chitosan (0, 1, 5, 10, 20 and 30 wt%) were fabricated using casting technique. The optical properties of colloidal Fe₂O₃ NPs and Fe₂O₃ NPs/chitosan nanocomposite films were recorded using UV–visible spectrophotometer. As the ratio of Fe₂O₃ NPs to chitosan increases from 0 to 30%, the energy band gap of Fe₂O₃ NPs/chitosan films decreases from 3.16 to 2.11 eV. This decrease is due to quantum confinement effect. The mechanical properties of the nanocomposite films as a function of sweeping temperature were measured using a dynamic mechanical analyzer. An enhancement in storage modulus, stiffness and glass transition temperature (T_g) has been observed as the ratio of Fe₂O₃ NPs/chitosan increases. T_g of Fe₂O₃ NPs/chitosan nanocomposite film shifts towards higher temperature side with respect to pure chitosan film from 152.1 to 166.3?°C as the ratio of Fe₂O₃ NPs/chitosan increases from 0 to 30 wt%. The increase in T_g is mainly attributed to the decrease in free volumes and vacancies in the nanocomposite films as the weight ratio of Fe₂O₃ NPs/chitosan increases.     

Microstructure and mechanical properties of reactively sputtered Ti–Si–N nanocomposite films

A series of Ti–Si–N nanocomposite films with different Si content were deposited by reactive sputtering in a gas mixed with Ar, N₂ and SiH₄. Energy dispersive spectroscope, X-ray diffraction, transmission electron microscope and nanoindentation technique were employed to characterize the microstructure and mechanical properties of the films. The results reveal that Ti–Si–N nanocomposite films with different Si content can be easily obtained by controlling SiH₄ partial pressure in the mixed gas. With Si content ranging from 4 at.% to 9 at.%, the films are strengthened and reach the highest hardness and elastic modulus of 34.2 GPa and 398 GPa, respectively. With a further increase of Si content, the mechanical properties of films decrease gradually. The microstructure of Ti–Si–N films with high hardness shows the existence of TiN nanocrystals surrounded by Si₃N₄ interphase. The grain size of TiN is about 20 nm and the thickness of Si₃N₄ interphase is less than 1 nm.     

Influence of reduced graphene oxide on mechanical behaviors of sodium carboxymethyl cellulose

Sodium carboxymethyl cellulose/reduced graphene oxide (NaCMC/rGO) nanocomposite films were prepared by a simple solution mixing-evaporation method. The NaCMC/rGO nanocomposite films were characterized and compared with sodium carboxymethyl cellulose/graphene oxide (NaCMC/GO) nanocomposite films. The stability of the rGO dispersion, and the structural and mechanical properties of the composite films were investigated by UV–Vis spectrophotometry, X-ray diffraction (XRD), scanning electron microscopy (SEM), Raman spectroscopy, and using a universal testing machine (UTM). The results revealed that CMC and rGO were able to form a homogenous mixture. Compared with pure CMC, the tensile strength and Young's modulus of the CMC/rGO nanocomposite films were considerably enhanced (by 72.52% and 131.79%, respectively) upon incorporation of 2 wt% rGO.     

Controlled growth and investigations on the morphology and mechanical properties of hydroxyapatite/titania nanocomposite thin films

In this paper, the focus is on understanding the properties of nanocomposite hydroxyapatite (HAp)/titania (TiO₂) thin films with respect to TiO₂ concentration. HAp/TiO₂ nanostructured composite thin films with different TiO₂ concentrations were successfully fabricated by a simple sol–gel dip coating method. Highly stable HAp and TiO₂ sols were prepared prior to the formation of nanocomposite thin films. The coatings were performed under controlled dipping and heat treatment processes. Phase pure HAp and TiO₂ were well developed in the nanocomposite after the heat treatment and this was confirmed by XRD. The SEM and AFM analyses of HAp/TiO₂ nanocomposite coatings show the variation in the morphology as a consequence different TiO₂ concentration. This shows a reduction in the particle size to nanoscale due to the addition of TiO₂. The mechanical strength of the coating also increased upon the addition of TiO₂ as determined by nanoindentation. The composite thin films with 50 and 80 vol.% of TiO₂ show good mechanical strength when compared to other concentrations of TiO₂.     

液晶显示屏用三醋酸纤维素的合成及性能

采用高温酯化、低温水解方法,制备了用于液晶显示屏的三醋酸纤维素(CTA)。采用IR、化学滴定等手段对产物的结构进行了表征,并对膜的透光率以及力学性能等进行了测试。结果表明,自制的CTA结合醋酸含量达到60%以上,透光率高达95%以上,双折射值极低,力学性能良好,基本符合液晶显示屏起偏振片保护膜的使用要求。     

The Improvement in Mechanical and Barrier Properties of Poly(Vinyl Alcohol)/Graphene Oxide Packaging Films

In this study, poly(vinyl alcohol) (PVA)‐graphite oxide and PVA‐graphene oxide (XGO) films were prepared by simple and environmentally friendly method. Fourier transform infrared spectroscopy, X‐ray diffraction and scanning electron microscope revealed the strong hydrogen‐bonding interactions between XGO and PVA matrix and the layered structure of tensile fracture surfaces of exfoliated PVA‐XGO films. These resulted in a remarkable improvement on mechanical and barrier properties of XGO/PVA nanocomposite films. The addition of 0.3 and 2.0 wt.% XGO showed an increase in tensile strength (49%) and failure stain (13–22%), in comparison with the neat PVA films. The dramatic improvement of 144% in elastic modulus was observed in PVA/2.0 wt.% XGO. Both O₂ and water vapour permeability coefficients of PVA film decreased by about 76% and 21% at an XGO loading of 2.0 wt.%, respectively. Preliminary test was performed to determine the use of nanocomposite films to extend the shelf life of bananas. It was found that bananas packaged in nanocomposite films were ripened slower than those unpackaged or packaged in PVA films. These results demonstrate that such films could dramatically promote the application of PVA‐based films in the packaging industry. Copyright © 2015 John Wiley & Sons, Ltd.     

Synergistic enhancement of dielectric constant of novel core/shell BaTiO3@MWCNTs/PEN nanocomposites with high thermal stability

In this work, the multi-walled carbon nanotubes (MWCNTs) cores were coated with inorganic BaTiO₃ (denoted as BaTiO₃@MWCNTs) via solvent-thermal method. Then, BaTiO₃@MWCNTs/polyarylene ether nitriles (PEN) nanocomposite films embedded with core/shell BaTiO₃@MWCNTs nanotubes were successfully prepared by solution-casting method. Pure PEN film, MWCNTs/PEN and BaTiO₃/PEN films were prepared for comparison. The micromorphology, thermal, and dielectric properties of the nanocomposite films were investigated. All the nanocomposite films exhibited excellent thermal stability endowed by PEN matrix. Interestingly, it was found that core/shell BaTiO₃@MWCNTs exhibited synergistic enhancement of dielectric constant of BaTiO₃@MWCNTs/PEN nanocomposite films.     

Mechanical Properties of Gelatin Film

Abstract

The mechanical properties of gelatin films were investigated. We prepared gelatin films under various conditions, such as changing temperature, storage time and humidity. The stress-strain curves were obtained by measuring the tensile-strength of sample films at various humidities. These results suggest that mechanical properties of gelatin films depend on the structure and water content of the sample. It was found that the structure of gelatin films was influenced by the drying process and the thermal history of the gelatin.     

Highly transparent o-PDA functionalized ZnS-polymer nanocomposite thin films with high refractive index

We prepared highly transparent nanocomposite films with high refractive index using fluorescent nanocrystal quantum dots (NQDs). The as synthesized transparent solution of ZnS NQDs was blended with poly(vinylpyrrolidone) (PVP) to prepare nanocomposite thin films. Morphological data, studied by atomic force microscopy (AFM) and X-ray diffraction (XRD), revealed that NQDs were impregnated with polymer matrix and the size distributions (3.0 ± 0.30 nm) of them were preserved in the composite films. The nanocomposite films show high optical transparency (T > 95% at 400 nm and T > 98.5% at 750 nm) and the refractive index is satisfactorily increased (1.565 at 550 nm, 15 wt.% ZnS) compared to the base polymer (1.480 at 550 nm). The nanocomposite films show defectless fluorescence emissions as observed from NQDs before impregnation.     

Polymer/organosilica nanocomposites based on polyimide with benzimidazole linkages and reactive organoclay containing isoleucine amino acid: Synthesis,characterization and morphology properties

Polyimide–silica nanocomposites are attractive hybrid architectures that possess excellent mechanical, thermal and chemical properties. But, the dispersion of inorganic domains in the polymer matrix and the compatibility between the organic and inorganic phases are critical factors in these hybrid systems. In this investigation, a reactive organoclay was prepared via ion exchange reaction between protonated form of difunctional l-isoleucine amino acid as a swelling agent and Cloisite Na⁺ montmorillonite. Amine functional groups of this swelling agent formed an ionic bond with the negatively charged silicates, whereas the remaining acid functional groups were available for further interaction with polymer chains. Then organo-soluble polyimide (PI) have been successfully synthesized from the reaction of 2-(3,5-diaminophenyl)-benzimidazole and pyromellitic dianhydride in N,N-dimethylacetamide. Finally, PI/organoclay nanocomposite films enclosing 1%, 3%, 5%, 7% and 10% of synthesized organoclay were successfully prepared by an in situ polymerization reaction through thermal imidization. The synthesized hybrid materials were subsequently characterized by Fourier transform infrared spectroscopy, X-ray diffraction, electron microscopy, and thermogravimetric analysis techniques. The PI/organoclay nanocomposite films have good optical transparencies and the mechanical properties were substantially improved by the incorporation of the reactive organoclay.     

Polyaniline–CuO hybrid nanocomposites: synthesis, structural, morphological, optical and electrical transport studies

Thin films of semiconducting polyaniline (PANi) nanofibers reinforced with copper oxide (CuO) nanoparticles (NPs) were prepared on glass substrate using spin coating technique. Polyaniline (PANi) have been synthesized by chemical oxidative polymerization method with monomer aniline in presence of (NH₄)₂S₂O₈ as an oxidant at 0 °C. The copper oxide (CuO) nanoparticles were synthesized by sol–gel method. Physical properties of nanocomposite (NCs) films were characterized and analyzed by X-ray diffraction, Scanning electron microscopy, Fourier transform infrared (FTIR) spectroscopy, UV–vis spectroscopy, Two probe resistivity measurement technique and Thermo-emf measurement. Structural analysis showed that the crystal structure of CuO is not disturbed in the PANi–CuO hybrid nanocomposite. Surface morphology study shows the uniform distribution of CuO nanoparticles in PANi matrix. FTIR and UV–Visible studies confirm the presence of polyaniline in emeraldine base form in the composites and suggest incorporation of CuO in polymer. Two probe electrical resistivity measurements of nanocomposites (NCs) film revealed that the resistivity of PANi increases with increasing content of CuO NPs.     

Preparation and characterization of self-assembled organic–inorganic nacre-like nanocomposite thin films

The SiO₂/Poly(DMCB) nanocomposite thin films were prepared by supermolerculer self-assembly method on glass substrate. In the nanocomposite thin films, the surfactant DMCB was used as both structure-directing agents and poly monomers. The structures of the films were characterized using FT-IR, XRD and TEM. The results indicated that the films were composed of organic and inorganic layers with orderly interlaced arrangement and the distance between organic layer and inorganic layer was 3.48 nm before polymerization and 2.84 nm after polymerization, respectively.     

Influence of Tartaric Acid on the Bioadhesion and Mechanical Properties of Hot-Melt Extruded Hydroxypropyl Cellulose Films for the Human Nail

ABSTRACT

The objective of this study was to investigate the influence of tartaric acid (TTA) on the bioadhesive, moisture sorption, and mechanical properties of hot–melt-extruded (HME) hydroxypropyl cellulose (HPC) films containing polymer additives. Two Klucel® EF and LF batches (HPC, MW: 80000 and 95000, respectively) containing the model antifungal drug ketoconazole (one batch of each MW with and without TTA 4%) were prepared into films by HME using a Killion extruder (Model KLB-100). The bioadhesive properties of the HPC films, with and without TTA, were investigated ex vivo on the human nails. The parameters measured were work of adhesion and peak adhesion force (PAF). A statistically significant increase in both the area under the curve (AUC) and PAF was seen for the HME films containing TTA than those without TTA. Moisture content of hot-melt extruded HPC films was determined using thermogravimetric analysis (TGA). TGA data collected at the two-week interval (25°C/60% RH), measured higher moisture content for the TTA-containing films than those without TTA. Tensile strength and percent elongation were determined utilizing a TA.XT2i Texture Analyzer® equipped with a 50-kg load cell, TA-96 grips, and Texture Expert? software. TTA functioned as an effective plasticizer, increasing percent elongation and decreasing tensile strength of the HPC films. TTA could potentially be a candidate for transnail applications in film devices prepared by hot-melt extrusion technology.