Fabrication and characterization of iron oxide nanoparticles filled polypyrrole nanocomposites

The effect of iron oxide nanoparticle addition on the physicochemical properties of the polypyrrole (PPy) was investigated. In the presence of iron oxide nanoparticles, PPy was observed in the form of discrete nanoparticles, not the usual network structure. PPy showed crystalline structure in the nanocomposites and pure PPy formed without iron oxide nanoparticles. PPy exhibited amorphous structure and nanoparticles were completely etched away in the nanocomposites formed with mechanical stirring over a 7-h reaction. The thermal stability of the PPy in the nanocomposites was enhanced under the thermo-gravimetric analysis (TGA). The electrical conductivity of the nanocomposites increased greatly upon the initial addition (20 wt%) of iron oxide nanoparticles. However, a higher nanoparticle loading (50 wt%) decreased the conductivity as a result of the dominance of the insulating iron oxide nanoparticles. Standard four-probe measurements indicated a three-dimensional variable-range-hopping conductivity mechanism. The magnetic properties of the fabricated nanocomposites were dependent on the particle loading. Ultrasonic stirring was observed to have a favorable effect on the protection of iron oxide nanoparticles from dissolution in acid. A tight polymer structure surrounds the magnetic nanoparticles, as compared to a complete loss of the magnetic iron oxide nanoparticles during conventional mechanical stirring for the micron-sized iron oxide particles filled PPy composite fabrication.     

Synthesis, characterization and infrared emissivity study of polyurethane/TiO2 nanocomposites

In this study, polyurethane/titania (PU/TiO₂) nanocomposites were prepared in ultrasonic process and characterized by fourier transform IR spectroscopy (FT-IR), powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and infrared emissivity analysis. The TEM and SEM results indicated that the nanoparticles were dispersed homogeneously in PU matrix on nanoscale. TGA-DSC confirmed that the heat stability of the composite was improved. Infrared emissivity study showed that the nanocomposite possessed lower emissivity value than those values of pure polymer and nanoparticles.     

Influence of lithium potassium zirconate nanoparticles on the electrical properties and structural characteristics of poly(vinyl alcohol) films

We investigated the influence of lithium potassium zirconate (LiKZrO₃) nanoparticles on the electrical properties and structural characteristics of poly(vinyl alcohol) (PVA) films. PVA/LiKZrO₃ nanocomposite films were prepared by casting of aqueous solutions with varying LiKZrO₃ content (0.5, 1.0, and 2.0 wt.%). The dielectric constant (ε′), dielectric loss (ε″), AC conductivity (σ_ac), dielectric loss tangent (tan δ), and electric modulus (M′ and M″) of the nanocomposite films were measured over a range of frequencies at ambient temperature. The results show increases in σ_ac and M′ with frequency, whereas ε′, ε″, and tan δ decreased with increasing frequency. The films were also characterized using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and X-ray diffraction (XRD) techniques. DSC and XRD revealed the nature of LiKZrO₃ nanoparticle interaction with the PVA matrix. TGA analysis revealed an increase in thermal stability of the nanocomposites with increasing nanoparticle concentration. Scanning electron microscopy confirmed uniform dispersion of LiKZrO₃ nanoparticles in the PVA matrix.     

The Effect of Zinc Oxide and Calcium Carbonate Nanoparticles on the Thermal Conductivity of Polypropylene

The thermal conductivity (TC) of compression-moulded polypropylene (PP) and PP filled with 5–15% zinc oxide (ZnO) or calcium carbonate (CaCO₃) nanoparticles, prepared by extrusion, was studied using a thermal conductivity analyzer (TCA). The effect of nanoparticle content and crystallinity on the thermal conductivity was investigated using conventional methods, including SEM, XRD, and DSC. The incorporation of nanoparticles improved the crystallinity and thermal conductivity simultaneously. The experimental TC values of the PP nanocomposites with different level of nanoparticles concentration showed a linear increase with an increase in crystallinity. The TC improvement in PP/ZnO nanocomposite was greater than that of PP/calcium carbonate nanocomposites. This fact can be attributed to the intrinsic, better thermal conductivity of the ZnO nanoparticles. Several models were used for prediction of the TC in the nanocomposites. In the PP/ZnO nanocomposites the TC values correlated well with the values predicted by the Series, Maxwell, Lewis and Nielson, Bruggeman, and De Loor models up to 10 wt%.     

Enhanced dielectric properties and energy storage density of interface controlled ferroelectric BCZT-epoxy nanocomposites

Polymer nanocomposites with ferroelectric fillers are promising materials for modern power electronics that include energy storage devices. Ferroelectric filler, Ba_0.85Ca_0.15Zr_0.1Ti_0.9O₃ (BCZT) nanopowder, was synthesized by sol-gel method. X-ray diffraction (XRD) studies confirmed the phase purity and the particle size distribution was determined by transmission electron microscopy (TEM). Extended aromatic ligand in the form of naphthyl phosphate (NPh) was chosen for surface passivation of BCZT nanoparticles. Surface functionalization was validated by thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), and impedance spectroscopy using slurry technique. The dielectric constant of surface-passivated BCZT nanopowder was ~155, whereas pristine BCZT nanopowder dielectric constant could not be assessed due to high innate surface conductivity. Furthermore, BCZT–epoxy nanocomposite films were prepared and analyzed by differential scanning calorimetry (DSC), dielectric spectroscopy, dielectric breakdown strength (DBS), and scanning electron microscopy (SEM). Owning to stronger polymer–particle interface, dielectric measurements of 5 vol.% NPh surface functionalized BCZT–epoxy nanocomposites indicated improved DBS and glass transition temperature (T_g), reduced dielectric loss, and enhanced energy storage density compared to untreated BCZT–epoxy composites and pure epoxy. The energy storage density of 30 vol.% NPh surface functionalized BCZT–epoxy nanocomposite of 20 μm film thickness was almost three times that of pure epoxy polymer of identical film thickness.     

Effect of ZnO filler concentration on the conductivity, structure and morphology of PVdF-HFP nanocomposite solid polymer electrolyte for lithium battery application

The polyvinylidene difluoride-co-hexafluoropropylene (PVdF-HFP) nanocomposite solid polymer electrolyte films were developed by solution-casting method. PVdF-HFP as a polymer host, lithium perchlorate (LiClO₄) as a salt for lithium ion, and ZnO nanoparticles as fillers were used to form the nanocomposite solid polymer electrolyte films. All the prepared samples were characterized by X-ray diffraction (XRD), differential scanning calorimetry, and scanning electron microscopy. The XRD patterns of the pure and nanocomposite solid polymer electrolyte samples indicate the formation of amorphous phase with 17.5 wt.% of lithium salt and ZnO fillers up to 3 wt.%. The total conductivity and lithium ion transference number were studied at room temperature by using impedance spectroscopy and Wagner’s polarization methods. The highest conductivity at room temperature for solid polymer electrolyte and nanocomposite solid polymer electrolyte are found to be 3.208?×?10^?4 and 1.043?×?10^?3 S/cm, respectively. Similarly, the lithium ion transference number is evaluated for the optimized solid polymer electrolyte and nanocomposite solid polymer electrolyte films with 3 wt.% of ZnO fillers. And it is found that ionic transference number could be enhanced from 92 to 95 % with the addition of nanosized ZnO fillers to the solid polymer electrolyte.     

Synthesis and characterization of poly(1-vinyl-1,2,4-triazole) (PVTri)-barium hexaferrite nanocomposite

We present a method for the fabrication of PVTri-BaFe₁₂O₁₉ nanocomposites by in-situ polymerization of PVTri in the presence of synthesized BaFe₁₂O₁₉ nanoparticles. Nanoparticles, polymer and nanocomposite were analyzed by XRD, FTIR, TGA, TEM, NMR, GPC and conductivity techniques for structural and physicochemical characteristics. Crystallographic analysis revealed the phase as hexaferrite and X-ray line profile fitting yielded a crystallite size of 17±5 nm. Conjugation of PVTri to nanoparticle surface was assessed to be via carbonyl groups on the polymer. TG analysis revealed that 45 wt% of nanocomposite is inorganic phase (BaFe₁₂O₁₉). It was found out that the ac conductivity of nanocomposite under a certain frequency increases with temperature.     

Preparation and characterization of polyindole–ZnO composite polymer electrolyte with LiClO<Subscript>4</Subscript>

This paper describes the preparation and conductivity studies of polyindole–ZnO composite polymer electrolyte (CPE) with LiClO₄. Polyindole–ZnO-based polymer nanocomposites were prepared by chemical method and characterized by XRD, infrared (IR), scanning electron microscope (SEM), transmission electron microscopy (TEM), and thermogravimetric analysis (TGA). The IR spectrum confirms the intermolecular interaction between polyindole and ZnO. The significant spectral changes of polyindole and ZnO nancomposites reveal the strong interaction between polyindole and ZnO nanoparticles. The structural morphologies of the ZnO, polyindole, and polyindole–ZnO are obtained from SEM. The TEM image of polyindole nanocomposite shows that ZnO is embedded in polyindole matrix. An enhanced conductivity of 4.405 × 10⁻⁷ S cm⁻¹ at 50 °C for the CPE was determined from impedance studies.     

In Situ Synthesis and Characterization of Polypyrrole/Graphene Conductive Nanocomposites via Electrochemical Polymerization and Chemical Reduction

Polypyrrole/graphene sheets (PPy/GNs) nanocomposite electrodes were in- situ synthesized via electrochemical polymerization and chemical reduction from pyrrole (Py) and graphene oxide (GO). The surface morphologies of the nanocomposites were observed by scanning electron microscopy (SEM). The SEM results showed graphene sheets (GNs) scattered on the surface of the polypyrrole (PPy), and the morphologies of PPy/GNs nanocomposites manufactured by pulse current (PC-PPy/GNs) or direct current (DC-PPy/GNs) were smoother than that of PC-PPy. The electrochemical capacitance properties of the nanocomposite films were measured by cyclic voltammetry (CV), galvanostatic charge and discharge (GC), and electrochemical impedance spectroscopy (EIS) techniques in 3 mol·L^?1 KCl aqueous solutions. The results indicated that the specific capacitance of the DC-PPy/GNs nanocomposite was 13.5% higher than that of a PC-PPy electrode. Comparison of the electrochemical performance of the nanocomposites indicated that the PC-PPy/GNs nanocomposite had higher specific capacitance and better charging/discharging capability than that of the DC-PPy/GNs nanocomposite. The specific capacitance of the PC-PPy/GNs nanocomposite could reach to 280 F·g^?1 at a scanning rate of 100 mV·s^?1.     

Influence of embedded particles on microstructure, corrosion resistance and thermal conductivity of CuO/SiO2 and NiO/SiO2 nanocomposite coatings

Homogeneous CuO/SiO₂ and NiO/SiO₂ nanocomposite coatings containing CuO and NiO nanoparticles in silica matrix were successfully synthesized by sol–gel process on an aluminum alloy substrate, respectively. The evolution of phase and morphology of both nanocomposites was characterized by XRD, SEM, TEM and FTIR. The effect of incorporating various nanoparticles on the corrosion behavior and the thermal conductivity of nanocomposite coatings was investigated by potentiodynamic polarization curve and comparative exponential method. The thermal conductivity as well as the corrosion resistance of nanocomposite coatings was significantly improved by the introduction of metal oxide particles. In comparison with NiO/SiO₂ nanocomposite coatings, CuO/SiO₂ composite coatings displayed lower protective behavior as well as higher thermal conductivity. Experimental results revealed that those improvements can directly be related to the nanocomposite effect and the nature of added nanoparticles.     

Preparation and properties of nano-sized Ag and Ag2S particles in biopolymer matrix

Silver (Ag) and silver sulfide (Ag₂S) nanoparticles were synthesized in a sago starch matrix. The resulting nanocomposites were investigated using structural, optical and thermal methods. XRD spectra of the nanocomposites confirmed the presence of nanostructured silver (cubic phase) and silver sulfide (monoclinic phase) in the matrix. TEM micrographs showed that the nanoparticles are mostly spherical in shape. Analyzes of the optical properties of the silver nanocomposite aqueous dispersions/solutions of various concentrations were carried out. The results and the theoretical considerations suggested that at high concentrations there is a release of silver nanoparticles from the composite in the water environment. Further dilution produces homogeneous solution in which silver nanoparticles are capped with starch macromolecules. TGA analysis revealed reduced thermal stability of the nanocomposites with respect to pure starch matrix.     

Induced Electronic and Thermal Effects of 86 MeV Nickel Ions in Bisphenol-A Polycarbonate

Bisphenol-A polycarbonate films were irradiated with 86 MeV swift heavy nickel ions at varying fluences, ranging from 1 × 10¹¹ to 1 × 10¹³ ions cm^?2, under vacuum at room temperature, to analyze the induced electrical and thermal modifications. AC conductivity measurements and UV-visible spectroscopy, Fourier transform infra-red (FTIR) spectroscopy, thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) techniques were applied to analyze the changes. A significant, exponential increase in conductivity at higher frequency was observed with the increase of nickel ion fluence. UV-visible analysis corroborated the results of the AC conductivity measurement, revealing the increase in size of the carbon clusters embedded in the polymer network, with the increase of heavy ion fluence. FTIR analysis revealed the formation of alkene and alkyne end groups at higher doses, which further supported the suggestion that the variation in electrical properties induced by the ion irradiation of the polymer was due to development of a carbonaceous phase inside the polymer due to the irradiation. Thermal analysis, i.e., TGA and DSC patterns, showed that chain-scission was the leading phenomena in the heavy ion-irradiated polycarbonate samples, resulting in degradation of their thermal stability.     

Preparation and Characterization of Poly(Vinyl Alcohol) (PVA)/SiO2, PVA/Sulfosuccinic Acid (SSA) and PVA/SiO2/SSA Membranes: A Comparative Study

Abstract

New organic–inorganic nanocomposites based on PVA, SiO₂ and SSA were prepared in a single step using a solution casting method, with the aim to improve the thermomechanical properties and ionic conductivity of PVA membranes. The structure, morphology, and properties of these membranes were characterized by Raman spectroscopy, small- and wide-angle X-ray scattering (SAXS/WAXS), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), water uptake (Wu) measurements and ionic conductivity measurements. The SAXS/WAXS analysis showed that the silica deposited in the form of small nanoparticles (～ 10?nm) in the PVA composites and it also revealed an appreciable crystallinity of pristine PVA membrane and PVA/SiO₂ membranes (decreasing with increasing silica loading), and an amorphous structure of PVA/SSA and PVA/SSA/SiO₂ membranes with high SSA loadings. The thermal and mechanical stability of the nanocomposite membranes increased with the increasing silica loading, and silica also decreased the water uptake of membranes. As expected, the ionic conductivity increased with increasing content of the SSA crosslinker, which is a donor of the hydrophilic sulfonic groups. Some of the PVA/SSA/SiO₂ membranes had a good balance between stability in aqueous environment (water uptake), thermomechanical stability and ionic conductivity and could be potential candidates for proton exchange membranes (PEM) in fuel cells.     

Synthesis and characterization of hybrid nanocomposites of polypyrrole filled with iron oxide nanoparticles

Hybrid polypyrrole (PPy)/α-Fe₂O₃ nanocomposite films were fabricated by spin coating on a glass substrate. X-Ray diffraction analysis revealed the crystalline structure of α-Fe₂O₃ nanostructures and the nanocomposites. The broad PPy peak weakened in intensity as the α-Fe₂O₃ content increased in PPy/α-Fe₂O₃ nanocomposites. Characteristic Fourier-transform IR peaks for pure PPy shifted to higher wavenumbers on addition of α-Fe₂O₃ to PPy/α-Fe₂O₃ nanocomposites. This can be attributed to better conjugation and interactions between PPy and α-Fe₂O₃ nanoparticles. Field-emission scanning electron microscopy, transmission electron microscopy, and atomic force microscopy images of the nanocomposites reveal a uniform distribution of α-Fe₂O₃ nanoparticles in the PPy matrix. UV-vis absorption spectroscopy revealed a blue shift from λ_max= 441 nm for PPy to λ_max= 392 nm for PPy/α-Fe₂O₃, reflecting strong interactions between PPy and α-Fe₂O₃ nanoparticles. The room-temperature dc electrical conductivity increased from 4.33×10⁻⁹ to 1.81×10⁻⁸ S/cm as the α-Fe₂O₃ nanoparticle content increased from 10 to 50 wt.% in PPy/α-Fe₂O₃ nanocomposites.     

Structural,thermal, and electrical studies of sodium iodide (NaI)-doped hydroxypropyl methylcellulose (HPMC) polymer electrolyte films

Solid polymer electrolyte films based on hydroxypropyl methylcellulose (HPMC) complexed with sodium iodide (NaI) were prepared using solution cast method. The dissolution of the salt into the polymer host and the structural properties of pure and complexed HPMC polymer electrolyte films were confirmed by X-ray diffraction (XRD) studies. XRD results revealed that the amorphous domains of HPMC polymer matrix were increased with increase in NaI salt concentration. The degree of crystallinity was found to be high in pure HPMC samples. The thermal properties were studied using differential scanning calorimetry (DSC). DSC results revealed that the presence of NaI in the polymer matrix increases the melting temperature; however, it is observed that fusion heat is high for pure HPMC films. The variation of film morphology was examined by scanning electron microscopy. Fourier transform infrared spectral studies revealed vibrational changes that occurred due to the effect of dopant salt in the polymer. Direct current conductivity was measured in the temperature range of 313–383 K. The magnitude of electrical conductivity was found to increase with the increase in salt and temperature concentration. The data on the activation energy regions (regions I and II) indicated the dominance of ion-type charge transport in these polymer electrolyte films. The composition HPMC:NaI (5:4) is found to exhibit the least crystallinity and the highest conductivity.     

Synthesis, structural and conductivity characterization of alginic acid–Fe3O4 nanocomposite

Alginic acid–Fe₃O₄ nanocomposite is synthesized by the precipitation of Fe₃O₄ in the presence of alginic acid (AA). Structural, surface, morphological, thermal and electrical transport properties of the nanocomposite were performed by XRD, FT-IR, TEM-SEM, TGA and conductivity measurements respectively. FT-IR analysis revealed that Fe₃O₄ NPs are strongly capped with AA and TGA analysis showed that nanocomposite have 80% of Fe₃O₄ content. TEM analysis of Fe₃O₄ NPs show an average particle size of 9.5 nm, and upon nanocomposite formation with AA these particles are observed to form aggregates of ~150 nm. The frequency-dependency of the AC conductivity show electrode polarization effect. Analysis of electrical modulus and dielectric permittivity functions suggest that ionic and polymer segmental motions are strongly coupled. DC electrical conductivity is strongly temperature dependent, and is classified into three regions over a limited temperature range of up to 100 °C.     

Preparation, characterization and surface morphology of novel optically active poly(ester-amide)/functionalized ZnO bionanocomposites via ultrasonication assisted process

Novel bionanocompoites (BNCs) were prepared using zinc oxide (ZnO) nanoparticles which functionalized by γ-methacryloxypropyltrimethoxysilane (KH570) as a coupling agent. Poly(ester-amide) (PEA) based on tyrosine natural amino acid was synthesized and used as a polymer matrix. PEA/ZnO BNCs were characterized by fourier transform infrared spectra (FT-IR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). All the results confirmed that the surface of ZnO particle has sufficient compatibility with PEA through the link of the coupling agent between ZnO and polymer and also proved that the presence of ZnO nanoparticles appeared to be dispersed in nanosize in polymer composite matrix. In addition, thermogravimetric analysis (TGA) data indicated an enhancement of thermal stability of new BNC materials compared with the pure polymer.     

Dielectric relaxation and ac conductivity behavior of carboxyl functionalized multiwalled carbon nanotubes/poly (vinyl alcohol) composites

We study the dielectric relaxation and ac conductivity behavior of MWCNT-COOH/Polyvinyl alcohol nanocomposite films in the temperature (T) range 303–423 K and in the frequency (f) range 0.1 Hz–1 MHz. The dielectric constant increases with an increase in temperature and also with an increase in MWCNT-COOH loading into the polymer matrix, as a result of interfacial polarization. The permittivity data were found to fit well with the modified Cole-Cole equation. Temperature dependent values of the relaxation times, free charge carrier conductivity and space charge carrier conductivity were extracted from the equation. An observed increment in the ac conductivity for the nanocomposites was analysed by a Jonscher power law which suggests that the correlated barrier hopping is the dominant charge transport mechanism for the nanocomposite films. The electric modulus study revealed deviations from ideal Debye-type behavior which are explained by considering a generalized susceptibility function. XRD and DSC results show an increase in the degree of crystallinity.     

Ag-ZnO纳米复合热电材料的制备及其性能研究

ZnO是一类具有潜力的热电材料, 但其较大声子热导率影响了热电性能的进一步提高. 纳米复合是降低热导率的有效途径. 本文以醋酸盐为前驱体, 溶胶-凝胶法制备了Ag-ZnO纳米复合热电材料. 扫描电镜照片显示ZnO颗粒呈现多孔结构, Ag纳米颗粒分布于ZnO的晶粒之间. Ag-ZnO纳米复合材料的电导率比未复合ZnO材料高出100倍以上, 而热导率是未复合ZnO材料的1/2. 同时, 随着Ag添加量的增加, 赛贝克系数的绝对值逐渐减小. 综合以上原因, 添加7.5%mol Ag的Ag-ZnO纳米复合材料在700 K时的热电优值达到0.062, 是未复合ZnO材料的约25倍. 在ZnO基体中添加导电金属颗粒有利于产生导电逾渗通道, 提高材料体系的电导率, 但同时导致赛贝克系数的绝对值减小. 总热导率的差异来源于声子热导率的差异. 位于ZnO晶界的纳米Ag颗粒, 有利于降低声子热导率. 关键词： 热电材料 ZnO 纳米复合 热导率     

Polypyrrole–montmorillonite nanocomposites synthesized by emulsion polymerization

The structural, electrical, magnetic, and thermal properties were investigated for the nanocomposites of polypyrrole (PPy) and inorganic clay (Na⁺-montmorillonite) prepared by emulsion polymerization. Dodecylbenzenesulfonic acid (DBSA) was used as emulsifier (surfactant) and dopant. The X-ray diffraction (XRD) patterns and transmission electron microscopy (TEM) images showed that the conducting PPy was intercalated into the clay layers in nanoscale (<10 Å). The dc conductivity (σ_dc) of PPy–DBSA with clay was 6 S/cm, while that of PPy–DBSA without clay was 20 S/cm at room temperature (RT). Temperature dependence of σ_dc of both samples followed the three dimensional variable range hopping (VRH) model. From the g-value and the temperature dependence of EPR linewidth, paramagnetic signals were strongly affected by the partially negatively charged clay layers. The thermogravimetric analysis (TGA) and differential scanning calorimeter (DSC) showed that the clay induced the thermal stability of the systems.