Synthesis and characterization of polypyrrole using TiO2 nanotube@poly(sodium styrene sulfonate) as dopant and template

A polypyrrole (PPy) using TiO₂ nanotube@poly(sodium styrene sulfonate) (TiO₂@PSS) as dopant and template was synthesized by chemical oxidation polymerization. The template TiO₂@PSS consisting of a TiO₂ nanotube core and PSS on the surface was prepared by a “grafting from” approach. PPy on the layer of TiO₂@PSS (TiO₂@PSS/PPy) was characterized by transmission electron microscopy, scanning electron microscopy, X‐ray photoelectron spectroscopy (XPS), Fourier‐transform infrared spectrometry (FTIR), Raman spectroscopic analysis, UV‐visible (UV‐vis) spectroscopy, thermo gravimetric analysis, and electrical conductivity analysis. Results showed that TiO₂@PSS/PPy was successfully fabricated. The electrical conductivity of the TiO₂@PSS/PPy nanocomposites at room temperature was 11.6 S cm⁻¹, which was higher than that of the PPy (4.2 S cm⁻¹). This result was consistent with those based on FTIR, UV‐vis spectroscopy, and XPS analyses. The nanocomposites have nanoparticle size and controllable morphology and thus potential applications in photoelectrochemical devices, photocatalytic devices, conductive inks, electronic printing sensors, and electrodes. POLYM. COMPOS., 37:462–467, 2016. © 2014 Society of Plastics Engineers     

Study of the effect of rutile/anatase TiO2 nanoparticles synthesized by hydrothermal route in electrospun PVA/TiO2 nanocomposites

Mixed rutile–anatase TiO₂ nanoparticles were synthesized by hydrothermal treatment under acidic conditions and incorporated into poly(vinyl alcohol) (PVA). These nanocomposites were electrospun to produce nanofibers of PVA/TiO₂, which were characterized by scanning electron microscopy, transmission electron microscopy, X‐ray diffraction (XRD), UV–vis diffuse reflectance spectroscopy, thermogravimetric analysis, and differential scanning calorimetry. The photocatalytic degradation of Rhodamine B and degradation of the polymer by UV‐C lamps were also investigated. The results showed that TiO₂ nanoparticles did not change the morphology and thermal behavior of the nanofiber polymer, but were effective in modifying the UV absorption of PVA without reducing its stability. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Photoactive behavior of polyacrylonitrile fibers based on silver and zirconium co‐doped titania nanocomposites: Synthesis,characterization, and comparative study of solid‐phase photocatalytic self‐cleaning

Silver and zirconium co‐doped and mono‐doped titania nanocomposites were synthesized and deposited onto polyacrylonitrile fibers via sol–gel dip‐coating method. The resulted coated‐fibers were characterized by X‐ray diffraction (XRD), scanning electron microscopy, energy dispersive spectroscopy, transmission electron microscopy, diffuse reflectance spectroscopy, thermogravimetric analysis, and BET surface area measurement. Photocatalytic activity of the TiO₂‐coated and TiO₂‐doped coated fibers were determined by photomineralization of methylene blue and Eosin Y under UV–vis light. The progress of photodegradation of dyes was monitored by diffuse reflectance spectroscopy. The XRD results of samples indicate that the TiO₂, Ag‐TiO₂, Zr‐TiO₂, and Ag‐Zr‐TiO₂ consist of anatase phase. All samples demonstrated photo‐assisted self‐cleaning properties when exposed to UV–vis irradiation. Evaluated by decomposing dyes, photocatalytic activity of Ag–Zr co‐doped TiO₂ coated fiber was obviously higher than that of pure TiO₂ and mono‐doped TiO₂. Our results showed that the synergistic action between the silver and zirconium species in the Ag‐Zr TiO₂ nanocomposite is due to both the structural and electronic properties of the photoactive anatase phase. These results clearly indicate that modification of semiconductor photocatalyst by co‐doping process is an effective method for increasing the photocatalytic activity. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Preparation and characterization of polypyrrole/TiO2 nanocomposites by reverse microemulsion polymerization and its photocatalytic activity for the degradation of methyl orange under natural light

PPy/TiO₂ nanocomposites were successfully prepared by reverse microemulsion polymerization and used as an effective photocatalyst for the degradation of methyl orange. Titanium dioxide (TiO₂) was modified by silane coupling agent to improve the dispersity before the polymerization. X‐ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier‐transform infrared spectra were carried out to characterize the morphology and structure of the samples. TEM analysis shows that TiO₂ particles are deposited by polypyrrole (PPy) and the existence of PPy mitigates the agglomeration of TiO₂. XRD spectra reveal that the deposition of PPy does not change the structure of TiO₂ particles. Uv–vis analysis shows that the PPy/TiO₂ nanocomposites have a higher photocatalytic activity under natural light than neat TiO₂. The highest degradation rate occurs when the mass ratio of PPy to TiO₂ is kept at 0.02. POLYM. COMPOS., 34:1076–1080, 2013. © 2013 Society of Plastics Engineers     

Efficient photocatalytic degradation of methylene blue over BiVO4/TiO2 nanocomposites

BiVO₄/TiO₂ nanocomposites were successfully synthesized by coupling the modified sol-gel method with hydrothermal method. The samples were physically characterized X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Brunauer, Emmett and Teller (BET)-specific surface area, UV–vis diffuse reflectance spectrophotometry, zeta potential, and photoluminescence techniques. The BiVO₄/TiO₂ nanocomposites exhibited good photocatalytic activity in degradation of methylene blue under simulated solar light irradiation. The photodegradation of methylene blue demonstrated that 0.5BiVO₄/0.5TiO₂ photocatalyst exhibited much enhanced photoactivity than pure BiVO₄ and TiO₂. Based on the obtained results, the as-prepare BiVO₄/ TiO₂ nanocomposite possessed great adsorptivity of methylene blue, extended light adsorption range, and efficient charge separation properties. Overall, this work could provide new insights into the fabrication of a BiVO₄/TiO₂ composite as high performance photocatalyst and promise as a solar light photocatalyst for dye wastewater treatment.     

TiO2 nanofibers assembled on graphene-silver platform as a visible-light photo and bio-active nanostructure

The heterogeneous titanium oxide-reduced graphene oxide-silver (TiO₂/RGO/Ag) nanocomposites were successfully prepared by incorporation of two dimensional (2D) RGO nanosheets and spherical silver nanoparticles (NPs) into the 1D TiO₂ nanofibers. The novel TiO₂/RGO/Ag nanocomposites were synthesized by loading TiO₂ nanofibers, prepared via electrospinning technique, on the RGO/Ag platform. The resulting nanocomposites have been characterized using various techniques containing transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and ultra-violet-visible (UV–vis) spectroscopy. Microscopic studies clearly verified the existence of TiO₂ nanofibers with Ag NPs on the surface of RGO sheet and formation of TiO₂/RGO/Ag nanocomposites. Moreover, the results of UV–vis spectroscopy demonstrated that TiO₂/RGO/Ag nanocomposites extended the light absorption spectrum toward the visible region and significantly enhanced the visible-light photocatalytic performance of the prepared samples on degradation of rhodamine B (Rh. B) as a model dye. It was found that, incorporation of 50 µl RGO/Ag into the TiO₂ nanofibers lead to a maximum photocatalytic performance. Also, the improvement of the inactivation of Escherichia coli (E. coli) bacteria under visible-light irradiation was revealed by introduction of RGO/Ag into the TiO₂ matrix. The significant enhancement in the photo and bio-activity of TiO₂/RGO/Ag nanocomposites under visible-light irradiation can be ascribed to the RGO/Ag content by acting as electron traps in TiO₂ band gap.     

One-dimensional spindle-like BiVO4/TiO2 nanofibers heterojunction nanocomposites with enhanced visible light photocatalytic activity

One-dimensional spindle-like BiVO₄/TiO₂ nanofibers heterojunction nanocomposites with high visible light photocatalytic activity have been successfully obtained by combining the electrospinning technique and solvothermal method. The as-obtained products were characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), UV–vis spectra and photoluminescence (PL) spectra. The results revealed that spindle-like BiVO₄ nanostructures were successfully grown on TiO₂ nanofibers. Photocatalytic tests showed that the BiVO₄/TiO₂ nanofibers heterojunction nanocomposites showed enhanced visible light photocatalytic activity than that of pure TiO₂ nanofibers, which might be attributed to the effective photogenerated electrons-holes separation based on the photosynergistic effect of the BiVO₄/TiO₂ heterojunction. Moreover, the BiVO₄/TiO₂ nanofibers heterojunction nanocomposites could be easily recycled without any decrease of the photocatalytic activity.     

Physical properties of epoxy resin/titanium dioxide nanocomposites

A polymeric nanocomposite system (nanodielectric) was fabricated, and its mechanical properties were determined. The fabricated nanocomposite was composed of low concentrations of monodispersed titanium dioxide (TiO₂) nanoparticles and an epoxy resin specially designed for cryogenic applications. The monodispersed TiO₂ nanoparticles were synthesized in an aqueous solution of titanium chloride and polyethylene glycol and subsequently dispersed in a commercial‐grade epoxy resin (Araldite® 5808). Nanocomposite thin sheets were prepared at several weight fractions of TiO₂. The morphology of the composites, determined by transmission electron microscopy, showed that the nanoparticles aggregated to form particle clusters. The influence of thermal processing and the effect of filler dispersion on the structure–property relationships were identified by differential scanning calorimetry and dynamic mechanical analysis at a broad range of temperatures. The effect of the aggregates on the electrical insulation properties was determined by dielectric breakdown measurements. The optical properties of the nanocomposites and their potential use as filters in the ultraviolet–visible (UV–vis) range were determined by UV–vis spectroscopy. POLYM. ENG. SCI., 2011. © 2010 Society of Plastics Engineers     

Structural and thermal characterization of poly(2‐chloroaniline)/red mud nanocomposite materials

We report the synthesis and characterization of a series of conducting poly(2‐chloroaniline) (P2ClAn)/red mud (RM) nanocomposite materials. The polymerization of 2‐chloroaniline in an aqueous medium in the presence of (NH₄)₂S₂O₈ and RM resulted in the formation of a nanocomposite (P2ClAn/RM). The extent of P2ClAn loading in the composites increased with increasing oxidant and monomer concentrations but decreased with RM. The properties of the nanocomposites were characterized with Fourier transform infrared (FTIR), ultraviolet–visible (UV–vis), conductivity measurements, scanning electron microscopy, thermogravimetric analysis, and differential scanning calorimetry analysis. The inclusion of P2ClAn in the composites was confirmed by FTIR studies. The UV–vis spectra of P2ClAn/RM nanocomposites were similar to that of P2ClAn. The conductivity changed in all the composites prepared under various conditions. Thermogravimetric analyses revealed the enhanced thermal stabilities of the nanocomposites with respect to P2ClAn. Morphological images of the as‐synthesized materials were also investigated with scanning electron microscopy and environmental scanning electron microscopy. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci, 2006     

In situ fabrication of polyaniline‐silver nanocomposites using soft template of sodium alginate

Polyaniline (PANI)‐Ag nanocomposites were synthesized by in situ chemical polymerization approach using ammonium persulfate and silver nitrate as oxidant. Characterizations of nanocomposites were done by ultraviolet–visible ( UV–vis), Fourier transform infrared (FTIR), X‐ray diffraction (XRD), scanning electron microscopy, and transmission electron microscopy (TEM). UV–vis, XRD and FTIR analysis established the formation of PANI/Ag nanocomposites and face‐centered‐cubic phase of silver. PANInanofibers were of average diameter ～ 30 nm and several micrometers in length. Morphological analysis showed that the spherical‐shaped silver nanoparticles decorate the surface of PANI nanofibers. Silver nanoparticles of average diameter ～ 5–10 nm were observed on the TEM images for the PANI‐Ag nanocomposites. Such type of PANI‐Ag nanocomposites can be used as bistable switches as well as memory devices. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Preparation,thermostability, and hydrophobic properties of TiO2/poly(dodecafluoroheptyl methacrylate) nanocomposites

Poly(dodecafluoroheptyl methacrylate) (PDFMA)/titanium dioxide (TiO₂) nanocomposites with high TiO₂ content were successfully prepared by emulsion polymerization process. Before polymerization, nano‐TiO₂ was pretreated by silane coupling agent. Surface groups and composition of the modified nano‐TiO₂ were characterized by Fourier transform infrared and X‐ray photoelectron spectra. The microstructure of nanocomposites was observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). In addition, the thermo‐stability and wetting behavior were also investigated in relation to the dosage of TiO₂. The results showed that the thermostability is improved with the increment of TiO₂ content while hydrophilic properties exhibit nonlinear variation with the content of TiO₂. The optimal percentage of TiO₂ content in the TiO₂/PDFMA nanocomposites is 30% that could lead to the higher thermostability and hydrophobicity properties of composites. The maximum water contact angle (WCA) of nanocomposites can reach 120° ± 1°. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44377.     

UV-curable polyurethane acrylate–Ag/TiO2 nanocomposites with superior UV light antibacterial activity

Polyurethane acrylate (PUA)–Ag/TiO₂ nanocomposites were synthesized through in situ polymerization. The well-dispersed Ag/TiO₂ nanorods serve as photoinitiator. Meanwhile, the PUA–Ag/TiO₂ nanocomposite films exhibit superior activity toward the photocatalytic degradation of Escherichia coli under UV light. The excellent UV curing and antibacterial activities can be ascribed to the synergistic effect of Ag and TiO₂, which promotes the effective electron/hole separation and thus generates various reactive species. Thin films with these nanoparticles are more hydrophilic after UV illumination. And the antibacterial mechanism of the UV-curable PUA–Ag/TiO₂ nanocomposites was proposed.     

Synthesis and characterizations of magnetite nanocomposite films for radiation shielding

Polyvinyl alcohol (PVA) films containing magnetite Fe₃O₄ nanoparticles have been prepared by co‐precipitation method for use in gamma ray shielding and protection. Characterizations of the magnetite/PVA nanocomposite films were investigated by X‐ray diffraction (XRD), transmission electron microscopy (TEM), UV–vis spectroscopy, and magnetization measurements. TEM images showed that the synthesized magnetite particles had about 6–11 nm dimensions. Optical study's results revealed that the optical energy band gaps of thin films range between 1.82 and 2.81 eV at room temperature using UV–visible absorption spectroscopy. The saturation magnetization (MS) value measured by vibrating sample magnetometer VSM was found to be 8.1 emu/g with superparamagnetic nature. The radiation shielding properties such as linear attenuation coefficients (μ ) and half‐value thickness (HVT) for the magnetite nanocomposite films have been obtained experimentally for different photon energies. The results imply that these nanocomposites films are promising radiation shielding materials. POLYM. COMPOS., 38:974–980, 2017. © 2015 Society of Plastics Engineers     

Conducting polyaniline‐titanium dioxide nanocomposites prepared by inverted emulsion polymerization

Conducting polyaniline (PAni)‐titanium dioxide (TiO₂) nanocomposites have been synthesized by the inverted emulsion polymerization method. Aqueous mixtures of aniline, a free‐radical oxidant, and/or TiO₂ nanoparticles (∼25 nm in diameter; mixture of anatase and rutile) are utilized to synthesize the hybrid nanocomposites. The polymerization is carried out in an organic solvent (chloroform, CHCl₃) in the presence of a protonic acid (hydrochloric acid, HCl) as a dopant and an emulsifier (cetyl trimethylammonium bromide). The resultant PAni‐TiO₂ nanocomposites are characterized with their structural, morphological, conducting, and optical properties. SEM and TEM images represent the PAni‐TiO₂ nanocomposites with the diameter range of 50–200 nm. Electrical conductivities are checked by standard four‐point probes method and found to be 0.38 S/cm for bulk PAni and 0.11 S/cm for PAni‐TiO₂ nanocomposites. UV–visible absorption shows two electronic bands at about 320 and 596 nm for bulk PAni and the blue‐shifted bands with the intensity changes due to the formation of PAni‐TiO₂ composites. Thermogravimetric analysis reveals that the composites have a higher degradation temperature than the PAni alone. POLYM. COMPOS., 2010. © 2009 Society of Plastics Engineers     

Synthesis,spectral analysis,and catalytic activity of poly(aniline‐co‐congored)–metal oxide nanocomposites

Electrically conducting, water‐soluble fluorescent copolymer nanocomposites were synthesized by a solution polymerization method under different experimental conditions in the presence of CuO and V₂O₅ nanoparticles. The prepared copolymer nanocomposites were characterized with analytical tools, including Fourier transform infrared spectroscopy, ultraviolet–visible (UV–vis) spectroscopy, and fluorescence emission spectroscopy. The order of copolymerization was determined on the basis of the UV–vis absorption spectra and fluorescence emission spectra. The copolymer–CuO nanocomposite system exhibited the highest electrical conductivity. The scanning electron microscopy image showed the presence of more CuO nanoparticles on the surface of the copolymer. Furthermore, the catalytic activity of the copolymer nanocomposites was tested for the reduction of p‐nitrophenol. All three types of polymer systems exhibited almost the same apparent rate constant values. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46469.     

Production and characterization of nanocomposites based on poly(amide-imide) containing 4,4′-methylenebis(3-chloro-2,6-diethylaniline) using nano-TiO2 surface-coupled by 3-aminopropyltriethoxysilane

In this work, the poly(amide-imide) (PAI) was synthesized from the polymerization reaction of 4,4′-methylenebis(3-chloro-2,6-diethyl trimellitimidobenzene) as a diacid with 4,4′-methylenebis(3-chloro-2,6-diethylaniline) under green condition using molten tetra-n-butylammonium bromide and triphenylphosphite. Ultrasonic technique was used for preparation of PAI/TiO₂ nanocomposites (PAI/TiO₂ NCs). For the improvement of TiO₂ nanoparticles (NPs) dispersion and enhancing interactions between NPs and polymeric matrix the surface of TiO₂ was successfully modified by silane coupling agent (3-aminopropyltriethoxysilane). The resulting NCs were characterized by FT-IR, X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA). The TGA of the obtained NCs proves the enhancement in the thermal stability with an increase in the percentage of titania NPs. TEM and FE-SEM images showed that the NPs were uniformly dispersed in the polymer matrix. The shielding effect of nano TiO₂ under UV radiation was examined by UV–vis.     

Mg Doped Copper Ferrite with Polyaniline Matrix Core–Shell Ternary Nanocomposite for Electromagnetic Interference Shielding

Electromagnetic interference shielding materials based on polyaniline/Mg_0.6Cu_0.4Fe₂O₄ ternary nanocomposites were prepared using in situ chemical oxidation polymerization method. The crystalline, structural and morphology analyses of the synthesized material were studied by X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR) and high resolution transmission electron microscopy (HR-TEM). The nanocomposites were examined by UV–Vis spectroscopy (UV–Vis), four probe resistivity, vibrating sample magnetometer (VSM), thermal gravimetric analysis (TGA) and vector network analyzer (VNA) for the optical, electrical, thermal, magnetic and shielding properties. XRD, FTIR and UV–Vis spectra analyses confirmed the formation of ferrites and polyaniline phases in the composites. The particle sizes of Mg_0.6Cu_0.4Fe₂O₄ are lying in the range of 15–40 nm verified by the HR-TEM. VSM study proved the presence of magnetic nanoparticles in the polyaniline matrix. TGA results revealed that the mixing of ferrites particles in polyaniline has improved its thermal stability. The nanocomposites are showing the significant shielding effectiveness value up to 32.8 dB in the X-band frequency range which makes them potential shielding material for electromagnetic interference shielding applications due to lightweight, good processability and low cost.     

In situ polymerized nanocomposites of poly(butylene succinate)/Tio2 nanofibers: molecular weight,morphology, and thermal properties

In this study, the nanocomposites of poly(butylene succinate) (PBS) and TiO₂ nanofibers were first synthesized via in situ polymerization. Molecular weight, morphology, and thermal properties of the nanocomposites were characterized. As the weight percentage of TiO₂ nanofibers increased from 0 to 2%, the molecular weight of PBS in the nanocomposites decreased gradually compared with that of pure PBS. In morphology, the nanocomposites were constituted by free PBS and PBS‐grafted TiO₂ nanofibers (PBS‐g‐TiO₂), which were proved by the Fourier transform infrared, scanning electron microscopy (SEM), and transmission electron microscopy. In addition, the SEM demonstrated the strong interfacial interaction and homogeneous distribution between TiO₂ nanofibers and PBS matrix. The thermal properties determined by differential scanning calorimetry and thermogravimetric analysis included the increasing of cold crystallization temperatures, the melting temperatures, and the thermal stability. Besides, the crystallinity and the rate of crystallization of the nanocomposites were enhanced, which were also observed by the X‐ray diffraction. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Palygorskite–TiO2 nanocomposites: Part 1. Synthesis and characterization

In this paper we describe the synthesis and characterization of small-sized TiO₂ particles supported on palygorskite (Pal) with Pal to TiO₂ mass ratios of 10:90, 20:80, 30:70, 40:60 and 50:50. The above Pal–TiO₂ nanocomposites were prepared by deposition of anatase form of TiO₂ on the Pal surfaces using a sol-gel method with titanium isopropoxide as a precursor under hydrothermal treatment at 180 °C. Phase composition, particle morphology and physical properties of these samples were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), attenuated total reflection using Fourier transform infrared spectroscopy (ATR-FTIR) and N₂ surface area analysis by BET. In order to investigate the absorption properties of the catalysts, UV–vis reflection spectra were measured. Preparation of Pal–TiO₂ nanocomposites led to good dispersion of TiO₂ on Pal surfaces. By increasing the amount of TiO₂, the deposited 3–10 nm TiO₂ particles were found to be aggregated on the surfaces of the Pal particles. However, by decreasing the amount of TiO₂, the Pal particles were found to be aggregated. After treating with TiO₂, Pal samples largely showed interparticle mesopores of about 5.8 nm. It was observed that the commercial titania P25 showed no absorption in visible light region. In contrast, the prepared Pal–TiO₂ samples showed gray color and absorption in visible light region.     

Preparation and property of raspberry‐like AS/SiO2 nanocomposite particles

Surfactant‐free poly(acrylonitrile‐co‐styrene)/silica (AS/SiO₂) nanocomposite particles was synthesized in the presence of cheap, commercially amorphous aqueous silica sol at ambient temperature. Thermogravimetric analysis (TGA) indicated silica contents ranging from 5 wt % to 29 wt %, depending on reaction conditions. Particle size distributions and morphologies were studied using dynamic light scattering (DLS) and transmission electron microscopy (TEM), which clearly showed that most of the colloidal nanocomposites comprised approximately spherical particle with raspberry‐like morphology and relatively narrow size distributions. The optical clarity of solution‐cast nanocomposite films was assessed using UV–vis spectrometer, with high transmission being obtained over the whole visible spectrum. Differential scanning calorimetry (DSC) studies showed that the glass transition temperature of AS/SiO₂ nanocomposites can be higher than the corresponding pure AS, resulting from the hydrophilicity of the nanometer silica. The robustness and simplicity of this method may make large‐scale manufacture of this nanocomposite possible. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 415–421, 2007