Preparation and properties of transparent and conducting nylon 6-based composite films

Highly transparent and conducting polypyrrole–(PPy–N) and polyaniline–nylon 6 (PAN) composite films could be easily obtained by immersing nylon 6 films containing pyrrole or aniline into an oxidant solution such as aqueous FeCl₃ solution or aqueous (NH₄)₂S₂O₈ solution containing HCl. The conductivity, transmittance, and mechanical properties of these composite films were affected by the preparative conditions. The maximum conductivity and transmittance of the PPy–N composite films were 10^?3 S/cm and about 75% at 550 nm, and in the case of the PA–N composite films, 10^?2 S/cm and 75%, respectively. The morphology of PPy–N and PA–N composite films depended on the polymerization conditions, which might be due to the difference in the polymerization speed of pyrrole or aniline in polymer matrices. These PPy–N and PA–N composite films exhibited good environmental stability and excellent mechanical properties. © 1994 John Wiley & Sons, Inc.     

Microwave irradiation graft copolymerization of hydroxyethyl methacrylate onto wool fabrics

Hydroxyethyl methacrylate was grafted onto woolen fabrics by microwave irradiation in the presence of catalyst (NH₄)₂S₂O₈. Various parameters of the graft copolymerization reaction, namely, time, microwave intensity, catalyst, and monomer concentration, were optimized. The graft copolymerization was also compared with conventional heating graft copolymerization at the same condition. Microwave irradiation was shown to improve the reactivity of the monomer. The moisture regain decreased as graft add-on increased. The Max load and the strain at Max load increased as graft add-on increased. The infrared spectra showed an additional peak at 1700 cm⁻¹, confirming ester carbonyl groups of the monomer. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 70: 2343–2347, 1998     

High Performance Organic Coatings of Polypyrrole Embedded with Manganese Iron Oxide Nanoparticles for Corrosion Protection of Conductive Copper Surface

Herein, we report the formation of organic composite coating consists of epoxy (EP) reinforced para toluene sulphonic acid (PTSA) doped polypyrrole (PPy)–manganese iron oxide (MnFe₂O₂) as an efficient corrosion inhibitor for copper substrates. The PTSA doped PPy:MnFe₂O₂ nanocomposite was synthesized via in situ polymerization of PPy in the presence of MnFe₂O₂ nanoparticles. Structural features of the prepared samples were characterized through scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), UV–visible spectroscopy and thermogravimetric analysis (TGA). The PTSA doped PPy:MnFe₂O₂ nanocomposite shows excellent conductivity and improved dielectric performance in comparison to pure PPy. The anti-corrosion performance of this organic composite coating was analyzed through Tafel polarization curves, open circuit potential (OCP), corrosion resistance, impedance spectroscopy and oxygen permeability barrier tests. The nanocomposite coating on copper substrate shows superior corrosion protection efficiency (99%) in comparison to pure epoxy (22%). Adhesion strength of the nanocomposite coating shows significant enhancement due to strong dispersions of MnFe₂O₂ nanoparticles in the host matrix. Owing to its improved conductivity, excellent anti-corrosion performance along with superior mechanical properties, the organic nanocomposite coating reported in this work can potentially be used to protect the conductive copper surfaces from harsh corrosive environments.

     

Influence of sintering aids and excess Lithium on the conductivity of perovskite-type Li3/8Sr7/16Zr1/4Nb3/4O3 solid electrolyte

Perovskite-structured Li_3/8Sr_7/16Zr_1/4Nb_3/4O₃ solid-state Lithium-conductors were prepared by conventional solid-state reaction method. Influence of sintering aids (Al₂O₃, B₂O₃) and excess Lithium on structure and electrical properties of Li_3/8Sr_7/16Zr_1/4Nb_3/4O₃ (LSNZ) has been investigated. Their crystal structure and microstructure were characterized by X-ray diffraction analysis and scanning electron microscope, respectively. The conductivity and electronic conductivity were evaluated by AC-impedance spectra and potentiostatic polarization experiment. All sintered compounds are cubic perovskite structure. Optimal amount of excess Li₂CO₃ was chosen as 20 wt% because of the total conductivity of LSNZ-20% was as high as 1.6×10⁻⁵ S cm⁻¹ at 30 °C and 1.1×10⁻⁴ S cm⁻¹ at 100 °C, respectively. Electronic conductivity of LSNZ-20% is 2.93×10⁻⁸ S cm⁻¹, nearly 3 orders of magnitude lower than ionic conductivity. The density of solid electrolytes appears to be increased by the addition of sintering aids. The addition of B₂O₃ leads to a considerable increase of the total conductivity and the enhancement of conductivity is attributed to the decrease of grain-boundary resistance. Among these compounds, LSNZ-1 wt%B₂O₃ has lower activation energy of 0.34 eV and the highest conductivity of 1.98×10⁻⁵ S cm⁻¹ at 30 °C.     

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     

Liquid crystal epoxy composites based on functionalized boron nitride: Synthesis and thermal properties

A composite was prepared by in-situ polymerization of liquid crystal epoxy (LCE₄) with a low dielectric and high thermal conductivity boron nitride (BN) filler, which the filler (f-BN) was surface-functionalized by γ-glycidoxypropyltrimethoxysilane (KH560) and aminopropylisobutyl polyhedral oligomeric silsesquioxane (NH₂-POSS). The surface-functionalized BN was more uniformly dispersed in LCE₄, which improved the interfacial compatibility between inorganic and organic phases. Compared with pure LCE₄, KH560, and NH₂-POSS modified f-BN/LCE₄ composites exhibited a higher glass transition temperature, better thermal stability, and higher thermal conductivity. For example, when the f-BN content reached 30 wt%, the energy storage modulus of the composite increased to 2580 MPa, and the glass transition temperature was 103°C. The thermal conductivity of this 30 wt% f-BN composite was 0.48 W m⁻¹ K⁻¹, 128.6% higher than that of pure LCE₄. In addition, thermal stability, low hygroscopicity, and dielectric properties of the composites were characterized and analyzed to explore the application prospects of f-BN/LCE₄ composites in electronic packaging and in high-performance microelectronic devices.     

Electrical conductivity and nonstoichiometry in doped Sr3Ti2O7

A series of doped Ruddlesden–Popper phases, of general formula Sr₃Ti_2-xM_xO_7-δ (M=Al, Ga, Co), were synthesized and their electrical conductivity characterized as a function of temperature and oxygen partial pressure. For fixed-valent dopants, p-type conductivity predominates at p(O₂)> 10⁻⁵ atm, followed by a p(O₂)-independent electrolytic regime, and n-type electronic conductivity at very low p(O₂). The electrolytic regime exhibits activation energies in the range 1·7–1·8 eV. Doping with transition metals such as Co results in a very significant increase in total conductivity with a p-type conductivity at high p(O₂). Furthermore, an apparent ionic regime at intermediate p(O₂) is observed, characterized by high conductivity (> 10⁻² S/cm at 700°C) and low activation energy (0·6 eV). This interpretation is consistent with iodometric measurements as interpreted by a defect chemical model. Other measurements are in progress to confirm this conclusion.     

Electrically conductive composites of polyurethane derived from castor oil with polypyrrole‐coated peach palm fibers

Electrically conducting fibers were prepared through in situ oxidative polymerization of pyrrole (Py) in the presence of peach palm fibers (PPF) using iron (III) chloride hexahydrate (FeCl₃·6H₂O) as oxidant. The polypyrrole (PPy) coated PPF displayed a PPy layer on the fibers surface, which was responsible for an electrical conductivity of (2.2 ± 0.3) × 10⁻¹ S cm⁻¹, similar to the neat PPy. Electrically conductive composites were prepared by dispersing various amounts of PPy‐coated PPF in a polyurethane matrix derived from castor oil. The polyurethane/PPy‐coated PPF composites (PU/PPF–PPy) exhibited an electrical conductivity higher than PU/PPy blends with similar filler content. This behavior is attributed to the higher aspect ratio of PPF–PPy when compared with PPy particles, inducing a denser conductive network formation in the PU matrix. Electromagnetic interference shielding effectiveness (EMI SE) value in the X‐band (8.2–12.4 GHz) found for PU/PPF–PPy composites containing 25 wt% of PPF–PPy were in the range −12 dB, which corresponds to 93.2% of attenuation, indicating that these composites are promising candidates for EMI shielding applications. POLYM. COMPOS., 38:2146–2155, 2017. © 2015 Society of Plastics Engineers     

Effects of polymerization medium on electrical conductivity and optical properties of organic semiconductor-based polypyrrole

The effects of tetrabutylammonium tetrafluoroborate (TBAFB), tetrabutylammonium hexafluorophosphate (TBAPF₆), and paratoluene sulfonoicacid (PTSA) polymerization mediums on the electrical conductivity and optical properties of the polypyrrole (PPy) have been investigated. The electrical conductivity and optical properties of the samples polymerized in presence of TBAFB, TBAPF₆, and PTSA organic salts change with medium of prepared polymer. The electrical conductivity of the TBAFB, PTSA, and TBAPF₆ samples at 27°C were found to be 3.43 × 10⁻¹, 4.48 × 10⁻², and 1.60 × 10⁻⁴ (S/cm), respectively. The lowest optical band gap of the polymer was found to be 2.23 eV. The refractive index dispersion of the samples obeys single oscillator model. The obtained results suggest that polymerization medium changes electrical conductivity and optical properties of the PPy. POLYM. ENG. SCI., 47:1016–1020, 2007. © 2007 Society of Plastics Engineers     

Process induced alignment of carbon nanotube decreases longitudinal thermal conductivity of Al2O3 based porous composites

Alumina (Al₂O₃) based porous composites, reinforced with zirconia (ZrO₂), 3 and 8 mol% Y₂O₃ stabilized ZrO₂ (YSZ) and 4 wt% carbon nanotube (CNT) are processed via spark plasma sintering. The normalized linear shrinkage during sintering process of Al₂O₃-based composite shows minimum value (19.2–20.4%) for CNT reinforced composites at the temperature between 1650 °C and 575 °C. Further, the combined effect of porosity, phase-content and its crystallite size in sintered Al₂O₃-based porous composite have elicited lowest thermal conductivity of 1.2 Wm⁻¹K⁻¹ (Al₂O₃-8YSZ composite) at 900 °C. Despite high thermal conductivity of CNT (∼3000 Wm⁻¹K⁻¹), only a marginal thermal conductivity increase (∼1.4 times) to 7.3–13.4 Wm⁻¹K⁻¹ was observed for CNT reinforced composite along the longitudinal direction at 25 °C. The conventional models overestimated the thermal conductivity of CNT reinforced composites by up to ∼6.7 times, which include the crystallite size, porosity, and interfacial thermal resistance of Al₂O₃, YSZ and, CNT. But, incorporation of a new process induced CNT-alignment factor, the estimated thermal conductivity (of <6.6 Wm⁻¹K⁻¹) closely matched with the experimental values. Moreover, the high thermal conductivity (<76.1 Wm⁻¹K⁻¹) of the CNT reinforced porous composites along transverse direction confirms the process induced alignment of CNT in the spark plasma sintered composites.     

Synthesis and improved mechanical properties of twin-mesogenic epoxy thermosets using siloxane spacers with different lengths

A series of twin-mesogenic epoxy resins with siloxane (di-, tri-, and tetra-siloxane) chain spacers of different lengths were successfully synthesized. Results showed that the melting point of the twin-mesogenic epoxy monomers decrease by more than 50 °C due to the change of siloxane spacer length. In particular, the tri- and tetra-incorporated siloxane twin-mesogenic epoxy monomers showed a liquid crystalline (LC) phase below 100 °C during the cooling process. Epoxy thermosets with isotropic and smectic (S_m) LC phases were then prepared using an aromatic amine and the dependence on curing temperature was investigated. Furthermore, the relationship between the ordered network chain structure and mechanical properties was investigated. Results were compared with isotropic and S_m LC phases. The tensile strain and fracture energy in the S_m type LC thermosets increased without a decrease in the tensile modulus, and this occurred in all systems irrespective of siloxane spacer length. The maximum value of the fracture energy (283 kJ m⁻²) reached by LC thermosets with increased spacer lengths was twice as large as that using the alkyl chain spacer (144 kJ m⁻²). © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47891.     

Effect of ethanol on chemically synthesized polyaniline nanothread

The nanothread of polyaniline (PANI) using ammonium persulphate ((NH₄)₂S₂O₈) as an oxidant was prepared. The solution is composed of 0.4 mol dm^?3 aniline, 1.0 mol dm^?3 hydrochloric acid, and different proportions ethanol. The resulting products were characterized using infrared spectroscopy, UV–vis spectra, transmission electron microscope, thermogravimetric analysis techniques, and X‐ray diffraction. The experimental results show that the content of ethanol has effects on the morphology of PANI, but the effects on the conductivity are not very obvious. When the volume ratio of ethanol to aniline is 1:2, the more uniform and regular PANI nanothread can be prepared. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 1848–1853, 2006     

Oxide ionic conductivity of apatite type Nd9·33(SiO4)6O2 single crystal

Single crystal of hexagonal apatite type Nd_9·33(SiO₄)₆O₂ which is an oxide ionic conductor was prepared by the FZ method and an anisotropy of its conductivity was investigated. The conductivity of a parallel component to a c-axis (2·1×10⁻⁸ S cm⁻¹ at 30°C) was higher about one order of magnitude, compared with that of perpendicular component.     

The accelerated degradation of aqueous polyacrylamide at low temperature

The accelerated degradation of aqueous polyacrylamide at low temperature was studied. The selected degradation agents included several peroxides, such as potassium persulfate (K₂S₂O₈), ammonium persulfate ((NH₄)₂S₂O₈), hydrogen peroxide (H₂O₂), and the potassium persulfate–sodium thiosulfate (K₂S₂O₈–Na₂S₂O₃) redox system. The redox system showed the highest degradation rate at the first 2 hours, but its final degradation level was lower than that of potassium persulfate. The degradation temperature, concentration of potassium persulfate and polyacrylamide, and original molecular weight of polyacrylamide all affected the degradation rate and final degradation level. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 69: 791–797, 1998     

Mixed conductivity of garnet phases based on gadolinium ferrite

Incorporation of Pr and Ca into the garnet lattice of Gd₃Fe₅O_12±δ was found to increase the electronic conductivity, and to decrease the thermal expansion coefficients and oxygen ion transference numbers. The ionic conductivity of Gd_2.2Pr_0.8Fe₅O_12±δ ceramics is similar to that of undoped gadolinium ferrite, whilst Gd_2.5Ca_0.5Fe₅O_12-δ exhibits slightly higher ionic transport, suggesting an enhanced vacancy contribution. The activation energies for ionic conduction in Gd₃Fe₅O₁₂-based materials vary in the narrow range 211–224 kJ/mol. Due to a significantly lower activation energy for the total conductivity (24–81 kJ/mol), the oxygen ion transference numbers in air increase with temperature, from 4 × 10⁻⁵ – 5×10⁻³. Steady-state oxygen permeation fluxes through dense garnet membranes are limited by bulk ambipolar conductivity. The thermal expansion coefficients of the ferrite ceramics (100–1000 °C) were found linear and in the range 10.36–10.86 × 10⁻⁶ K⁻¹.     

Improvement of microwave absorption for PAni/HA/TiO2/Fe3O4 nanocomposite after chemical treatment

In order to obtain efficient microwave absorbers that possess high conductivity, dielectric and magnetic properties, hexanoic acid doped polyaniline (PAni) nanocomposites which contain different ratios of ferum (II) oxide (Fe₃O₄) and titanium dioxide (TiO₂) nanoparticles were successfully prepared by in situ chemical polymerization through template free method. Chemical structure, conductivity, morphology, thermal stability, magnetic properties, and amorphous/crystalline behavior of PAni nanocomposites were characterized by Fourier transform infrared spectrometer (FTIR), four point probe, field emission scanning electron microscope (FESEM), thermal gravimetric analysis (TGA), vibrating samples magnetometer (VSM), and X‐ray diffractometer (XRD), respectively. From this study, conductivity was significantly improved from 8.48 × 10⁻⁴−1.23 × 10⁻² S/cm for PAni nanocomposites without any chemical treatment (during addition of Fe₃O₄) to 3.58 × 10⁻²−4.77 × 10⁻² S/cm for those with chemical treatment. PAni nanocomposites with chemical treatment show a narrow sharp reflection loss (RL) peak with high absorption (−48.9 dB) at lower frequency due to the limited individual Fe₃O₄ nanoparticles outside the nanorods/nanotubes as proved by the new proposed mechanism (Fig. 5 ), while it shows a broad RL peak with poor absorption (−13 dB) at higher frequency for those without chemical treatment. The novelty of this research has been focused on PAni with chemical treatment which yield better microwave absorption property (99.999% absorption), combination of high conductivity (3.58 × 10⁻²−4.77 × 10⁻² S/cm), high heterogeneity and moderate magnetization (Ms = 8.87–28.49 emu/g) compare to the PAni without chemical treatment. POLYM. COMPOS., 34:1186–1194, 2013. © 2013 Society of Plastics Engineers     

The influence of ammonium and methods for removal during the anaerobic treatment of poultry manure

The addition of exogenous NH₄Cl to poultry manure and synthetic medium was used to study the effect of ammonia-nitrogen on the activity and composition of a methanogenic consortium. Results indicated that the production of biogas and methane was not affected by the variation in NH₄Cl concentration within the range 2–10 g dm⁻³ (0·5–2·6 g N-NH₄ dm⁻³). At higher values of ammonium (10–30 g dm⁻³ or 2–8 g N-NH₄ dm⁻³) a significant decline in both parameters (by 50–60% for biogas and 80–90% for methane) was observed. A significant decrease in the numbers of bacteria of all physiological groups (especially proteolytic and methanogenic) was observed when more than 30 g NH₄Cl dm⁻³ (7·8 g N-NH₄ dm⁻³) was added to the fermentation medium. The addition of 10% (w/v) of powdered phosphorite ore enhanced the production of biogas and methane at NH₄Cl concentrations up to 30 g dm⁻³, and also changed the composition of the methanogenic consortium. A partial recovery in the numbers of proteolytic and methanogenic bacteria coupled with the decrease in the density of sulphate-reducers was observed. High concentrations (more than 50 g dm⁻³) of NH₄Cl seemed to cause irreversible inhibition of methanogenesis which could not be eliminated by the addition of phosphorites. ©1997 SCI     

Preparation and characterization of conductive and magnetic PPy/Fe3O4/Ag nanocomposites

In this article, conductive and magnetic nanocomposites composed of polypyrrole (PPy), magnetite (Fe₃O₄) nanoparticles (NPs), silver (Ag) NPs, have been successfully synthesized with a two step process. First, the PPy/Fe₃O₄ was prepared by the ultrasonic in situ polymerization. Next, the PPy/Fe₃O₄/Ag was synthesized through the electrostatic adsorption. The products were characterized by fourier‐transform infrared (FTIR) spectroscopy, Scanning electron microscopy (SEM), Thermogravimetric (TG), conductivity and magnetization analysis, and the results showed that the Ag NPs with the good conductivity coated uniformly on the surface of PPy/Fe₃O₄ and improved the conductivity of PPy/Fe₃O₄/Ag composites. In addition, as compared with PPy/Fe₃O₄, PPy/Fe₃O₄/Ag composites also have the excellent electro‐magnetic property and enhanced thermostability. POLYM. COMPOS., 35:450–455, 2014. © 2013 Society of Plastics Engineers     

Physico‐chemical and dielectric characterization of polypyrrole clay composite

In this study, we report on the chemical and dielectric properties of polypyrrole (PPy) clay composite. The in situ polymerization has been carried out in an aqueous solution using ammonium persulfate (APS) as oxidant. Molar ratio of Pyrrole (Py) to interlayer clay cation was fixed to 4 and that of APS to Py (R ) was varied in the range of 0.25–4.00. It was shown that both the chemical and dielectric behaviors were affected by the variation of (R ). XRD results showed an intercalated structure of PPy for a value of R corresponding to 0.25. Above this value, the basal distance (d ₀₀₁) was found to be around 1.3 nm, implying that PPy is essentially located at the surface of Montmorillonite (MMT). From FTIR spectroscopy, it was found that for R = 4, PPy was degraded, resulting in a decrease of the degree of polymerization and conductivity. For all samples the AC conductivity was found to be constant until 2 × 10⁵ Hz but increased steeply above this value. The highest conductivity was found to be around 3.95 10⁻³ S.cm⁻¹ for R = 1. The composite exhibited very large values of ε′ and ε ″ at a low frequency, these values decreased with the increase of frequency. Curves of imaginary electric modulus (M ″) exhibited a frequency peak due to the process of relaxation time of conductivity (τ = 6.9410⁻⁸ s) for R = 1. POLYM. COMPOS., 38:2043–2051, 2017. © 2015 Society of Plastics Engineers     

Spark plasma sintering of (5RE.2)Ta3O9 high-entropy ceramics and their thermal properties

Six rare-earth tantalate high-entropy ceramics of (5RE_.2)Ta₃O₉ (RE represents any five elements selected from La, Ce, Nd, Sm, Eu, Gd) were designed and prepared by spark plasma sintering process at 1400°C in this study. The (5RE_.2)Ta₃O₉ ceramics only consist of a single-phase solid solution with perovskite structure. Their relative densities are all above 90%, and the average grain size is in the range of 1.47–2.92 μm. The thermal conductivity of (5RE_.2)Ta₃O₉ ceramics is in 2.24–1.90 W m⁻¹ K⁻¹ (25°C–500°C), which is much lower than that of yttria-stabilized zirconia. In six samples, (La_.2Nd_.2Sm_.2Gd_.2Eu_.2)Ta₃O₉ possesses a thermal conductivity of 1.90 W m⁻¹ K⁻¹, a thermal expansion coefficient of 3.47 × 10⁻⁶ K⁻¹ (500°C), a Vickers hardness of about 7.33 GPa, and a fracture toughness of about 5.20 MPa m^1/2, which are suitable for its application as thermal barrier coatings.