An approach towards the growth of polyaniline nanograins by electrochemical route

The growth of electropolymerized polyaniline nanograins has been carried out from aqueous solution of 0.45 M aniline (C₆H₅NH₂) + 0.5 M H₂SO₄. These polyaniline nanograins were characterized using Raman spectroscopy, field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), contact angle measurement and optical studies. The presence of characteristic bonds of polyaniline was observed from Raman shift experiment. Based on field emission scanning electron microscopy and transmission electron microscopy analysis, the formation of the polyaniline nanograins with average diameter of about 50 nm was inferred. Surface of the polyaniline film was hydrophilic with contact angle 17 ± 1°. A blue shift of 0.30 eV with characteristic absorption peak at 427 nm has been attributed due to quantized size of polyaniline nanograins.     

Theoretical and experimental study of structures and properties of cement paste: The nanostructural aspects of C-S-H

Ordinary Portland cement (OPC) paste with water to cement ratio 0.5 has been studied by FTIR spectroscopy and TEM/SAED techniques. The progressive shift in frequencies and change in intensity of characteristic peaks in the FTIR spectra of cement powder indicate polymerization of silicates due to hydration reaction. The appearance of new peaks around 975-985 and 3640-3650 cm⁻¹ in FTIR spectra of cement paste has been attributed to the formation of two principal hydration products (C-S-H) and Ca(OH)₂, respectively. There is a strong resemblance of peak shape at 980 cm⁻¹ of cement paste with that of synthesized 1.1 nm Tobermorite. TEM/SAED techniques reveal the presence of three distinct types of C-S-H nanostructures viz. spherical particles, fibres and bundle of fibres, and nano tubes in cement paste. Theoretical study of two C-S-H clusters by MNDO and Density Functional Techniques shows excellent agreement between computed structural data and reported experimental results of Tobermorite and Jennite. The computed interplanar Ca-Ca distance (11.162 Å) of C-S-H cluster (Ca/Si=1.125) indicates greater structural similarity of this cluster to 11 Å Tobermorite. There is a strong similarity of IR profile of C-S-H cluster (Ca/Si=1.125) with 1.1 nm Tobermorite. Above study indicates that this cluster is probably the most likely basic unit of C-S-H phases formed during the early stage of OPC cement hydration.     

Dielectric behavior and charge transport in polyaniline nanofiber reinforced PMMA composites

PAni nanofibers synthesized by interfacial polymerization were reinforced in the PMMA matrix in different weight ratios. Randomly oriented polyaniline nanofibers were observed in the TEM image with diameter ranging from 20 to 30 nm. The SEM revealed the microstructure of the fiber reinforced composites showing better connectivity. The XRD spectra of the composites showed peaks at 2θ=17.05°, 20.3°, 27.15° and 30.05° that were indexed in a pseudo-orthorhombic unit cell. The dielectric constant measured over a frequency range of 42 Hz-1 MHz and in the temperature range of 303-373 K showed dependence upon frequency, temperature and concentration of the conducting nanofibers in the composites. The ac conductivity (σ_ac) was interpreted as a power law of frequency. The frequency exponent s was found to lie in the range from 0.4 to 0.65 and decreased with the increase in temperature, which suggested that correlated barrier hopping (CBH) was the dominant charge transport mechanism. Existence of polarons as major charge carriers was confirmed by the low values of polaron binding energy (W_M). Decrease in the values of density of states N(E_F) with the increase in PAni nanofiber concentration indicated increased delocalization of electronic states in the band gap causing the increase in ac conductivity.     

Synthesis of praseodymium oxide nanofiber by electrospinning

Well-defined and uniform Pr₆O₁₁ nanofibers were synthesized by electrospinning of an aqueous sol-gel consisting of praseodymium nitrate hexa-hydrate and polyvinyl acetate. The synthesized Pr₆O₁₁ nanofibers mat was dried at 80 °C for 24 h under vacuum and finally annealed at 600 °C for 2 h in static air furnace. From crystalline properties, the synthesized Pr₆O₁₁ nanofibers XRD analysis revealed the typical cubic structure. The morphological observation showed that the synthesized Pr₆O₁₁ nanofibers composed of fibers length in several 100 nm and diameter of ∼20 nm. Similarly, transmission electron microscope (TEM) measurement revealed the good crystalline nature of the synthesized Pr₆O₁₁ nanofibers with the average diameter of ∼20 nm. Photoluminescence (PL) demonstrated a strong green-blue emission peak at 521 nm, suggesting that the Pr₆O₁₁ nanofiber exhibited good crystal quality with very less structural defects.     

In situ synthesis and characterization of LiNi0.5La0.08Fe1.92O4-polyaniline core-shell nanocomposites

Core-shell-structured LiNi_0.5La_0.08Fe_1.92O₄-polyaniline (PANI) nanocomposites with magnetic behavior were synthesized by in situ polymerization of aniline in the presence of LiNi_0.5La_0.08Fe_1.92O₄ nanoparticles. The structure, morphology and magnetic properties of samples were characterized by powder X-ray diffraction (XRD), Fourier transform infrared (FTIR), UV-vis absorption, transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM) technique. The results of spectroanalysis indicated that there was interaction between PANI chains and ferrite particles. TEM study showed that LiNi_0.5La_0.08Fe_1.92O₄-PANI nanocomposites presented a core-shell structure with a magnetic core of 30-50 nm diameter and an amorphous shell of 10-20 nm thickness. The nanocomposites under applied magnetic field exhibited the hysteresis loops of the ferromagnetic nature. The saturation magnetization and coercivity of nanocomposites decreased with decreasing content of LiNi_0.5La_0.08Fe_1.92O₄. The polymerization mechanism and bonding interaction in the nanocomposites have been discussed.     

Low-temperature growth and ethanol-sensing characteristics of quasi-one-dimensional ZnO nanostructures

ZnO nanorods, nanobelts, nanowires, and tetrapod nanowires were synthesized via thermal evaporation of Zn powder at temperatures in the range 550-600 °C under flow of Ar or Ar/O₂ as carrier gas. Uniform ZnO nanowires with diameter 15-25 nm and tetrapod nanowires with diameter 30-50 nm were obtained by strictly controlling the evaporation process. Our experimental results revealed that the concentration of O₂ in the carrier gas was a key factor to control the morphology of ZnO nanostructures. The gas sensors fabricated from quasi-one-dimensional (Q1D) ZnO nanostructures exhibited a good performance. The sensor response to 500 ppm ethanol was up to about 5.3 at the operating temperature 300 °C. Both response and recovery times were less than 20 s. The gas-sensing mechanism of the ZnO nanostructures is also discussed and their potential application is indicated accordingly.     

Preparation and characterization of polyaniline (PANI)-Mn3O4 nanocomposite

Polyaniline (PANI)-Mn₃O₄ nanocomposite was synthesized by a combination of sonochemical synthesis of Mn₃O₄ NP's and in-situ polymerization of aniline. Structural characteristics were evaluated by XRD, FT-IR, TGA, VSM, TEM and SEM analysis, and conduction characteristics were evaluated by total conductivity measurements in the temperature range of 20-100 °C and frequency range of 0.1 Hz-1 MHz. Our findings show that PANI is successfully coated on nanoparticles surface and overall conductivity of nanocomposite is approximately 50-1000 times higher than that of uncapped Mn₃O₄ or PANI base with increase in temperature. Morphology of the synthesized powder was observed to be thin nanosheets with a thickness of 2-3 nm based on SEM analysis. Room temperature magnetization curves for nanocomposite show no hysteresis, indicating the super-paramagnetic character of the sample in the region of measured field strength. σ_AC increased after polyaniline coating.     

Perovskite nanoparticles: Preparation by reactive milling and magnetic characteristics

La_0.7Sr_0.3MnO₃ and La_0.7Ca_0.3MnO₃ nanoparticles were synthesized by reactive milling method. Grain size determined from XRD, TEM, and magnetization measurements show an average diameter ?18 nm and decreasing with increasing milling time. DC and AC magnetic measurements evidenced an interacting superparamagnetism due to clustering of perovskite nanoferromagnets with spin dynamic time in range of 10⁻⁹–10⁻¹⁰ s.     

Preparation, magnetic and electromagnetic properties of polyaniline/strontium ferrite/multiwalled carbon nanotubes composite

Strontium ferrite particles were firstly prepared by sol-gel method and self-propagating synthesis, and then the polyaniline/strontium ferrite/multiwalled carbon nanotubes composites were synthesized through in situ polymerization approach. Structure, morphology and properties of the composite were characterized by various instruments. XRD analysis shows that the output of PANI increases with the increase of the content of MWCNTs, due to the large surface area of MWCNTs. Because of the coating of PANI, the outer diameter of MWCNTs increases from 10 nm to 20-40 nm. The electrical conductivity of the composites increases with the amount increase of MWCNTs and reaches 7.2196 S/cm in the presence of 2 g MWCNTs. The coercive force of the composites prepared with 2 g MWCNTs is 7457.17 Oe, which is much bigger than that of SrFe₁₂O₁₉ particles 6145.6 Oe, however, both the saturation magnetization and the remanent magnetization of the composite become much smaller than those of SrFe₁₂O₁₉ particles. The electromagnetic properties of the composite are excellent in the frequency range of 2-18 GHz, which mainly depend on the dielectric loss in the range of 2-9 GHz, and mainly on the magnetic loss in the range of 9-18 GHz.     

Reflux synthesis of Co3O4 nanoparticles and its magnetic characterization

Co₃O₄ nanoparticles have been prepared for the first time via reflux method, as an alternative low-temperature high-yield process, starting from one single precursor. A plausible mechanism is suggested for the synthetic process. XRD, TEM, FTIR and VSM were used for the structural, morphological, spectroscopic, and magnetic characterization of the product respectively. X-ray diffraction line profile fitting showed that average particle size of the sample is 28 nm. Morphology of the synthesized powder was observed to be thin nanosheets with a thickness of 2-3 nm based on SEM and TEM analyses. Magnetic measurements showed a deviation of the Neel temperature from the bulk value which is attributed to the finite size effects. A loop shift with an enhanced coercivity is observed in the field-cooled hysteresis loops. The opening of the hysteresis loop reveals the existence of the spin-glass like surface spins of the Co₃O₄ nanoparticles.     

Synthesis of bamboo-leaf-shaped ZnO nanostructures by oxidation of Zn/SiO2 composite films deposited with radio frequency magnetron co-sputtering

Bamboo-leaf-shaped ZnO nanostructures were synthesized by oxidation of metal Zn/SiO₂ matrix composite thin films deposited on Si(1 1 1) substrates with radio frequency magnetron co-sputtering. The synthesized bamboo-leaf-shaped ZnO are single crystalline in nature with widths ranging from 30 to 60 nm and lengths of up to 5-10 μm, room temperature photoluminescence spectrum of the nanostructures shows a strong and sharp UV emission band at 372 nm and a weak and broad green emission band at about 520 nm which indicates relatively excellent crystallization and optical quality of the ZnO nanostructures synthesized by this novel method.     

Nanostructured Fe50Ni50 alloy formed by chemical reduction

A high purity Fe₅₀Ni₅₀ nanometric alloy was synthesized by ultra rapid autocatalytic chemical reduction of the corresponding transition metal ions in an aqueous solution. The ratio of metal concentration in solution is preserved in the precipitated powder alloy and no metal segregation has been detected. The alloy was characterized as a nanostructured chemically disordered taenite phase by X-ray diffraction (XRD) and Mössbauer spectroscopy (MS). Transmission electron microscopy (TEM) showed that the as prepared alloy contained spherical particles with 96 nm mean diameter size. The particles are composed of crystallites (of ∼15 nm size) and a predominant disordered interfacial region. A thermal treatment of 673 K/2 h produced a structural relaxation with a significant narrowing in the XRD and Mössbauer lines with a exothermic flow in the DSC signal and an increase in the crystallite size to 30 nm.     

Synthesis and characterization of Sr(ZnZr)x Fe12−2xO19-PANI composites

Strontium zinc zirconium hexaferrites/polyaniline (Sr(ZnZr)_xFe_12−2xO₁₉-PANI, x=0, 0.5, 1.0) composites were synthesized by oxidative chemical polymerization of aniline in the presence of ammonium peroxydisulfate (APS). The structure and morphology of the product was characterized by FTIR, TGA and SEM. The particle size of the core material was found to be about 250-500 nm. After coating with polyaniline, the particle size of Sr(ZnZr)_0.5Fe₁₁O₁₉-PANI composites grew upto 0.5-1.0 μm. XRD of the ferrites indicated that the structure of the core materials is hexagonal, with lattice constants around 5.886-5.885 Å. It was found that the saturation magnetization (M_S) and coercivity (H_C) for Sr(ZnZr)_xFe_12−2xO₁₉-PANI composites decreased after polyaniline coating. The composite under applied magnetic field, exhibited ferromagnetic hysteretic loops with high saturation magnetization (M_S=18.9-3.8 emu/g) and coercivity (H_C=3850.0-583.91 Oe).     

Synthesis of lanthanum nickelate perovskite nanotubes by using a template-inorganic precursor

A new route to obtain metal oxide nanotubes is presented: an inorganic coordination complex precursor containing the metal ions and impregnated into alumina membrane templates yield hollow tubular nanostructures of LaNiO₃ by calcination at 600 °C as characterized by powder X-ray diffraction (XRD). Scanning electron microscopy (SEM) shows that the resulting nanotubes have 200 nm in diameter in good agreement with the template pore. Transmission electron microscopy (TEM) and dark field transmission electron microscopy (DF-TEM) show that the nanotubes with 10-20 nm walls and internal separations are composed of 3-5 nm crystals.     

Structural, optical and electrical characterization of antimony-substituted tin oxide nanoparticles

Antimony-doped tin oxide (ATO) nanostructures were prepared using chemical precipitation technique starting from SnCl₂, SbCl₃ as precursor compounds. The antimony composition was varied from 5 to 20 wt%. The lower resistance was observed at composition of Sn:95 and Sb:05, when compared with undoped and higher doping concentration of antimony. The average crystalline size of undoped and doped tin oxide was calculated from the X-ray diffraction (XRD) pattern and found to be in the range of 30-11 nm and it was further confirmed from the transmission electron microscopy (TEM) studies. The scanning electron microscopy (SEM) analysis showed that the nanoparticles agglomerates forming spherical-shaped particles of few hundreds nanometers. The samples were further analyzed by energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and electrical resistance measurements.     

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.     

Interfacial p-n heterojunction of polyaniline-nickel ferrite nanocomposite as room temperature liquefied petroleum gas sensor

In this work, we introduce polyaniline–nickel ferrite (PANI-NF) nanostructured composite to detect liquefied petroleum gas (LPG) at room temperature. The composite synthesized by relatively simple method of in-situ chemical polymerization was structurally characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques. The presence of characteristic absorption bands of both PANI and NF in the FTIR spectrum of the composite with small shifts confirmed interfacial interaction of PANI with NF. The XRD studies also confirmed interfacial interaction between PANI and NF in the composite and its crystalline nature with an average crystallite size of 20 nm. Highly agglomerated granular porous morphology favourable for LPG adsorption was revealed by SEM image of the composite. The TEM image of the composite clearly showed nanosized NF particles embedded in PANI matrix. The LPG sensing performance of the composite at room temperature was tested using a film prepared by depositing the composite on an ordinary glass substrate by cost-effective spin coating technique. The maximum sensing response of the composite was found to be 57% at 700 ppm of LPG, with a response time of 50 s and a recovery time of 200 s. The composite was found to be stable for a period of one month. The sensing mechanism has been discussed on the basis of formation of interfacial p–n heterojunction barrier.     

Microwave synthesis, characterization, and electrochemical properties of α-Fe2O3 nanoparticles

Ultrafine α-Fe₂O₃ nanoparticles with an extremely narrow distribution were synthesized by microwave heating. Transmission electron microscopy (TEM) images showed that most primary particles have ellipsoid shapes, and the average diameter of the primary particles was less than 10 nm. The electron diffraction pattern and fringes in some particles in TEM images showed that these nanoparticles were single crystals. The BET surface area of the freeze-dried product was 217 m²/g. The initial discharge capacity of the α-Fe₂O₃ nanoparticles exceeded 1007 mA/g (cut-off voltage: 0.5 V). This large capacity corresponds to that calculated by assuming the reduction of Fe³⁺ to Fe⁰. The α-Fe₂O₃ nanoparticles also work as a rechargeable electrode material. The charge-discharge test between 4 V and 1.5 V gave a good rechargeable capacity of about 150 mAh/g.     

The effect of substrate surface roughness on ZnO nanostructures growth

The ZnO nanowires have been synthesized using vapor-liquid-solid (VLS) process on Au catalyst thin film deposited on different substrates including Si(1 0 0), epi-Si(1 0 0), quartz and alumina. The influence of surface roughness of different substrates and two different environments (Ar + H₂ and N₂) on formation of ZnO nanostructures was investigated. According to AFM observations, the degree of surface roughness of the different substrates is an important factor to form Au islands for growing ZnO nanostructures (nanowires and nanobelts) with different diameters and lengths. Si substrate (without epi-taxy layer) was found that is the best substrate among Si (with epi-taxy layer), alumina and quartz, for the growth of ZnO nanowires with the uniformly small diameter. Scanning electron microscopy (SEM) reveals that different nanostructures including nanobelts, nanowires and microplates have been synthesized depending on types of substrates and gas flow. Observation by transmission electron microscopy (TEM) reveals that the nanostructures are grown by VLS mechanism. The field emission properties of ZnO nanowires grown on the Si(1 0 0) substrate, in various vacuum gaps, were characterized in a UHV chamber at room temperature. Field emission (FE) characterization shows that the turn-on field and the field enhancement factor (β) decrease and increases, respectively, when the vacuum gap (d) increase from 100 to 300 μm. The turn-on emission field and the enhancement factor of ZnO nanowires are found 10 V/μm and 1183 at the vacuum gap of 300 μm.     

Magnetic and microwave absorbing properties of polyaniline/γ-Fe2O3 nanocomposite

The conducting protonated polyaniline (ES)/γ-Fe₂O₃ nanocomposite with the different γ-Fe₂O₃ content were synthesized by in-situ polymerization. Its morphology, microstructure, DC conductivity and magnetic properties of samples were characterized by transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), four-wire-technique, and vibrating sample magnetometer (VSM), respectively. The microwave absorbing properties of the nanocomposite powders dispersing in wax coating with the coating thickness of 2 mm were investigated using a vector network analyzers in the frequency range of 7–18 GHz. The pure ES has shown the absorption band with a maximum absorption at approximately 16 GHz and a width (defined as frequency difference between points where the absorption is more than 8 dB) of 3.24 GHz, when 10% γ-Fe₂O₃ by weight is incorporated , the width is broadened to 4.13 GHz and some other absorption bands appear in the range of 7–13 GHz. The parameter dielectric loss tan δ_e (=ε″/ε′) in the 7–18 GHz is found to decrease with increasing γ-Fe₂O₃ contents with 10%, 20%, 30%, respectively, but magnetic loss tan δ_m (=μ″/μ′) increases with increasing γ-Fe₂O₃ contents. The results show that moderate content of γ-Fe₂O₃ nanoparticles embedded in protonated polyaniline matrix may create advanced microwave absorption properties due to simultaneous adjusting of dielectric loss and magnetic loss.