Synthesis and structural characterization of urea–isobutyraldehyde–formaldehyde resins

Urea–isobutyraldehyde–formaldehyde (UIF) resins were synthesized using urea, isobutyraldehyde, and formaldehyde; sulfuric acid was used as a catalyst. The effects of molar ratio of urea/isobutyraldehyde/formaldehyde (U/I/F) on the properties of resins were investigated, and the structures of the resins were characterized by FTIR, ¹H-NMR, and ¹³C-NMR. When U/I/F was 1.0/3.6/2.4, the yield of the resin was 76.5%. The softening point and hydroxyl value were 90°C and 32 mg KOH/g, respectively. The FTIR, ¹H-NMR, and ¹³C-NMR results showed that an α-ureidoalkylation reaction occurred between urea and isobutyraldehyde to form a lactam. The UIF resins also contained hydroxyl groups and aldehyde groups; the content of aldehyde groups in the resin increased as the amount of isobutyraldehyde increased.     

Synthesis,characterization, and electrical properties of polypyrrole–bimetallic oxide composites

In this study, polypyrrole (PPy) and its bimetallic oxide composites (PPy–V₂O₅–MnO₂) were synthesized via a modified chemical oxidation polymerization method in the aqueous medium with FeCl₃·6H₂O as an oxidant. The synthesized materials were characterized with various analytical techniques to investigate their structural, crystallographic, thermal, morphological, optical, and electrical properties. The Fourier transform infrared study confirmed the successful synthesis of the materials, whereas the X-ray diffraction analyses showed the amorphous and crystalline natures of the PPy and PPy–V₂O₅–MnO₂ composites, respectively. The bimetallic oxide content improved the thermal stability of the composites, as ratified by thermal analysis. The synthesized PPy had a globular and spongy nature, whereas the composites were mixtures of short and long rod-shaped particles. The bimetallic oxide blend enhanced the doping, surface area and semiconducting nature of composites, and lower electrical resistance compared with those of the PPy. The resistance of the synthesized materials depended on the V₂O₅–MnO₂ blend content in the composites and the temperature. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2020 , 137, 47680.     

Synthesis,characterization and controlled release properties of zinc–aluminium-beta-naphthoxyacetate nanocomposite

An organic–inorganic nanohybrid nanocomposite was synthesized by co-precipitation method using beta-naphthoxyacetate (BNOA) as guest anion and zinc–aluminium layered double hydroxide (Zn–Al-LDH) as the inorganic host. A well-ordered nanohybrid nanocomposite was formed when the concentration of BNOA was 0.08 M and the molar ratio of Zn to Al, R = 2. Basal spacing of layered double hydroxide containing nitrate ions expanded from 8.9 to 19.5 Å in resulting of Zn–Al-BNOA nanocomposite was obtained indicates that beta-naphthoxyacetate was successfully intercalated into interlayer spaces of layered double hydroxide. It was also found out the BET surface area increased from 1.13 to 42.79 m² g^?1 for Zn–Al-LDH and Zn–Al-BNOA nanocomposite, respectively. The BJH average pore diameter of the synthesized nanocomposite is 199 Å which shows mesoporous-type of material. CHNS analysis shows the Zn–Al-BNOA nanocomposite material contains 36.2 % (w/w) of BNOA calculated based on the percentage of carbon in the sample. Release of BNOA from the lamella of Zn–Al-BNOA was controlled by the zeroth and first order kinetics at the beginning of the deintercalation process up to 200 min and controlled by pseudo-second order kinetics for the whole process. This study suggests that layered double hydroxide can be used as a carrier for organic acid herbicide controlled release formulation of BNOA.     

Thermal,mechanical and structural investigation of copolyimide–silica hybrids containing phosphine oxide

In this study, a novel hybrid copolyimide was synthesized from copolyamic acid solutions (PAAs) obtained by the reaction between bis(3-aminophenoxy-4-phenyl)phenylphosphine oxide (m-BAPPO), 3,3′-diaminodiphenyl sulfone (DDS) and 3,3′,4,4′-benzophenone tetracarboxylic dianhydride (BTDA), followed by thermal imidization. Hybrid materials containing 5% SiO₂ were synthesized by sol–gel technique. The polyimide–silica hybrids were characterized by Fourier Transform Infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). Thermogravimetric analysis showed that the weight loss of hybrids is shifted to the higher temperature compared to the neat copolyimide. The contact angle measurements confirmed the hydrophobic surface of hybrids. Moreover, the gas permeability measurements were also done to take a step for forthcoming gas separation studies. The tensile modulus and strength of the copolyimides are good.     

Morphological,structural, dielectric and electrical properties of PEO–ZnO nanodielectric films

The morphological, structural, dielectric and electrical properties of aqueous solution-cast prepared poly(ethylene oxide)–zinc oxide (PEO–ZnO) nanocomposite films have been investigated as a function of ZnO nanoparticle concentrations up to 5 wt%. Scanning electron microscopy (SEM) images of these films show that the morphology of pristine PEO aggregated spherulites changes into fluffy, voluminous and highly porous with dispersion of ZnO nanoparticles into the PEO matrix. X-ray diffraction (XRD) study confirms that the crystalline phase of PEO greatly reduces at 1 wt% ZnO, and it again increases gradually with further increase of ZnO concentration. The dielectric relaxation spectroscopy (DRS) over the frequency range 20 Hz–1 MHz reveals that the real part of complex dielectric permittivity at audio frequencies decreases non-linearly whereas it remains almost constant at radio frequencies for these polymeric nanocomposites. Dispersion of nanosize ZnO particles into the PEO matrix reduces the values of dielectric permittivity which also exhibits a correlation with the dispersivity of ZnO nanoparticles. The relaxation peaks observed in the dielectric loss tangent and electric modulus spectra reveal that the electrostatic interactions of nanoscale ZnO particles with the ethylene oxide functional dipolar group of PEO monomer units decrease the local chain segmental dynamics of the polymer. Real part of ac conductivity spectra of these films have been analyzed by power law fit over the audio and radio frequency regions, respectively, and the obtained dc conductivity values for these regions differ by more than two orders of magnitude. The temperature dependent relaxation time and dc conductivity values of the nanodielectric material obey the Arrhenius relation of activation energies and confirm a correlation between dc conductivity and PEO chain segmental motion which is exactly identical to the characteristics of solid polymer electrolytes. Results imply that these nanocomposite materials can serve as low permittivity flexible nanodielectric for radio frequency microelectronic devices and also as electrical insulator for audio frequency operating conventional devices in addition to their suitability in preparation of solid polymer electrolytes.     

Homoleptic manganese(II)–azide layer: Synthesis,structural characterization and magnetic properties

A host–guest compound {(MV)[Mn(N₃)₄]}_n (1), where MV²⁺ (methylviologen dication) is generated in situ through the decarboxylation of 4,4′-dipyridinio-N,N′-diacetate, has been synthesized and characterized by X-ray crystallography and magnetic measurements. This is the first homoleptic two-dimensional Mn–azide compound, which contains single μ_1,3-azide bridged Mn(II) square layers with the organic MV²⁺ cations intercalated between the inorganic layers. Magnetic studies show antiferromagnetic interactions between adjacent metal ions (J = ?4.4 cm^?1), and the symmetric feature of the structure precludes the possibility of spin canting in this compound.     

Preparation,structural and thermo-mechanical properties of lithium aluminum silicate glass–ceramics

Lithium aluminum silicate glasses of composition (wt%) 12.6Li₂O–71.7SiO₂–5.1Al₂O₃–4.9K₂O–3.2B₂O₃–2.5P₂O₅ were prepared by the melt quench technique. These glasses were converted to glass–ceramics based on DTA data. X-ray diffraction (XRD) and Fourier transform infra-red spectroscopy (FTIR) were used to discern the phases evolved in the glass–ceramics. Phase morphology was studied using scanning electron microscopy (SEM). Thermal expansion coefficient (TEC) and glass transition temperature (T_g) of all samples were measured using thermo-mechanical analyzer (TMA). It was found that 3 h dwell time at crystallization temperature yielded samples with good crystallinity with a TEC of 9.461 × 10⁻⁶ °C⁻¹. Glass–ceramic-to-metal compressive seal with SS-304 was fabricated using LAS glass–ceramic. The presence of metal housing and compressive stresses at the glass–ceramic-to-metal interface reduced average grain size and changed the overall microstructure.     

Physical properties and electrochemical performance of molybdenum–lead-germanate glasses and glass ceramics

Glasses and glass ceramics of the xMoO₃(100?x)[7GeO₂·3PbO] system where x=0–30 mol% MoO₃ were synthesized and characterized in order to obtain information about the structural correlations and the relationship between structure and physical properties in these materials. Changes of the FTIR, UV–vis and EPR data are discussed in view of the glass network structural changes determined by the evolution of molybdenum ions state, glass composition and MoO₃ concentration.The spectroscopic studies indicate that with increasing of MoO₃ content a fraction of the Mo⁶⁺ ions convert Mo³⁺ and Mo⁵⁺ ions. Accordingly, these modifications cause the depolymerization of the host network, the increase of the structural disorder and formation of GeO₂ and PbMoO₄ crystalline phases. The shape of EPR spectra is modified by the increase of the MoO₃ concentration indicating that molybdenum ions exists in glass and glass ceramics in more than one valence state. The EPR spectra contain a broad line located at g～5.2 and, for the samples with a MoO₃ content up to x≥15 mol%, the presence of the hyperfine structure characteristic for the Mo⁵⁺ ions can be observed, too.The electrochemical performances of the glass and glass ceramics samples with x=10 and 30 mol% MoO₃ were demonstrated by cyclic voltammetry.     

Sol-gel–mediated synthesis of TiO2 nanocrystals: Structural,optical, and electrochemical properties

Nanoparticles of titanium dioxide were prepared using the sol-gel method without any impurity. Rietveld refinement of XRD data confirmed the anatase phase of synthesized nanoparticles with space group I4_1/amd (141). XRD pattern revealed the crystalline nature of synthesized nanopowder. The average crystallite size of synthesized nanoparticles was calculated 7.5 nm. The electrochemical performance of synthesized TiO₂ nanopowder was investigated as working electrode. The electrochemical reaction was found diffusion-controlled as observed from cyclic voltammetry (CV) studies at different scan rates. The diffusion-controlled charge storage mechanism also confirmed by charge transfer resistance and Warburg impedance, as calculated from the EIS analysis. SEM micrograph showed the plate-like structure grown in cluster cloud of particles of synthesized TiO₂ nanocrystals. Absorbance and optical bandgap were obtained using UV-Vis spectra. De-convoluted PL spectra provided the emission pattern from the ultra-violet region to green region due to the presence of interstitial oxygen vacancies. The tune bandgap with EIS measurements of synthesized TiO₂ nanoparticles offers its potential application in energy storage devices and photovoltaic applications.     

Synthesis and structural,morphological, compositional,optical and electrical properties of DBSA-doped PPy–WO3 nanocomposites

Synthesis of DBSA-doped PPy–WO₃ (organic–inorganic) nanocomposites, using a novel approach, has been proposed, and further envisaged for their structural, compositional, morphological, optical and electrical properties. DBSA-doped PPy–WO₃ nanocomposites demonstrate superior above mentioned properties than their counterparts i.e. either PPy or WO₃. The XRD spectra of nanocomposites supported to conclude that both i.e. PPy and DBSA have no impact on the crystallinity of WO₃ nanoparticles. The chemical structure of DBSA-doped PPy–WO₃ nanocomposites have been elucidated using FTIR spectra. The morphologies and surface roughnesses of the DBSA-doped PPy–WO₃ nanocomposites were confirmed using scanning electron microscope and atomic force microscope images, respectively. Interconnected type morphology and 13 nm average surface roughness were confirmed for DBSA doped PPy–WO₃ hybrid nanocomposites. The EDX and XPS analyses evidence that, the formation of DBSA doped PPy–WO₃ hybrid nanocomposites without any elemental impurities. The absorption peak of DBSA-doped PPy–WO₃ nanocomposites shift towards the lower wavelength side as compared to the PPy–WO₃ (50%) hybrid nanocomposites. Anionically charged sulfonate group which is supposed to stabilize doped state of the DBSA-PPy–WO₃ nanocomposites, may be responsible for this shift. The dc electrical conductivity of DBSA-doped PPy–WO₃ nanocomposites increases as the content of DBSA is increased from 10 to 50% this could be accounted for by the generation of conduction path through the PPy–WO₃ nanocomposites as DBSA has anionic surfactant nature by preventing an agglomeration of functional material.     

Synthesis,characterization, and magnetic properties of α-MnS nanocrystals

MnS nanocrystals have been prepared by a colloidal synthesis route through the reaction of MnCl₂ and S[Si(CH₃)₃]₂ in trioctylphosphineoxide. The nanocrystals were characterized using X-ray diffraction and transmission electron microscopy. The magnetic properties were studied with SQUID magnetometry. X-ray diffraction shows that the nanocrystals are of the thermodynamically stable α-MnS (alabandite) structure. Size control was achieved by changing the concentration of the precursors. Nanocrystal sizes were measured by transmission electron microscopy, and three samples of average diameters 20, 40, and 80 nm were obtained, with narrow size distribution (σ˜9%). The zero field cooled magnetization curves for the 80-, 40-, and 20-nm samples showed a cusp at 116 K, 97 K, and 50 K respectively, all smaller than the antiferromagnetic transition temperature, T_N = 130 K, of bulk α-MnS. Below T_N the magnetization exhibits a paramagnetic behavior unlike typical antiferromagnetic materials. These results indicate that there is a mixture of paramagnetic and antiferromagnetic phases in the nanocrystals. The size dependence shows a general trend of decrease of T_N with reduced particle size, indicating size dependent magnetic ordering.     

Synthesis,characterization, and photophysical properties of covalent-linked ferrocene–porphyrin–single-walled carbon nanotube triad hybrid

The ferrocene–porphyrin–single-walled carbon nanotube (Fc–H₂P–SWCNT) triad hybrid was prepared by amidation reaction between carboxylated SWCNT and aminoporphyrin bearing an appended ferrocenyl substituent. The hybrid described here was fully characterized by a combination of analytical techniques such as Fourier transform infrared spectroscopy, Raman, absorption and emission spectroscopy, atomic force and scanning electron microscopy, thermogravimetric analysis, and X-ray photoelectron spectroscopy. The steady emission characteristics revealed the existence of the effective photoinduced electron transfer among ferrocene, excited porphyrin moiety and SWCNT, which was further confirmed by the results of time-resolved transient absorption spectra. The final lifetime of charge-separation state was observed to be 62.9 μs in N,N-dimethylformamide, which was significant increased compared to the reference nanohybrid porphyrin–SWCNT and the reported ferrocene–porphyrin–fullerene triad. Therefore, Fc–H₂P–SWCNT triad hybrid constructed by amidation is rationally expected to be an improved photon-to-electron conversion system.     

Thermo and electrochemical characterization of sulfonated PEEK–WC membranes and Krytox-Si-Nafion® composite membranes

Two types of membranes, the sulfonated PEEK-WC (poly(oxa-p-phenylene-3,3-phthalido-p-phenylene-oxyphenylene)(SPWC) and Krytox-Si-Nafion® (KSiN) composite membranes are proposed for DMFC applications.The properties based on water uptake, ion exchange capacity, proton conductivity, gas permeability, thermal stabilityand methanol crossover are summarized. The comparative studies on SPWC and Nafion® 117 membranes clarify us that the amorphous sulfonated PEEK-WC polymer shows thermal and mechanical stability with less methanol flux and gas permeability. The membrane also exhibits the increase in water uptake, ion exchange capacity and proton conductivity as sulfuric acid doping agent concentration was increased. The KSiN is unique in term of its miscible hybrid structure of silica particles modified with Nafion® structured Krytox 157 FSL chain (KSi) andNafion®. Based on the KSiN membranes with different KSi content, it was found that when KSi content increased, the reduction of gas permeability, methanol crossover and thermal stability are improved. The composite membrane performs the proton conductivity in the wide range of high temperature (60–130°C).     

Sol-gel synthesis,structural, morphological and magnetic properties of BaTiO3–BiMnO3 solid solutions

In this study, solid solutions of (1-x)BaTiO₃-xBiMnO₃ have been synthesized by an aqueous sol-gel method. It was determined that single-phase compounds can be obtained up to x = 0.6 and with further increase in percentage of BiMnO₃ component additional crystal phases were detected. Perovskite crystal structure was determined for all synthesized compounds regardless of chemical composition. Raman spectra of synthesized solid solutions showed gradual change of the shape with an increase of BiMnO₃ fraction. It was demonstrated that partial substitution of BaTiO₃ by BiMnO₃ led to the drastic growth of grains of the end products. Magnetization measurements showed that all BiMnO₃-containing samples are characterized by paramagnetic behavior. Clear correlation between magnetization values and composition of the materials was observed, magnetization values increased with increasing of BiMnO₃ content in solid solutions.     

Study of the mechanical and structural properties of Zn–Ni–Co ternary alloy electroplating

Ternary zinc–nickel–cobalt alloys were electrodeposited on steel substrates from sulfate bath by direct current. Microstructural and mechanical properties of Zn–Ni–Co ternary alloy coatings were investigated and contrasted with the characteristics of Zn–Ni and Zn–Co alloy coatings. It was found that the obtained Zn–Ni–Co alloy exhibited more preferred surface morphology and mechanical properties as compared to the other alloy coatings electroplated at the same conditions. X-ray diffraction studies showed that the deposits of Zn–Ni–Co alloy coatings consisted of Zn, ZnNi₃, and ZnCo₁₃ phases. The structure, surface morphology, and surface topography of the deposited alloys were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) with energy dispersive X-ray microanalysis (EDS), and atomic force microscopy (AFM). In addition, hardness, elasticity modulus, and adhesion strength of coated alloys were measured with dynamic ultra-microhardness (DUH) and Scratch tester.     

Effect of heat treatment on structural,morphological, dielectric and magnetic properties of Mg–Zn ferrite nanoparticles

Green combustion was used to prepare a ferrite composition of Mg_0.4Zn_0.6Fe₂O₄ using a blend of fresh lemon juice as a natural fuel-reductant. Effect of heat treatment on phase, morphological, dielectric, and humidity sensor properties is discussed. The formation of a cubic spinel ferrite has been established by XRD-diffraction and vibrational spectroscopic studies. The experimental lattice parameter ranges from 8.3721 to 8.3631 Å. The broadening of octahedral band (υ₂) in the vibrational spectra is an identification for the existence of ferrite nanoparticles in various sizes. The typical crystallite size ranges from 10.2 to 36.9 nm. Using micrographs obtained from field-effect scanning electron microscopy (FESEM), researchers observed a spherical-shaped microstructure with agglomerated nanoparticles. Dielectric investigations have shown that the current ferrite composition has typical dielectric dispersion. The highest reported value for saturation magnetization (M_s) in the present study is 33 emu/g. Magnetic behaviour is primarily influenced by magnetocrystalline anisotropy, cation distribution, and crystallite size. The existence of void spaces in the sintered samples, as well as their porous nature, rendered them suitable for humidity sensor applications. Sintered samples have good sensing capability at 900 °C. The current findings are integrated in terms of cation distribution and magnetocrystalline anisotropy, assuming fine size effects of ferrite nanoparticles.     

A study of the structural and morphological properties of Ni–ferrite,Zn–ferrite and Ni–Zn–ferrites functionalized with starch

Zinc–ferrite, nickel–ferrite and mixed nickel–zinc ferrites were successfully synthesized via the thermal decomposition method from acetylacetonate complexes. To control the particle size and enhance dispersibility in an aqueous medium, starch, a natural and biocompatible compound, was used for the first time for coating such magnetic powders. X-ray powder diffraction (XRPD) was performed to study the structural properties of all samples. The presence of a single-phase spinel structure as well as the cation distribution in both sites of all investigated magnetic powders was confirmed. The values of unit cell parameters obtained from the results of the Rietveld analysis decreased, while the average crystallite size increased with increasing Ni²⁺ content. The average microstrain parameters unambiguously showed a change in the spinel structure with cation distribution. Scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS) and Fourier transform infrared spectroscopy (FTIR) analyses were also utilized to characterize the synthesized materials, corroborating the XRPD data. The obtained results indicated that functionalization by starch was successfully achieved.     

Effects of Ca–Gd co-substitution on the structural,magnetic, and dielectric properties of M-type strontium hexaferrite

Sr_1−xCa_xFe_12−xGd_xO₁₉ (x = 0, 0.04, 0.08, 0.12, 0.16, 0.20) hexaferrites were characterized by several techniques, such as X-ray diffraction, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy, and vibrating sample magnetometer. Structural results indicate the formation of a pure-phase Sr_1−xCa_xFe_12−xGd_xO₁₉ hexaferrite with space group P6₃/mmc. SEM photography confirms that there are a smaller number of defects due to the reduced porosity and surface area (increased particle size). Magnetic investigations showed a rise of the coercive force from 5069.8 to 5757.4 Oe and saturation magnetization from 79.25 to 80.68 emu/g. The maximum values appear to be for sample x = 0.16, which may be useful in such as permanent magnets, and high-density media for magnetic storage devices. Dielectric parameters, such as conductivity, the real part of permittivity, dielectric loss, dielectric tangent loss, and complex modulus, were studied. Impedance analysis shows that the conduction process is mainly governed by the long-range movement of the charge carriers based on the Debye model for x = 0.12.