High-PL efficiency of polyaniline using various dopants

Polyaniline (PANI) was doped with hydrochloric acid (HCl), succinic acid (C₄H₆O₄) and sulphuric acid (H₂SO₄) by chemical oxidation method. The samples were characterized by using various techniques such as XRD, photoluminescence IR and UV spectroscopy. FTIR study confirmed the presence of dopant molecules in the molecular structure. UV spectra revealed that absorption peaks at 350 nm and 600 nm are due to π–π* transition of polyaniline. The strong band at 600 nm showed extension of polymer chains in the prepared samples. XRD pattern confirmed the amorphous nature of polymer samples. The photoluminescence (PL) spectrum shows good emission at 490 nm. The intensity of photoluminescence depends upon the dopants nature.     

Application of polyaniline nanowires electrodeposited on the FTO glass substrate as a counter electrode for low-cost dye-sensitized solar cells

Polyaniline nanowires (PANI NWs) were deposited onto fluorine-doped tin oxide (FTO) glass substrate using the cyclic voltammetric method with aniline monomer precursor in HCl aqueous solution. The secondary oxidation peak plays an important role in polymerization of aniline monomer and the optimization of catalytic activity of PANI-based counter electrodes was achieved by controlling the number of cycles. The photovoltaic performance of the dye-sensitized solar cells (DSSCs) with PANI NWs counter electrodes (CEs) was optimized at 4th cycles, and then following parameters were obtained: J_sc = 17.2 mA cm⁻², V_oc = 0.71 V, FF = 59.3%, and efficiency (η) = 7.24%. While, J_sc = 14.7 mA cm⁻², V_oc = 0.77 V, FF = 70.6%, and efficiency (η) = 7.98% in cells with Pt CEs. The PANI NWs were attractive as an alternative CEs for the low-cost DSSCs instead of Pt.     

Synthesis and microwave absorption properties of graphene-oxide(GO)/polyaniline nanocomposite with gold nanoparticles

A composite of graphene/PANI/GAunano is synthesized using the co-blend method. The morphologies and microstructures of samples are examined by transition electron microscopy(TEM) and Fourier transform infrared spectroscopy(FTIR). Moreover, the microwave absorption properties of both graphene/PANI and GO/PANI/ GAunano composites are investigated in a microwave frequency band from 1 GHz to 18 GHz. The maximum reflection loss(RL) of GO/PANI/GAunano with a thickness of 2 mm is up to-24.61 d B at 15.45 GHz, and the bandwidth corresponding to RL at-10 d B can reach 4.08 GHz(from 13.92 GHz to 18.00 GHz) for a 2-mm-thick layer. The electromagnetic data demonstrate that GO/PANI/GAunano can be used as an attractive candidate for microwave absorbers.     

Sonocatalytic rapid degradation of Congo red dye from aqueous solution using magnetic Fe0/polyaniline nanofibers

Nano-sized magnetic Fe⁰/polyaniline (Fe⁰/PANI) nanofibers were used as an effective material for sonocatalytic degradation of organic anionic Congo red (CR) dye. Fe⁰/PANI_, was synthesized via reductive deposition of nano-Fe⁰ onto the PANI nanofibers at room temperature. Prepared catalyst was characterized using HR-TEM, FE-SEM, XRD, FTIR instruments. The efficacy of catalyst in removing CR was assessed colorimetrically using UV–visible spectroscopy under different experimental conditions such as % of Fe⁰ loading into the composite material, solution pH, initial concentration of dye, catalyst dosage, temperature and ultrasonic power. The optimum conditions for sonocatalytic degradation of CR were obtained at catalyst concentrations = 500 mg.L⁻¹, concentration of CR = 200 ppm, solution pH = neutral (7.0), temperature = 30 °C, % of Fe⁰ loading = 30% and 500 W ultrasonic power. The experimental results showed that ultrasonic process could remove 98% of Congo red within 30 min with higher Q_max value (Q_max = 446.4 at 25 °C). The rate of degradation of CR dye was much faster in this ultrasonic technique rather than conventional adsorption process. The degradation efficiency declined with the addition of common inorganic salts (NaCl, Na₂CO₃, Na₂SO₄ and Na₃PO₄). The rate of degradation suppressed more with increasing salt concentration. Kinetic and isotherm studies indicated that the degradation of CR provides pseudo-second order rate kinetic and Langmuir isotherm model compared to all other models tested. The excellent high degradation capacity of Fe⁰/PANI under ultrasonic irradiation can be explained on the basis of the formation of active hydroxyl radicals (OH) and subsequently a series of free radical reactions.     

Synthesis and significantly enhanced microwave absorption properties of hematite dendrites/polyaniline nanocomposite

Hematite dendrites/polyaniline (HDs/PANI) nanocomposite, i.e. coating HDs with conductive PANI, has been successfully synthesized through a two-step polymerization of aniline monomers on the surface of pre-synthesized HDs for the first time. It is discovered that a lower concentration of HCl (0.02 mol?L^?1) has only a slight adverse effect on the dendritic structures of the coated HDs, while a higher concentration of HCl (0.04 mol?L^?1) results in severe damage to the sub-branches of the HDs. The morphology, composition, structure, static magnetic, and spectral properties of the as-prepared pristine HDs and HDs/PANI composites were thoroughly characterized by various physicochemical techniques. Moreover, the electromagnetic and microwave absorbing properties of the HDs and HDs/PANI wax composites were compared in detail. It was found that the frequency of absorption obeys a quarter-wavelength model for both of them, and the HDs/PANI wax composite exhibits far superior microwave absorption properties. This phenomenon can be attributed to the improved dielectric loss abilities and the complementary behaviors resulting from the PANI coatings and fractal-structured HDs.     

Dielectric and impedance studies of DBSA doped polyaniline/PVC composites

Polyaniline (PANI) was doped with dodecylbenzene sulfonic acid (DBSA) and then mixed with PVC by solution blending method to prepare DBSA doped PANI (PAND)/PVC composites. FTIR spectroscopy indicates the strong dipole–dipole interaction between the individual components of the composites. The ac electrical properties of the synthesized composites were investigated by complex impedance spectroscopy in the frequency range of 0.5–10⁶ Hz at room temperature. Both dielectric loss factor and permittivity increase with the decrease of frequency exhibiting strong interfacial polarization at low frequency. Addition of PAND in PVC reduces the charge trapping centers by increasing the number of conducting channels participating in the relaxation process; hence an increase in conductivity is observed.     

Synthesis and electrochemical performance of Li1+xV3O8 as cathode material prepared by citric acid and tartaric acid assisted sol–gel processes

Lithium-ion battery cathode material Li_1+xV₃O₈ is synthesized by a citric acid/tartaric acid assisted sol–gel method and sintered at 350 °C, 450 °C and 550 °C for 3 h for the formation of Li_1+xV₃O₈ phase. The synthesized samples were fully characterized by FTIR, TG/DTA, XRD, SEM, EIS and charge–discharge tests. Li_1+xV₃O₈ material synthesized by tartaric acid assisted route and sintered at 450 °C for 3 h shows best electro-chemical performance. It shows a high initial capacity of 249 mAh g^?1 and still reserves a discharge capacity of 260 mAh g^?1 after 50 cycles. Moreover, in the case of tartaric assisted products, no capacity decadence is observed in 50 cycles. XRD together with TG/DTA measurements reveal that compared with citric acid assisted products, the adoption of tartaric acid as chelating agent effectively lowers the crystallization temperature of amorphous Li_1+xV₃O₈. Therefore, precursors obtained by tartaric acid route calcinated at 450 °C for 3 h exhibit lower crystallinity and smaller grain size, which contributes to the better electrochemical performance of the cathode electrodes. From EIS measurements, the bulk resistance is reduced, which favors the intercalation and de-intercalation of lithium ions while cycling.     

A simultaneous,direct microwave/ultrasound-assisted digestion procedure for the determination of total Kjeldahl nitrogen

Simultaneous direct irradiation with microwaves and ultrasound was used to determine total Kjeldahl nitrogen. The method involves chemical digestion in two steps, mineralization with sulfuric acid and oxidation with H₂O₂. The most influential variables for the microwave/ultrasound (MW/US)-assisted digestion were optimized using tryptophan as the model substance. The optimum conditions were: H₂SO₄ volume, 10 mL; H₂O₂ volume, 5 mL; weight of sample, 0.05 g; MW power, 500 W; US power, 50 W; digestion time, 7 min (i.e., 5 min mineralization and 2 min oxidation). A modification of the classical Kjeldahl (Hach) method and an US-assisted digestion method were used for comparison. The latter was also optimized; the optimum conditions were: H₂SO₄ volume, 10 mL; H₂O₂ volume, 5 mL; sonication time with H₂SO₄, 15 min; sonication time with H₂O₂,10 min; US power, 50 W; weight of sample, 0.05 g. Five pure amino acids and two certified reference materials (NIST standard reference materials 1547 (peach leaves), and soil, NCS DC 73322) were analyzed to assess the accuracy of our new MW/US-assisted digestion method, that was successfully applied to five real samples. The significant reduction in digestion time (being 30 min and 25 min for classical Kjeldahl and US-assisted digestion methods, respectively) and consumption of reagents show that simultaneous and direct MW/US irradiation is a powerful and promising tool for low-pressure digestion of solid and liquid samples.     

Electrochemical synthesis of nanocrystalline zinc oxide and phase transformations of zinc hydroxides

Nanoscaled ZnO was synthesized by an electrochemical process using zinc or Al-alloyed zinc electrodes in an aqueous system with acetic acid as a conductive salt. Depending on the synthetical parameters, the precipitated precursor solids were found to consist of various compounds such as zincite, presumably δ-Zn(OH)₂, β₁-Zn(OH)₂, ε-Zn(OH)₂, Zn₅(CO₃)₂(OH)₆ and, in case an Al-alloyed electrode was used for the synthesis, Zn_0.71Al_0.29(OH)₂ (CO₃)_0.145·xH₂O. The intermediate solids served as precursors for the subsequent thermal treatment resulting in zincite powders with various morphologies. Depending on the processing conditions, zincite was formed between 100 and 260 °C with a mean crystallite size between 6 and 25 nm. Selected zincite powders were pressed to pellets, sintered at temperatures between 900 and 1,100 °C and characterized by measurements of the electrical bulk conductivities, yielding values up to 1.69 S cm⁻¹ in samples with 1.24 wt% Al. Comparison with samples prepared by precipitation methods showed that the latter had values of up to 44 S cm⁻¹.     

Novel molybdenum disulfide nanosheets–decorated polyaniline: Preparation,characterization and enhanced electrocatalytic activity for hydrogen evolution reaction

Novel molybdenum disulfide nanosheets–decorated polyaniline (MoS₂/PANI) was synthesized and investigated as an efficient catalyst for hydrogen evolution reaction (HER). Compared with MoS₂, MoS₂/PANI nanocomposites exhibited higher catalytic activity and lower Tafel slope for HER in H₂SO₄ solution. The amount of 19 wt% PANI for coupling with MoS₂ resulted in a high current density of 80 mA cm⁻² at 400 mV (vs. RHE). In addition, the optimal MoS₂/PANI nanocomposite showed impressive long-term stability even after 500 cycles. The enhanced catalytic activity of MoS₂/PANI nanocomposites was primarily ascribed to the effective electron transport channels of PANI and the increase of electrochemically accessible surface area in composite materials, which was advantageous to facilitate the charge transfer at catalyst/electrolyte interface.     

Comparison of Spectroscopic and Lasing Properties of Different Types of Sol-Gel Glass Matrices Containing Rh-6G

Rhodamine-6G (Rh-6G) is embedded in sol-gel glass samples which have been prepared by three different methods namely: 1) using HCl as catalyst and glycerol as Drying Control Chemical Additive (DCCA), 2) using HCl as catalyst at 60 °C and drying at room temperature and 3) using HCl as catalyst at 60 °C and heated at 600 °C for 3 h. Comparative studies of spectroscopic and lasing properties of the three types of Rh-6G containing samples were carried out with the lapse of time upto 8 months. Photostability of Rh-6G containing sol-gel samples is measured in terms of half life under Nitrogen laser pumping as number of pulses of N₂ laser necessary to reduce the dye laser intensity to 50% of the original value and value is 7500 pulses at 1.67 Hz rate. The best performance of Rh-6G, as far as its spectroscopic and lasing properties are concerned was found in third type of host matrices using HCl as catalyst at 60 °C and heated at 600 °C for 3 h.     

Polyaniline nanoparticles with controlled sizes using a cross-linked carboxymethyl chitin template

Polyaniline (PANI) nanoparticles were chemically synthesized in the presence of a cross-linked carboxymethyl chitin (CM-chitin) acting as a template. The reaction was performed under acidic conditions and the template was removed after the polymerization of aniline was completed. The morphology of the synthesized PANI was globular with a diameter in the nanometer range. The degree of cross-linking of the CM-chitin played an important role in determining the size of the obtained PANI nanoparticles, which decreased from approximately 392 to 160 nm with increase in concentration of the cross-linking agent, glutaraldehyde, from 0 to 9 μmol, respectively. At a higher glutaraldehyde concentration (18 μmol), an aggregated PANI network was observed due to the incomplete removal of the more highly cross-linked CM-chitin. Molecular characterization (including UV-Visible, FTIR, TGA, and XRD techniques) revealed that the structure of the synthesized PANI nanoparticles is identical to that of conventional PANI. A mechanism is proposed for the formation of PANI nanoparticles in the presence of the cross-linked CM-chitin template.     

Ultrasound irradiation effect on morphological and adsorptive properties of a nanoscale 3D Zn-coordination polymer and derived oxide

In this work, Zn-based coordination polymer [Zn₂(1,3-bdc)bzim₂]_n was successfully synthesized by the sonochemical method using a 13 mm probe-type ultrasound operating at 20 kHz and amplitudes of 30, 40 and 50% corresponding to an acoustic power of 5.5, 8.6, and 10.3 W, respectively. Additionally, a sample was prepared by the slow-diffusion method for comparison. The samples were characterized by FTIR, PXRD, SEM, and BET techniques. The influence of the time and sonication amplitude on the yield of the reaction, crystallite size, and morphology were also studied. It was found that the sonochemical method provided the desired product in 83.9% within 20 min of sonication using the highest level of sonication amplitude. Moreover, this approach resulted in regular, controlled morphology, smaller particles, and higher surface area of the Zn-sample and derived oxide, than the slow diffusion method. The samples prepared by different methodologies were tested for the adsorption of BTEX (benzene, toluene, ethylbenzene, and xylenes) components in six different systems, and the uptakes were quantified by ¹³C NMR spectroscopy. Both samples showed excellent adsorption of benzene, 119.8 mmol/g, and 88.1 mmol/g, for the coordination polymers prepared via the sonochemical and slow-diffusion methods, respectively, corresponding to 63.9%, and 46.9%. These results are in agreement with the non-polar surface of these samples.     

Electrochemical synthesis and performance of PANI electrode material for electrochemical capacitor

Polyaniline (PANI) electrode materials doped with sulfuric acid (H₂SO₄) were prepared by cyclic voltammetry (CV) method in different reaction conditions. The structure and morphology of PANI samples were characterized by Fourier transform infrared spectroscopy and scanning electron microscope. The electrochemical properties of PANI samples were studied by CV, galvanostatic charge/discharge, and electrochemical impedance spectroscopy tests. Additionally, the effects of reaction conditions including aniline concentration, voltammetry scan rate, and deposition time on the morphology and properties of PANI samples were investigated in detail. The results showed that the PANI synthesized under the optimal conditions of 0.2 mol?L^?1 aniline, scan rate 20 mV?s^?1, and deposition time 50 min is in the form of nanorods with a cross-linked network structure. It exhibits an outstanding capacitive performance with good cycle stability and high rate performance. Besides, the specific capacitance of PANI is as high as 757 F?g^?1.     

γ-MnO2/polyaniline composites: Preparation, characterization, and applications in microwave absorption

MnO₂/doped polyaniline (PANI) is prepared by an in situ polymerization method using γ-MnO₂ as the addition agent and hydrochloric acid as the doping agent. Products are characterized by FT-IR, UV-vis, XRD, and TEM. Conductivity, electromagnetic properties, and microwave absorption properties are first discussed on the basis of structural characterization. The as-prepared products of MnO₂/PANI are partially crystalline in nature and spherical in pattern with grain sizes of 50-70 nm. MnO₂ particles are successfully decorated with doped PANI. MnO₂/PANI displays moderate electric conduction, excellent dielectric losses, and microwave absorption capabilities. Compared to pure MnO₂, the dielectric and reflection loss properties of MnO₂/PANI composites exhibit significant improvements, with an effective absorption band at 5 GHz under −10 dB and maximum reflection loss of −21 dB at 13.56 GHz. Pure MnO₂ shows an effective absorption band of 3 GHz under −10 dB and a maximum reflection loss of −14.20 dB at 11.5 GHz. Thus, MnO₂/PANI composites are found to be a promising microwave absorption material.     

Simultaneous detection of dopamine and ascorbic acid in urine using the H-point standard addition method

A highly sensitive H-point standard addition method (HPSAM) was investigated for identification of dopamine and ascorbic acid in some synthetic and pharmaceutical samples in an aqueous medium at pH 9.2 using a universal buffer. The most suitable wavelengths for dopamine and ascorbic acid detection are 260:271 nm and 248:270 nm respectively. Recovery values are between 99.0–101 %. Also, the effect of most common interferents was studied. Detection ranges for dopamine and ascorbic acid are 2·10^–6–5·10^–5 M and 6·10^–6–3·10^–5 M respectively with an RSD range between 1.3 and 2.0 %. The method was used to determine both reagents in real and synthesized samples.     

Improved direct synthesis of TiO2 catalyst using sonication and its application for the desulfurization of thiophene

TiO₂ catalyst was synthesized in the presence of ultrasound (ultrasonic horn at 20 kHz frequency and 70% duty cycle) at different power (80 W to 120 W) and durations as well as surfactant concentration with an objective of establishing best conditions for achieving lowest particle size of the photocatalyst. Detailed characterization in terms of crystal phase, crystallinity, functional groups and morphology of the photocatalyst has been performed using SEM, XRD and FTIR analysis. It was demonstrated that sonication significantly reduced the particle size with high degree of sphericity and homogeneity as compared to conventionally synthesized TiO₂ with similar crystallinity in both cases. The catalytic performance was subsequently evaluated for the deep desulfurization of thiophene. Different desulfurization approaches including individual US (ultrasonic horn at 20 kHz frequency, 110 W power and 70% duty cycle) and UV irradiations, US/UV, US/UV/H₂O₂, US/UV/TiO₂ and US/UV/H₂O₂/TiO₂ were applied to evaluate the catalytic activity. The best approach was demonstrated as US/UV/H₂O₂/TiO₂ and also activity of catalyst synthesized using ultrasound was much better compared to conventionally synthesized catalyst. The studies related to different model solvents demonstrated lowest reactivity for toluene whereas n-hexane and n-octane resulted in complete desulfurization in 60 min and 50 min treatment respectively. The desulfurization followed pseudo first order reaction kinetics irrespective of the solvent used. Overall the work clearly demonstrated the efficacy of ultrasound in improving the catalyst synthesis as well as desulfurization of thiophene.     

Ac and Dc conductivities of polyaniline/poly vinyl formal blend films

The synthesis and characterization of polyaniline (PANI)/poly vinyl formal (PVF) blend films were carried out in this work. Polyaniline base was doped using dodecylbenzene sulfonic acid (DBSA). These blend films were characterized by UV–Visible, FTIR spectra and scanning electron microscopy (SEM) to investigate their optical, structural and morphological properties. It was found that the percolation threshold of these blends is 4.4 wt% of PANI. The dc and ac conductivities of these blend films have been measured at a temperature range from 300 to 100 K in the frequency range of 10 kHz to 1 MHz. The electrical conductivity of the blend films enhanced with the increase of polyaniline amount up to a value of 2.5 × 10⁻⁴ S cm⁻¹ at 65 wt% of polyaniline. The dc conductivity of the PANI/PVF blend films follows the three-dimension variable range hopping. Temperature variation of frequency exponents in this blend suggests that ac conduction is attributed to be correlated barrier hopping.     

Ultrasound microwave-assisted enzymatic production and characterisation of antioxidant peptides from sweet potato protein

Herein, we investigated the effects of ultrasound microwave (UM)-assisted hydrolysis using Alcalase (ALC), Flavourzyme (FLA), and their combination (ALC + FLA), on the production of sweet potato protein hydrolysates (SPPH). UM-assisted enzymatic hydrolysis significantly increased the degree of hydrolysis of SPPH compared with untreated (UN) samples. Fractions with differences in molecular weight (MW) of >10, 3–10, and < 3 kDa in SPPH from UM-assisted ALC, FLA, and ALC + FLA hydrolysis displayed higher antioxidant activities than those from UN samples. MW < 3 kDa fractions of SPPH from UM-assisted ALC and ALC + FLA hydrolysis treatments presented much stronger Fe²⁺-chelating activity (98.48% and 98.59%), ·OH scavenging activity (67.11% and 60.06%), and higher ORAC values (110.32 and 106.32 µg TE/mL), from which diverse peptides with potential antioxidant activities were obtained by semi-preparative HPLC and LC-MS/MS. All identified peptide sequences exhibited at least three potential antioxidant amino acids. Additionally, changes in peptide conformational structure and antioxidant amino acid composition were revealed by structure–activity relationship analysis. Thus, ultrasound microwave treatment has great potential in antioxidant peptides production.     

Preparation of poly(2-ethyl aniline)/kaolinite composite materials and investigation of their properties

Conductive poly(2-ethyl aniline) (PEAn)/kaolinite composite was prepared by chemical polymerization in aqueous HCl medium in the presence of kaolinite particles by using potassium chromate (K₂CrO₄) as oxidant. Effects of polymerization conditions, such as concentrations of oxidant and 2-ethyl aniline, polymerization time and temperature on PEAn content and conductivity of composite, were investigated. The prepared composite material, having the highest PEAn content and conductivity, was obtained in the polymerization carried out at 20 °C for 2 h with 0.2 M K₂CrO₄ and 0.2 M EAn. It was observed that the micro-hardness of prepared composites increased with the increase in the PEAn contents of composites. The highest micro-hardness value of 7.92 kg mm⁻² was reached at 24.6% PEAn content. Characterization of composites was carried out by FTIR spectroscopy, XRD, TGA and SEM techniques.