EDAX Methods Research Articles

Electroless Synthesis of Ni-P-ZrO<sub>2</sub> Nanocomposite to Analyse Corrosion

Electroless Synthesis of Nicle phosphate zirconium dioxide (EL NiP/-ZrO2) has been carried out with ZrO2 nanocomposite (50 to 160 nm and concentration 4 gpl) and randomly dispersed into an alkaline Ni-P electroless bath (pH 8.0). The deposited thickness of NiP/-ZrO2 nanocoatings resting on mild steels (MS) substrate (AISI 1040 grade) is carried out to evaluate the surface morphology and elemental composition. The SEM, EDAX and XRD methods elucidated clear difference between Ni-P along with NiP/-ZrO2 nanocomposite coatings. Moreover NiP/-ZrO2 nanocoatings contain uniform burly of ZrO2 nanoparticles like whitish globules. Further the as-coated Ni-P/-ZrO2 nanocoatings revealed mostly amorphous structures, while in heated coatings (temperatures 150, 350, and 550 °C with pure Ar) as temperature rises, the amorphous structure transformed leisurely to crystalline structure. The microhardness values in Vickers-unit of the developed nanocomposite coatings are determined and it is found that for a particular load with increase of temperature microhardness as well as corrosion resistancealso increases. Keywords: Electroless; Corrosion; Ni-P/-ZrO2; nanocoatings; Microhardness

Erythrocyte membrane-camouflaged mesoporous silica composite nanoparticles for loading and controlled release of the hepatoprotective agent silibinin: A-synthesis and physicochemical characterization.

Milk thistle has long been used in the treatment of liver and biliary disorders. In the present study, to make a long-acting delivery system for silibinin (SBN, a major active constituent of milk thistle seeds with antioxidant and hepatoprotective function), mesoporous silica composite nanoparticles (NC) were synthesized and coated with RBC membrane. A modified Stöber method was used for NC synthesis, which was then characterized using FE-SEM, DLS, TEM, FTIR, and EDAX techniques. A suitable lysis buffer was used to prepare RBC-ghost, and sonication was used to coat SBN-loaded NC (SBN-NC). The RBC-ghost coated SBN-NC (SBN-NC-RBCG) was evaluated by SDS-PAGE, Bradford, TEM, EDAX, and DLS methods. SBN release was then compared for the SBN-NC and SBN-NC-RBCG samples. the RBC membrane proteins were recovered from the coating of SBN-NC-RBCG, and SBN release was sustained over 24 h when compared with the SBN-NC. Overall, through prolonging circulation in the bloodstream and evading the immune system, the developed system can improve SBN bioavailability in liver inflammation and fibrosis conditions that need further research.

Superior antibacterial performance of surfactant-assisted ZnO nanoflakes produced via Co-precipitation method

Microbiological infections are one of the major problems that modern people encounter. Zinc oxide (ZnO) nanoflakes are excellent antimicrobial agents. The objective of this work was to synthesize ZnO nanoflakes with the assistance of surfactants and investigate the processes behind their antibacterial properties. The experiment involved the synthesis of ZnO using several surfactants, including cetyl trimethyl ammonium bromide (CTAB), polyvinyl pyrrolidone (PVP), and polyethylene glycol (PEG), and its analysis using XRD, FT-IR, SEM, EDAX, and BET methods. Both Gram-positive and Gram-negative bacterial strains were used in these investigations. ZnO nanoflakes aided by CTAB (R-2) had the most promising action against the tested bacterial strains like Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, and Bacillus cereus. These ZnO nanoflakes with CTAB assistance consistently had greater inhibitory zones than other samples. The R-2 sample’s enhanced surface area and particle size, which result in improved antibacterial activity. The investigation’s outcomes show that the produced nanoflakes have the potential to be useful in antibacterial and other medicinal applications.

Применение сорбентов на основе природного цеолита и шамотной глины для извлечения ионов натрия и калия из соленой воды: предварительное исследование

In this work, sorbents based on natural zeolite (Z) and chamotte clay (ChC) treated with NaCl and HNO3 solutions were obtained to extract Na+ and K+ ions from saline water. The physicochemical characteristics of the obtained sorbents were studied by SEM, EDAX, and BET methods. It was found that successive treatment with NaCl and HNO3 solutions has a positive effect on the sorption properties of the studied materials. The maximum increase in the specific surface area from 4.5 m2/g to 39.3 m2/g is observed for acid-treated Z, and the specific surface area of ChC also increases almost 2-fold from 8.4 m2/g to 15.3 m2/g. Na+ and K+ ions are extracted from water due to ion exchange with Z and ChC cations. As a result of determining the cation exchange capacity (CEC) of the studied sorbents, it was found that treatment with a NaCl solution improves the ion exchange properties of the sorbent and leads to the formation of a “homoionic” form of aluminosilicates. Due to that the sorbents more easily enter ion exchange reactions. The authors established the sorption activity of the obtained materials based on natural Z and ChC with respect to Na+ and K+ cations. The maximum recovery rate is 28.45% for Na+ ions with the ChC-Na-H sorbent and 76.28% for K+ ions with the ChC-Na sorbent. Among Z-based sorbents, the most effective forms are Z-Na-H (15.44% Na+ recovery) and Z-Na (60.47% K+ recovery).

Electrical, Optical, and Structural Stability Over Ten Years for Sb Based III-V Semiconducting Bulk Grown by VDS

III-V semiconductors have an advantage of not being degraded with time at room temperature, among non-silica semiconductors. This stability property is useful at the places where frequent device replacement is not possible. Determination of stability parameters are needed to be studied prior to their application as a junction substrate. The Vertical Directional Solidification (VDS) technique is employed for the growth of bulk crystals, without the seed, without contact to the ampoule wall, without coating, and without external pressure. The antimony based III-V substrates have been studied before and after an interval of ten years for any possible degradation in quality that may affect their applicability. XRF, EDAX, FTIR, XRD, Raman, and resistivity measurements methods were used to measure compositional optical, structural, and electrical consistency over the time. These bulk crystals revealed a high degree of stability within experimental limits for more than ten years, including intact crystalline structure, no formation of oxides, compositional stability, and no significant variation in band gap and resistivity, and hence still appropriate to be applied in semiconductor junction fabrications.

Bi2Te3 nanotubes and nanoplates for thermoelectric applications: Effect of surfactant on crystal growth

Bi2Te3 is a benchmark thermoelectric material suitable for near room temperature device applications. It wields unique properties at nanometer level from its bulk material. In this study, Bi2Te3 nanostructures with diverse morphology have been synthesized through a single pot, scalable hydrothermal method by using different surfactants. The structural and morphological properties of the nanostructures are found to be varied with addition of surfactant. Bi2Te3 nanostructures were characterized by using XRD, FESEM, EDAX, Raman studies, HRTEM and SAED methods. Bi2Te3 nanoplates were obtained with polyvinyl pyrrolidone (PVP) and Bi2Te3 Nanotubes with varying cross sections were found to be formed with disodium ethylene diamene terra acetic acid (EDTA) as surfactants. A growth mechanism is proposed for the obtained crystals, by analysing the experimental results.

Synthesis, Optimization, and Characterization of Ecofriendly Production of Gold Nanoparticles Using Lemon Peel Extract.

This study examines the importance of utilizing green synthesis using lemon peel for gold nanoparticles over other chemicals since it is environmentally friendly, available, and cheap. Several parameters were optimized to ensure the extraction of the GNPs concentration of lemon peels using HAuCl4 and lemon peel extract having a ratio of 2 : 1. For the optimum result, the ratio used was 2 : 1. The gold nanoparticles fabrication happened in 10 minutes. The initial observation was the color change of the solution. The UV-visibility spectroscopic studies are performed to confirm the result. The experiments are done concurrently to ensure the solution is mixed on the proper ratio. The GNP is also characterized by the different techniques in their sizes and electronic transmission microscopy, essential in extracting gold nanoparticles. Other elements of the composition are removed by the EDAX methods, the FTIR method, and the TEM methods, all of which reveal the real reason behind the required extraction capacity. Most gold nanoparticles show a maximum absorption rate at the peak of 535 to 579 nm. The result obtained from the TEM and the SEM analysis revealed that the grain size is analogized to the average size of 6.67 nm. With a simple synthesis of the price, some processes show that the medically available nanoparticles are necessary. The used method in this paper to fabricate GNPs is cheap, easy, fast, and sustainable and it can be done with ease in any laboratory.

Biosynthesis of iron oxide nanoparticles from dates, characterization, and investigation of anticarcinogenic and antimicrobial properties

Nanomaterial synthesis using natural biological systems, especially plant-based green synthesis has evinced great excitement and interest. In this study, iron oxide nanomaterials were synthesized from three different varieties of date palms obtained from Srivilliputhur, Tamil Nadu, India. The extract of date palms reduced ferric chloride in solution and facilitated the formation of iron oxide nanomaterials. Phytochemical studies of the extracts obtained from all three varieties of date palms indicated the presence of phenols. The synthesized nanomaterials were characterized by UV-VIS spectroscopy, SEM, EDAX, XRD and FTIR methods. The ability of the synthesized nanomaterials to inhibit human microbial pathogens proliferation was tested in Staphylococcus sp. and Bacillus sp. by turbidity method and recorded the maximum antimicrobial property against Bacillus sp. in the iron nanomaterial synthesized from Sukhri date palm. The cytotoxic potential of the iron oxide nanomaterials was assessed against two human cancer cell lines (A-549 and MDA-MB-231) by MTT assay. The substantial cytotoxicity response was detected from the iron oxide nanomaterials made from Sukhri date palm.

Production, Characterization and Application of Oxide Nanotubes on Ti-6Al-7Nb Alloy as a Potential Drug Carrier.

This work concerns the development of a method of functionalization of the surface of the biomedical Ti–6Al–7Nb alloy by producing oxide nanotubes (ONTs) with drug-eluting properties. Shaping of the morphology, microstructure, and thickness of the oxide layer was carried out by anodization in an aqueous solution of 1 M ethylene glycol with the addition of 0.2 M NH4F in the voltage range 5–100 V for 15–60 min at room temperature. The characterization of the physicochemical properties of the obtained ONTs was performed using SEM, XPS, and EDAX methods. ONTs have been shown to be composed mainly of TiO2, Al2O3, and Nb2O5. Single-walled ONTs with the largest specific surface area of 600 cm2 cm−2 can be obtained by anodization at 50 V for 60 min. The mechanism of ONT formation on the Ti–6Al–7Nb alloy was studied in detail. Gentamicin sulfate loaded into ONTs was studied using FTIR, TG, DTA, and DTG methods. Drug release kinetics was determined by UV–Vis spectrophotometry. The obtained ONTs can be proposed for use in modern implantology as carriers for drugs delivered locally in inflammatory conditions.

Hydroxyapatite surface-functionalized monolithic column for selective in-tube solid phase microextraction of zoleronic acid and risedronic acid

To date, hydroxyapatite (HAP) based monoliths were mainly fabricated by directly doping of HAP, which suffered from less effective coverage of HAP. Herein, a HAP surface-functionalized monolithic column (HAP@PDA@UF) has been prepared by in-situ biomineralization and applied as sorbent for selective in-tube solid phase microextraction of zoleronic acid and risedronic acid. A polydopamine coating was first generated on the surface of the parent urea-formaldehyde resin monolith; and then HAP microcrystals were further grew on the polydopamine coating to achieve this preparation. SEM, EDAX, FTIR, XPS and mercury intrusion method were utilized for the characterization of the HAP@PDA@UF monolith, and provided evidences of this successful preparation. The selective extraction mechanism of the HAP@PDA@UF monolith was investigated by the optimization of methanol percentage in the sampling solution, phosphate concentration in the eluent. Other crucial factors, including sampling and elution flow rate, and collection time span, were also optimized for the desired SPME performance. Under the optimal conditions, the proposed method showed low LODs of 0.1 μg/mL, satisfactory recoveries of 79.6%-92.5% with RSDs less than 2.7%, and good reproducibility with RSD less than 6.9%, which demonstrated the excellent application of the HAP@PDA@UF monolith, and its potential as a promising selective sorbent for bisphosphonates.

Analysis of the physicochemical and sorption characteristics of composites based on zeolite and chamotte clay

Clays and aluminosilicate materials are known as effective sorbents for purification of wastewater from various types of contaminants. Some properties and sorption activity of materials based on the zeolite of Shankanai deposit and Chamotte clay towards Cd2+ ions were analyzed in the present work. The structural characteristics of the studied objects, their qualitative and quantitative composition were determined by the SEM and EDAX methods. It was found that maximum adsorption capacity (qe) of the initial zeolite for extraction Cd2+ ions is (7.3±0.11) mg/g, while for Chamotte clay this value equals to (5.3±0.12) mg/g. After modification with polyvinylpyrrolidone, qe increased to (10.1±0.08) mg/g for zeolite, and (8.5±0.15) mg/g for Chamotte clay. Developed specific surface of the composite material (sorbent) and complexation with the active centres of thepolymer couldbe a resultof Cd2+ ions binding.

Synthesis and Characterization of Anti-Scratch and Anti-Corrosion Hybrid Nanocomposite Coatings Based on Sol-Gel Process

Hybrid nanocomposite coatings containing SiO2, TiO2, ZnO, and ZrO2 particles were synthesized based on sol-gel precursors, including tetraethoxysilane (TEOS), 3glycidoxypropyl trimethoxysilane (GPTMS), tetra(n-butylorthotitanate) (TBT), zinc acetate dihydrate, and zirconium chloride (IV). The nanocomposites were characterized using FTIR, SEM, DLS, and EDAX methods. Results indicated that the size of the inorganic particles was in the range of nanometer (283.3, 163.5, 99.2, and 2.5 nm for ZrO2, SiO2, ZnO, and TiO2, respectively) with a very uniform distribution and dispersion. Hybrid nanocomposite coatings containing different amounts of nanozirconia were prepared on a 30-μm thick steel sheet for the subsequent scratch test. The highest scratch resistance of 3950 g was associated with the coating containing 0.0015 g nanozirconia. The electrochemical properties of the composite coating were investigated using potentiodynamic polarization (TOEFL) and electrochemical impedance spectroscopy (EIS). The results showed that the corrosion resistance of the steel sheet coated with zirconia composite is much better than that without the coating. The ZrO2 composite coating also showed better corrosion inhibition and improving surface resistance against mechanically induced scratches, without any trade-off in transparency.

Chromium substituted nickel ferrites (NiFe2−xCrxO4, x = 0.0, 0.1, 0.2, 0.3, and 0.4) magnetically recoverable reusable heterogeneous nano catalysts

Nano ferrite particles were synthesized by oxalate precursor method, characterized by TGA/DTA analysis to know the pattern of decomposition, an elemental stoichiometry confirmed by EDAX method. The X-ray diffraction (XRD) and Infra-Red patterns were used to determine structural parameters, indicate the formation of single-phase cubic spinal structure. The average crystalline size was calculated from FWHM of most intensive pick 311, also confirmed from TEM analysis observe in the range of 29–34 nm. The structural parameters like lattice constant, X-ray density, bulk density and porosity increases with Cr3+ ion concentration. The magnetic parameters like saturation magnetizations and magnetic moments shown decreasing tendency. Bis-(4-hydroxycoumarin) methane derivatives successfully synthesized from 4 hydroxycoumarin 1) aromatic aldehydes 2, and using 20 mol % NiFe2−xCrxO4 nanoparticles as magnetically recoverable and reusable catalyst.

Bi-Functional Pd/Y-Zeolite Reforming Nanocatalyst Engineered Employing Polyvinylpyrrolidone and 2-(3,4-epoxycyclohexyl)Ethyltrimethoxysilane

This article reports novel engineering route of bi-functional Pd/Y-zeolite reforming nanocatalyst. Palladium nanostructures, synthesized adopting 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane as the reducing species and polyvinylpyrrolidone as the capping moiety, have been impregnated on Y-zeolite catalyst support for the purpose of imparting enhanced catalytic efficiency. Various characterization techniques have been performed such as UV/Visible spectroscopy, TEM, EDAX, SEM and BET method.

Voltammetric food analytical sensor for determining vanillin based on amplified NiFe2O4 nanoparticle/ionic liquid sensor

We describe a powerful type of vanillin electrochemical sensor based on a carbon paste electrode (CPE) modified with NiFe2O4 nanoparticle and 1-hexyl-3-methylimidazolium chloride (1H3MCl). The NiFe2O4 nanoparticle was synthesized by co-precipitation strategy and characterized by FESEM, XRD, and EDAX methods. The results revealed a spherical shape NiFe2O4 nanoparticle with diameter ~ 22 nm. The oxidation peak of vanillin was recorded at potentials + 690 and + 650 mV at the surface of CPE and NiFe2O4/1H3MCl/CPE by cyclic voltammetric method, respectively. The NiFe2O4/1H3MCl/CPE exhibited high electro-catalytic ability toward vanillin electro-oxidation and indicated two separated oxidation signals at potentials 640 and 1050 mV for vanillin and tryptophan by differential pulse voltammetric method. The sensitivity 0.1011 and 0.5058 μA µM−1 as well as the detection limits 1.0 nM and 0.09 µM were observed for determination of vanillin and tryptophan at the surface of NiFe2O4/1H3MCl/CPE, respectively. The NiFe2O4/1H3MCl/CPE was used as a food analytical sensor for determining vanillin and tryptophan in food samples such as coffee milk, chocolate, and biscuit.

Corrosion Resistance of Electroless Ni-P-SiC/ Ni-P-TiO2-ZrO2 Nano-Coatings in Paper Mill Bleach Plant

Abstract In present investigation, electroless Ni-P-SiC/Ni-P-TiO2-ZrO2 nano-composite platings have been deposited upon mild steel substrate (AISI 1040). A homogeneous and consistent allocation of SiC, TiO2 and ZrO2 nano-particles into EL Ni-P matrix is recognized in as plated and heated (400°C) coupons respectively through SEM and EDAX methods. The investigated coupons exhibited resistance against corrosion in order as: 254SMO > SS2205 > Ni-P-TiO2-ZrO2 as-plated > Ni-P-TiO2-ZrO2 heat treated > Ni-P-SiC as-plated > Ni-P-SiC heat treated > SS316L. The corrosion resistance seems too dependent upon Cr, Mo and N content and hence correlate well with the PRE number of the respective alloys. The conventional materials of construction SS 316L are not suitable for both C and D washers. Avesta 254SMO shows immunity to attack in these environments. On the basis of corrosion resistance, mechanical properties and cost comparison, Avesta 254 SMO seems acceptable material for gaseous phase of C and D washers while duplex stainless steel 2205 and Ni-P-SiC/Ni-P-TiO2-ZrO2 as-plated and heated coatings seems acceptable for the other application in these washers.

Adsorption of lead (II) ions from water solutions with natural zeolite and chamotte clay

Natural zeolites and clays are known as effective and low-cost materials to use as adsorbents of different pollutants. The adsorption behavior of the Pb2+ ions adsorption on Kazakhstani natural zeolite and Ukrainian Chamotte clay has been studied in this work. The samples are characterized by SEM, EDAX, and XRD methods. The maximum uptake of lead ions (qmax) was determined as 14 mg/g for zeolite and 11 mg/g for clay. Langmuir and Freundlich isotherm models were used to describe the adsorption mechanism. It was observed that Langmuir isotherm model best describes the adsorption of Pb2+ on natural zeolite and clay. The separation factors (KR) were calculated from the Langmuir isotherm.

Simultaneous determination of cholesterol, ascorbic acid and uric acid as three essential biological compounds at a carbon paste electrode modified with copper oxide decorated reduced graphene oxide nanocomposite and ionic liquid

In this article, we report the simultaneous determination cholesterol (CL), ascorbic (AA) acid and uric acid (UA) at a carbon paste electrode (CPE) modified with copper oxide decorated reduced graphene (CuO-rGR), with 1-methyl-3-octylimidazolium tetrafluoroborate (1M3OIDTFB) as a binder. The electrode, CuO-rGR/1M3OIDTFB/CPE, showed remarkable sensitivities towards the determination of the analytes, and well defined and clearly separated oxidation peaks were obtained during their simultaneous analysis in a buffer solution at pH 7.4. The differences observed between their peaks potentials are as follows: 430 mV (between CL and AA), 270 mV (between AA and UA) and 700 mV (between CL and UA). The morphologies and structure properties of the CuO-rGR were investigated by FESEMD and EDAX methods. The CuO-rGR/1M3OIDTFB/CPE displayed linear response in the concentration ranges 0.04–300.0 μM, 0.04–240.0 μM and 0.4–400.0 μM for CL, AA and UA with the detection limits 9.0 nM, 9.0 nM and 0.08 μM, respectively. The CuO-rGR/1M3OIDTFB/CPE displayed high performance for the determination of CL, AA and UA in real samples.

Nanocrystalline Nickel Electrodeposition on Carbon Steel Using Eco-Friendly Aqueous Ananas comosus Juice

The present study aims to investigate the effect of Ananas comosus juice on nickel electrodeposition on mild steel. The effect of this additive on electrodeposition behaviour, bath composition, surface morphology and corrosion performance of the nickel electrodeposited mild steel were investigated. The bath constitutents are optimized through Hull cell experiments. To investigate the nature of the deposits, FT-IR, scanning electron microscopy, EDAX, XRD and electrochemical methods are applied. Current efficiency and polarization studies were carried out. The results confirmed the influence of Ananas comosus juice on nickel electrodeposition.

Synergistic effect of branched polymer/nano silica on the microstructures of cement paste and their rheological behaviors

Various branched polymers as superplasticizer containing nano silica were synthesized via in situ solution polymerization. The molecular structures of the branched polymers were characterized using 1HNMR and GPC methods. The interactions between the prepared polymers and nano silica were also investigated using TGA methods. After the neutralization and ultra sonication of the resulting nano suspensions possessing different amounts of nano particles, the size of the aggregated nano silica and branched polymers and their dispersion behavior were studied using DLS and SEM methods. The SEM results showed that the cement paste microstructure and morphology were different in the presence of the branched polymers and nano particles. The branched polymers influenced the cement microstructure and morphology of the hydrated calcium silicate crystals. In addition, the distribution of nano silica particles examined using EDAX method. The rheological properties of the cement pastes were examined at different water to cement ratios and pHs. The viscosity of the cement suspension was different depending on the concentration of the branched polymers as the superplasticizer and nano silica state. The branched polymer was desorbed from nano silica surface and then was adsorbed on the cement particle leading to decreasing the cement suspension viscosity and improving dispersion behavior of the cement particles.