Thermal and sensitivity analysis of nano aluminium powder for firework application

The performance of the fireworks is governed by the sound level it produces. As per Govt. of India notification, crackers sound level should not exceed 125 dB (AI) or 145 dB(C) pk. In this study, nAl powder was synthesised at different particle sizes of 113, 187 and 218 nm as a fuel. These powders are well mixed with the oxidizer (KNO₃) and the igniter (S), and the cake bomb was manufactured with various compositions and checked for their performance. The thermal analysis was performed by DSC and DTA, and the impact sensitivity was analysed for all compositions. The nano-sized chemicals showed high thermal energy content and high sensitivity for various compositions. Further it is observed that the nAl chemical for producing the optimum sound level in the cake bomb has been reduced to 62.5% when compared with μm powder.     

Thermal and spectral behavior of (Y,Eu)VO4 powder

Thermal analysis of Y_xEu_1?xVO₄ powder (used as “phosphor” coating for a high pressure mercury lamp) was done under a non-isothermal linear regime, both in a dynamic air regime and in a nitrogen atmosphere. The heating in air atmosphere gave on TG curve small rate of mass increase due to oxygenation and two endothermic effects are observed on DTA and DSC curves. By contrary, in nitrogen atmosphere a continuous stepped mass loss of powder (around 0.65 %), is recorded in the range of temperatures from room temperatures to 1,200 °C, and only one endothermic effect, to eliminate the gases accumulated on the crystallite surface. The powder was heated for 3 h in a Nabertherm furnace at 350, 800, and 1,100 °C using quite similar rate for heating program followed by a furnace cooling to room temperature. XRD and FTIR analyses showed the sample purification by thermal treatment and a very small increase of nanocrystallite sizes. The time evolution of the optical emission spectra in the range from 186.2 to 877.47 nm were recorded for different lamp powers in two different situations: with the outer bulb coated with Y_xEu_1?xVO₄ type “phosphor”, and without it. We observed that UV-Hg lines are absorbed by Y_xEu_1?xVO₄ type “phosphor” with different percents (100 % for 253.73 nm, 95 % for 312.65 nm, and 33 % for 365.12 nm) but the heating of the powder do not influence the UV-absorption properties of the powder.     

An H2O2 Biosensor Based on Immobilization of Horseradish Peroxidase Labeled Nano‐Au in Silica Sol‐Gel/Alginate Composite Film

Abstract

A novel approach to assemble an H₂O₂ amperometric biosensor was introduced. The biosensor was constructed by entrapping horseradish peroxidase (HRP) labeled nano‐scaled particulate gold (nano‐Au) (HRP‐nano‐Au electrostatic composite) in a new silica sol‐gel/alginate hybrid film using glassy carbon electrode as based electrode. This suggested strategy fully merged the merits of sol‐gel derived inorganic‐organic composite film and the nano‐Au intermediator. The silica sol‐gel/alginate hybrid material can improve the properties of conventional sol‐gel material and effectively prevent cracking of film. The entrapment of HRP in the form of HRP‐nano‐Au can not only factually prevent the leaking of enzyme out of the film but also provide a favorable microenvironment for HRP. With hydroquinone as an electron mediator, the proposed HRP electrode exhibited good catalytic activity for the reduction of H₂O₂. The parameters affecting both the qualities of sol‐gel/alginate hybrid film and the biosensor response were optimized. The biosensor exhibited high sensitivity of 0.40 Al mol^?1 cm^?2 for H₂O₂ over a wide linear range of concentration from 1.22×10^?5 to 1.46×10^?3 mol L^?1, rapid response of <5 s and a detection limit of 0.61×10^?6 mol L^?1. The enzyme electrode has remarkable stability and retained 86% of its initial activity after 45 days of storage in 0.1 mol L^?1 Tris‐HCl buffer solutions at pH 7.     

Nano oxides incorporated sulfonated poly(ether ether ketone) membranes with improved selectivity and stability for vanadium redox flow battery

Three kinds of sulfonated poly(ether ether ketone) (SPEEK)/nano oxide (Al₂O₃, SiO₂, and TiO₂) composite membranes are fabricated for vanadium redox flow battery (VRFB) application. The composite membranes with 5 wt% of Al₂O₃, SiO₂, and TiO₂ (S/A-5 %, S/S-5 %, and S/T-5 %) exhibit excellent cell performance in VRFB. Incorporation of nano oxides (Al₂O₃, SiO₂, and TiO₂) in SPEEK membrane improves in aspect of thermal, mechanical, and chemical stabilities due to the hydrogen bonds’ interaction between SPEEK matrix and nano oxides. The energy efficiencies (EEs) of composite membranes are higher than that of Nafion 117 membrane, owing to the good balance between proton conductivity and vanadium ion permeability. The discharge–capacity retentions of composite membranes also overwhelm that of Nafion 117 membrane after 200 cycles, indicating their good stability in VRFB system. These low-cost SPEEK/nano oxide composite membranes exhibit great potential for the application in VRFB.     

Effervescence-assisted dispersive liquid-liquid microextraction based on deep eutectic solvent for preconcentration and FAAS determination of copper in aqueous samples

A new effervescence-assisted dispersive liquid-liquid microextraction, EA-DLLME, technique was developed for preconcentration and flame atomic absorption spectrometric determination of copper in aqueous samples. Effervescence assistance and DES combination for metal ion extraction was used for the first time. In the presented study, six different effervescence powders were examined to achieve maximum extraction efficiency. In addition, 1,5 diphenyl carbazide was used as complexing agent and DES prepared by mixing choline chloride and phenol was used as extraction solvent. The effect of several parameters such as pH, concentration of complexing agent, composition and volume of DES, amount of THF, composition and amount of effervescent agent were examined. Performed experiments showed that optimum pH was 6.0, the best effervesce powder composition was NaH₂PO₄:Na₂CO₃ with 2 × 10^?3:1 × 10^?3 molar ratio and the amount of effervesce powder was 0.4 g. Under optimum conditions enhancement factor, limit of detection and limit of quantification were calculated as 78, 2.9 and 9.7 μg L^?1, respectively. In addition, to prove precision of the method intra-day relative standard deviations were calculated for 10 and 50 μg L^?1 Cu²⁺ concentrations and found as 2.1% and 1.3%, respectively. The proposed method showed good linearity within the range of 10.0–100 μg L^?1. Finally, proposed method was successfully applied to determination of copper traces in aqueous samples.     

Antimony phosphate nanoribbons: sorbents for uptake of uranyl ion

Antimony phosphate nanoribbons was synthesized and characterized using different techniques. Studies showed that the synthesized antimony phosphate possessed highly crystalline monoclinic SbPO₄ phase with an average crystallite size of 14 nm. TEM studies showed that antimony phosphate was present both as nano ribbons and nano particles. It is observed that the nano ribbons have length in the range of 500–700 nm and width around 100–200 nm whereas the nanoparticles size in the range of 1–5 nm. The synthesized nano phosphate was studied for its efficiency as sorbent for uptake of various metal ions including uranyl ion. The results indicated that a clean separation of uranyl ion from its various binary mixtures could be achieved at optimized pH of 4.5 and equilibration period of 1 h using 0.1 g of the sorbent.     

A highly sensitive nonenzymatic glucose sensor based on nickel oxide–carbon nanotube hybrid nanobelts

In this study, we demonstrated a highly sensitive electrochemical sensor for the determination of glucose in alkaline aqueous solution by using nickel oxide single-walled carbon nanotube hybrid nanobelts (NiO–SWCNTs) modified glassy carbon electrode (GCE). The hybrid nanobelts were prepared by the deposition of SWCNTs onto the Ni(SO₄)_0.3(OH)_1.4 nanobelt surface, followed by heat treatment at different temperatures ranging from 400 °C to 600 °C. The NiO–SWCNTs hybrid nanobelts modified electrode prepared at 500 °C displays enhanced electrocatalytic activity towards glucose oxidation, revealing a synergistic effect between the NiO and the deposited SWCNTs. The as-fabricated nonenzymatic glucose sensor exhibits excellent glucose sensitivity (2,980 μA cm^?2 mM^?1), lower detection limit (0.056 μM, signal/noise [S/N] ratio?=?3), and wider linear range (0.5–1,300 μM). Moreover, the sensor has been successfully used for the assay of glucose in serum samples with good recovery, ranging from 96.4 % to 102.4 %.     

Phase diagram study of CaBr2–CaHBr system

A study of binary, CaBr₂–CaHBr system was carried out by differential thermal analysis (DTA), covering the composition range from 100 % CaBr₂ to 100 % CaHBr between room temperature and 800 °C. From DTA results, the contour of solidus and liquidus temperatures with composition is plotted and the phase diagram of CaBr₂–CaHBr system is constructed. The system shows an eutectic reaction at 576 °C and the eutectic composition is 79.6 mol% CaBr₂. Co-existing phases in different phase fields are characterized by X-ray diffraction analysis.     

Decomposition of perfluoropolyether lubricants

Decomposition has been studied in the chemistry of perfluoropolyethers (PFPE), thus far no molecular structure information is reported. TG-MS is a tool to follow the off gassing of decomposition for clues. We selected two PFPEs that have different properties: Krytox® XHT-1000 and Fomblin Z60 heating to normal decomposition and catalytic decomposition in the presence of alumina powder. Comparing the decomposition fragment intensities, the molecular structure of the branched Krytox® XHT-1000 oil is more stable than the blocky Fomblin Z60. We see aluminum-containing fluorine fragments in the rapid decomposition of oils in contact with alumina powder. It has been suggested the formation of Al(O_6?n F _n ), where n = 1, 2, and 3, in which the fluorine atoms are selectively associated with aluminum atom. The major decomposition products are small and large fragments of fluorocarbons and perfluoroalkoxy. In the absence of alumina powder, Krytox XHT-1000 shows only a loss of 13 mass/% after several hours at 330 °C, whereas in the presence of 1 mass/% alumina powder the oil has rapidly decomposed to 67 mass/% of its original mass within 15 min. Fomblin Z60, a product might not be designed for high temperature, exposing to the same conditions at 330 °C for several hours and shows a loss of 98 mass/% alone, but in the presence of 1 mass/% alumina powder shows a loss of 98 mass/% in 3.6 min. When 3 mass/% of two new developmental additives were added to the both oils, the catalytic decomposition in the presence of 1 mass/% alumina powder was significantly reduced in Krytox® XHT-1000, showing only a loss of 23 mass/% in 4 h, but nearly all weight for Z60 in 60 min. In the oil grades that contain the new additives, we see the fragments of Al–O–S, and F–Al–O–S. The sulfur-containing compound has been reported ionically bonded to oxide in a tripod configuration of alumina surface, which shields the formation of Al–F.     

Identification of gamma-irradiated Chinese herbs by thermoluminescence analysis

The feasibility of thermoluminescence (TL) to differentiate irradiated Chinese medicinal herbs from non-irradiated was investigated. Thirty different dried Chinese herbs were tested, including root, flower, ramulus, rhizome, cortex, and whole plant samples. Irradiation of Chinese herbs was associated with strong TL peaks at ~150–250 °C, while TL curves of non-irradiated herbs had very low intensities above 250 °C, which was also confirmed by the TL ratio (non-irradiated, TL₁/TL₂ < 0.1). The ability to determine the irradiation dose by the TL method was influenced by the amount and types of minerals in the samples. All levels of irradiation doses could be detected when between 0.1 and 1.0 kGy, except for three herbs at 0.1 kGy dose. Different blends with small quantities (0.1–10 %) of irradiated herbs were also tested in this study. Samples with powder mixtures containing 1 % irradiated components could be differentiated (TL₁/TL₂ > 0.1) except for sterculia lychnophora, semen cassia, flos inulae, and anemone root. TL ratios of some herbs indicated irradiation (TL₁/TL₂ > 0.1) even if the irradiated components were as low as 0.1 %. Thus we demonstrated that TL analysis had excellent sensitivity and reliability for the identification of irradiated Chinese herbs.     

Electrocatalysis of Puerarin on a Nano-CeO2/MWCNTs Composite Modified Electrode and Its Determination in Pharmaceutical Preparations

A good route for the fabrication of CeO₂ nanoparticles (nano‐CeO₂)/multi‐walled carbon nanotubes (MWCNTs) modified glassy carbon electrodes (GCE) was proposed. MWCNTs are used to immobilize nano‐CeO₂. What′s more, with the addition of the MWCNTs, the agglomeration level of CeO₂ nanoparticles can be reduced, the extremely large surface area can be obtained and the electron transfer rate can be increased. The morphological characterization of nano‐CeO₂/MWCNTs was examined by scanning electron microscopy (SEM). The performances of the nano‐CeO₂/MWCNTs/GCE were characterized with cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and typical amperometric response (i‐t). The potential utility of the constructed electrodes was demonstrated by applying them to the analytical determination of puerarin concentration. The catalytic oxidation of puerarin has a better result on nano‐CeO₂/MWCNTs/GCE because of the synergistic effect of nano‐CeO₂ and MWCNTs. An optimized limit of detection of 8.0×10^?9 mol/L was obtained at a signal‐to‐noise ratio of 3 and with a fast response time (within 3 s). Additionally, the nano‐CeO₂/MWCNTs/GCE exhibited a wide linear range from 0.04 to 6.0 μmol/L and high sensitivity.     

Thermal stability of nanocrystalline ε-Fe2O3

Thermal behavior of highly crystalline ε-Fe₂O₃ nanoparticles of different apparent crystallite sizes was characterized using thermogravimetry, differential thermal analysis, and analysis of evolved gas by mass spectrometry. Phase composition of the samples was monitored ex situ by X-ray powder diffraction. The results show that the thermal stability of this metastable iron oxide polymorph decreases with increasing particle size. For the particle diameter of 19(2) nm, the transformation temperature was equal to 794(5) °C, while for 28(2) nm only 755(10) °C. Surface of the nanoparticles contained adsorbed water and carbon dioxide. Elimination of these species proceeds in two steps. Water is removed at temperatures below 200 °C and CO₂ in the temperature range between 200 and 450 °C.     

TL characteristics of Ce3+-doped NaLi2PO4 TLD phosphor

Ce³⁺-doped NaLi₂PO₄ orthophosphate (with different impurity concentrations, i.e., 0.01–0.3 mol%) was prepared by a solid state reaction method. Formation of the material was confirmed using powder X-ray diffraction analysis. TL intensity was found to be the highest for the material having impurity concentration 0.2 mol% after annealing it at around 600 K for 1 h and subsequently quenching to room temperature. A typical glow curve consists of three peaks at around 454, 493 and 570 K (dosimetry peak). Good sensitivity (~8 times more than that of TLD-100), low fading (~15 % in 2 months), low-Z material (Z _eff ≈ 10.8), very wide dose response (i.e., 0.1 Gy–1.0 kGy of γ rays) make the material a ‘good’ thermoluminescent dosimeter (TLD) phosphor suitable for personnel, medical and environmental dosimetry of high-energy radiation using TL. It could also be used during cancer therapy and sterilization of food where high doses are needed to be monitored.     

Influence of MoSi2 content in suspension on the phase, microstructure and properties of hydrothermal electrophoretic deposited SiC n �CMoSi2 coating for SiC pre-coated C/C composites

To protect carbon/carbon (C/C) composites from oxidation at high temperature, a nano SiC?CMoSi₂ (SiC _n ?CMoSi₂) coating on SiC pre-coated C/C composites was prepared by hydrothermal electrophoretic deposition. The phase composition, surface and cross-section microstructures of the prepared SiC _n ?CMoSi₂ coating deposited with different MoSi₂/SiC _n mass ratio were characterized by X-ray diffraction (XRD), energy-dispersive spectroscopy (EDS) and scanning electron microscopy (SEM). The influence of MoSi₂ content in the hydrothermal electrophoretic deposition suspension on the phase composition, microstructure and high-temperature oxidation resistance of the multi-layer coatings were investigated. Results showed that the content of MoSi₂ phase in the prepared coating increases with the increase of MoSi₂ content in the suspension. The density and oxidation resistance of the SiC_n-MoSi₂ coating improve with the increase of MoSi₂ mass content from 20 to 60 wt% in the deposition suspension. However, micro-cracks and micro-holes in the coating are found when deposited with 80 wt% MoSi₂, and a decrease in oxidation resistance was also detected. The multi-layer coatings deposited with suspension of 60 wt% MoSi₂ exhibited the best anti-oxidation ability, which can effectively protect C/C composites from oxidation in air at 1,873 K for 90 h with weight loss of 2.08%.     

Copolymeric nano/microgels of N-isopropylacrylamide and carboxyalkyl methacrylamides: Effect of methylene chains and the ionization state of the weak acids on size and sensitivity to pH and temperature

ABSTRACT

We prepared nano/microgels by precipitation copolymerization of N-isopropylacrylamide (NIPAAm), and one of three different carboxyalkyl methacrylamides [methacryloylamido hexanoic acid (M₅), 8-methacryloylamido octanoic acid (M₇), and 11-methacryloylamido undecanoic acid (M₁₀)], either in the acid forms or as carboxylates (potassium salts). The hydrodynamic diameter (Dh) of the nano/microgels prepared with the carboxylates was smaller (≈100 nm for M₁₀ copolymers), compared to the size of homopolymeric NIPAAm microgels prepared by dispersion polymerization (around 600 nm), indicating that the carboxylates act as surfactants reducing the size of the seeds during the polymerization process. These materials presented a swollen-shrunken transition temperature (T _tr) similar to the T _tr of the homopolymeric NIPAAm microgels, without pH sensitivity. On the other hand, the copolymeric microgels prepared from the acid form of the comonomers have a similar or bigger size than NIPAAm microgels. For these copolymers, the T _tr can be tuned by the type and proportion of acid comonomer used and present pH sensitivity. This is important for biomedical applications such as positive temperature control release. Polyelectrolyte titration demonstrates that the nano/microgels prepared with the carboxylates behave as hard spheres, while the microgels prepared with the weak acid behave as porous materials.     

A thermoanalysis of phase transformations and linear shrinkage kinetics of ceramics made from ultrafine plasmochemical ZrO2(Y)–Al2O3 powders

The methods of X-ray diffraction analysis, thermogravimetric analysis, differential scanning calorimetry, and dilatometry are used to study special features of the structural-phase state of the 80 mass% ZrO₂(Y)–20 mass% Al₂O₃ plasmochemical powders (PCPs) and their effects on the sintering of composite ceramics. It is revealed that the ZrO₂(Y)–Al₂O₃ powder composite represents a mechanical mixture containing crystalline tetragonal zirconium dioxide and aluminum oxide nanoparticles, the latter found in an amorphous state and partially included into the ZrO₂(Y) lattice, thus forming metastable solid solutions of variable composition. Heating of the composite powder within the temperature range 740–1,000 °C reveals an exothermal effect associated with decomposition of metastable states of aluminum oxide. This is accompanied by the formation of the corundum-phase nuclei having subcritical dimensions. They achieve the critical sizes at higher temperatures T > 1200 °C, when α-Al₂O₃ is finally crystallized. The shrinkage response of the powder compacts during non-isothermal sintering is measured in a sensitive dilatometer. It is shown that the shrinkage curve consists of several stages that closely correlate with the concurrent structural-phase transformation in the composite ZrO₂(Y)–Al₂O₃ powder mixture. The decisive contribution into shrinkage during non-isothermal sintering of composite comes from the high-temperature stages with the maximum shrinkage rate at the temperatures 1,250 and 1,550 °C. It is found out that the regime of sintering the ultrafine PCPs (T = 1,600 °C, t = 1 h) allows producing composite ceramic materials with a porosity of Q ≈ (5–7) %, microhardness H _v = 12.3 GPa, and crack resistance К _1c = (10–11) MPa m^0.5.     

Dispersibility of Barium Titanate Suspension in the Presence of Polyelectrolytes: A Review

Dispersibility of colloidal barium titanate suspensions is reviewed with an emphasis on the use of various polyelectrolytes as dispersants. The fundamentals of colloidal stability are discussed followed by the colloidal properties of barium titanate powder. Dispersion behavior of BaTiO₃ in both nonaqueous and aqueous media has been reviewed. Several studies on the stabilization of micron and nano‐sized barium titanate using various polymeric dispersants and a rhamnolipid biosurfactant are presented and discussed. The article attempts to provide a comprehensive review of the current state‐of‐the‐art in the area of colloidal processing of barium titanate.     

Synthesis of nanometric β-barium metaborate powder from different borate solutions by ultrasound-assisted precipitation

In this study, the synthesis of barium metaborate powder (BaB₂O₄) was carried out by ultrasound-assisted precipitation using different borate solutions. Different solutions such as borax (Na₂B₄O₇, BD), boric acid (H₃BO₃, BA), and sodium metaborate (NaBO₂, SMB) were used in the synthesis and an ultrasonic immersion horn probe was used as the major source of ultrasound. The effect of reaction temperature and time, pH, and crystallization time on the BaB₂O₄ yield (%) was investigated. The ultrasound-assisted synthesis up to 90 % yield could be achieved using a 0.2 M BD solution at 80 °C, reacting for 5 min at pH 13 followed by 2 h of crystallization. Following crystallization, the obtained powder was heated up to 140, 250, 650, and 750 °C for 2.5 h, and it was shown that β-BaB₂O₄ nanometric powders were obtained after the 750 °C heat treatment.     

Reactivity of CO2 traps in aerogel–wollastonite composites

Synthetic wollastonite has been used as the active phase embedded into two different silica aerogel composites. These composites are different in respect of the route used for the synthesis of the wollastonite powder. Texture and composition of both types of composite have been characterized. In addition, several factors (pH, reaction time, CO₂ saturation, etc.) that could help to optimize the carbonation process at room temperature and pressure have been studied. Under the same conditions, both composites confirm previous results showing efficiencies as CO₂ sequesters between 80% and 100% in only 15 min of gas flow. The textural characteristics of the aerogel, together with the grain size of the synthetic wollastonite powder, not only increase the speed of the reaction, but also inhibit the appearance of a passivating layer on the surface of the wollastonite grains attacked by the CO₂. This is an outstanding feature as it insists on a cutting-edge challenge of the CO₂ research: its economical availability.     

Preparative isolation of paclitaxel and related taxanes from cell cultures of Taxus chinensis using reversed-phase flash chromatography

In this study, paclitaxel, baccatin III, taxuyunnanine C and sinenxane C were successfully separated by reversed-phase flash chromatography on a manually packed C₁₈ column from Taxus chinensis cell culture extract. The crude cell culture extract was first treated with Al₂O₃ column chromatography and then divided into two parts: fraction 1 and fraction 2. Ten milligrams of baccatin III and 19 mg of paclitaxel were obtained from 100 mg dried fraction 1. Fifty-two milligrams of taxuyunnanine C and 11 mg sinenxane C were obtained from 100 mg dried fraction 2. The purities of the four compounds were 98.02%, 98.53%, 98.93% and 98.76%, respectively. Their structures were characterised by using UV, MS and NMR. These results indicate that paclitaxel and related taxanes including baccatin III can be obtained from cell culture in a highly pure state using reversed-phase flash chromatography.