The steric effect of exfoliation agent for fabrication of layer niobium oxide nanosheet

In this research, the steric effect of an exfoliation agent between n-ethylamine and triethylamine for the fabrication of Ca₂Nb₃O₁₀⁻ nanosheet was investigated. The experimental results revealed that the different structures of the exfoliation agent have affected to fabrication of Ca₂Nb₃O₁₀⁻ nanosheet. The use of n-ethylamine as an exfoliation agent gave a maximum exfoliation efficiency of 10 wt.% while the maximum exfoliation efficiency of triethylamine was 90 wt.%. The result showed that the difference in exfoliation efficiency was caused by the steric effect of exfoliation agents. The image of transmission electron microscopy exhibited Ca₂Nb₃O₁₀⁻ nanosheets which were formed by exfoliation of HCa₂Nb₃O₁₀. Furthermore, the reaction time for liquid exfoliation was studied in this work. The reaction time at 4 h gave a maximum of exfoliation efficiency. The Ca₂Nb₃O₁₀⁻ suspension was tested capability to remove hazardous ions. After the experiment, we found the white precipitate which was the formation of CsCa₂Nb₃O₁₀. The result showed that the Ca₂Nb₃O₁₀⁻ nanosheet was efficient for the removal of Cs⁺ ions in the wastewater.     

Improved selectivity in discriminating handedness and diameter of single-walled carbon nanotubes with N-substituted 3,6-carbazolylene-bridged chiral diporphyrin nanotweezers

Chiral diporphyrin nanotweezers 1 consisting of two chiral porphyrins with N-substituted 3,6-carbazolylene in between have been studied for the separation of single-walled carbon nanotubes (SWNTs). As compared to the analogous nanotweezers 2 without an N-substitutent, nanotweezers 1 with the N-octylcarbazolylene spacer exhibit much higher extraction ability and better selectivity for SWNTs. A narrower diameter range of SWNTs, from 0.88 to 0.92 nm, was selectively extracted with nanotweezers 1. In addition, only (7,6)-SWNTs of 0.90 nm diameter were optically enriched through extraction with 1, while SWNTs extracted with 2 showed lower optical purity of (7,6)-SWNTs. These enhanced extraction and discrimination abilities of 1 can be attributed to the formation of a more stable SWNT complex of 1 than of 2 in methanol.     

High-sensitivity determination of graft ratio of maleic anhydride-grafted polyolefin by anhydride methylation in supercritical methanol followed by H NMR spectroscopy

A wide range of graft ratios in Maleic anhydride (MA)-grafted polyolefin (PO), MA-g-PO, was determined by the combination of the methylation of grafted MA in supercritical methanol with quantification by ¹H NMR spectroscopy. The combination enabled the determination of a graft ratio as low as 0.01 wt% (100 ppm) in MA-g-PO.     

Preparation of novel silica/poly(butylene succinate-co-adipate) organic–inorganic hybrid biodegradable material via sol–gel method

Silica/poly(butylene succinate-co-adipate) organic–inorganic hybrid biodegradable materials were prepared by the sol–gel method. Fourier-transform infrared spectroscopy (FT-IR) and Thermogravimetry/differential thermal analysis (TG/DTA) indicated that the inorganic (SiO₂, C₆H₅SiO_3/2) and organic (PBSA) components were well dispersed in the hybrid material. Heat resistant test shows that the hybrid material was both heat resistant and flexible. The presence of phenyl groups and siloxane network was responsible for the flexibility and heat resistance.     

Dependence of property, cathode characteristics, thermodynamic stability, and average and local structures on heat-treatment condition for LiNi0.5Mn0.5O2 as a cathode active material for Li-ion battery

LiNi_0.5Mn_0.5O₂ was heat-treated under high oxygen-pressure and Ar-reducing conditions, and then the cathode properties, thermodynamic stability and average and local structures were investigated. From X-ray diffraction and ICP measurements, it was found that the pristine LiNi_0.5Mn_0.5O₂ had a single phase of the layered rock-salt structure although the Ni content was slightly rich compared with the nominal one. These characteristics were kept even after the heat-treatments. Charge–discharge cycle tests clarified that the cycle performance of LiNi_0.5Mn_0.5O₂ was improved by both the reducing and oxidizing treatments. From neutron diffraction and X-ray absorption fine structure measurements, the local distortion around the transition metal, especially Ni, was supposed to be one of the important factors to determine the cathode properties. It was also found that the sample with higher thermodynamic stability exhibited better capacity retention in the discharge–charge cycle tests.     

Shielding effect of double microelectrode tips in a scanning electrochemical microscope

Electrochemical interaction of coaxial double microelectrodes, in which a ring microelectrode was surrounded by another ring microelectrode, was investigated. Mass-transfer reactions that occurred on both inner and outer microelectrodes interfered with each other and showed a “shielding” effect depending on potentials and geometries of microelectrodes. Application of the inner microelectrode of the double microelectrodes for a probing tip of a scanning electrochemical microscope (SECM) revealed that the shielding effect by the outer microelectrode affected the electrochemistry on the inner microelectrode in the vicinity of the substrate surface. The effect was intensified above the insulator but attenuated above the conductor as the microelectrodes approached in feedback mode of the SECM. Approach to a critical interelectrode distance also intensified the shielding effect in the substrate generation/tip collection mode. An SECM line-scan using a platinum/epoxy resin-model substrate was carried out to investigate the shielding effect on current sensitivity and lateral resolution of an SECM image.     

Physicochemical Characterization of Chrysin‐Derivative‐Loaded Nanostructured Lipid Carriers with Special Reference to Anticancer Activity

Homologues long‐chain chrysin derivatives (LCD, C _n: 8–18) were synthesized and incorporated into nanostructured lipid carriers (NLC) with the aim to treat human neuroblastoma. Mutual miscibility and attractive interactions among the NLC components, namely tripalmitin (TP), cetyl palmitate (CP), oleic acid (OA), and the chrysin (CHR) derivatives (LCD) at the air–water interface were assessed by the Langmuir monolayer approach. Optimum combination for the NLC formulations was found to be 2:2:1 (M/M/M) for TP/CP/OA, respectively. NLC formulations, both in the absence and presence of LCD, were characterized by combined dynamic light scattering, electron microscopy, atomic force microscopy, and differential scanning calorimetry. The size and zeta potential of the NLC formulations were found in the range 200–350 nm and ?12 to ?18 mV, respectively. Encapsulation efficiency and release kinetics of CHR and LCD when loaded into NLC were also evaluated. LCD exhibited maximum incorporation, drug‐loading capacity, and sustained release because of its enhanced hydrophobicity. Superior incorporation efficiency and sustained‐release profile of LCD were able to enhance their anticancer activity against human neuroblastoma cell lines, compared to CHR, making them promising agents in combating cancer.     

Distribution of carbon contamination in MgAl2O4 spinel occurring during spark-plasma-sintering (SPS) processing: I – Effect of heating rate and post-annealing

Carbon contamination from the carbon paper/dies during spark-plasma-sintering (SPS) processing was examined in the MgAl₂O₄ spinel. The carbon contamination sensitively changes with the heating rate during the SPS processing. At the high heating rate of 100 °C/min, the carbon contamination having organized structures occurred over almost the entire area from the surface to deep inside the SPSed spinel disk. In contrast, at the slow heating rate of 10 °C/min, the carbon contamination having disordered structures occurred only around the surface area. The carbon phases transform into high pressure CO/CO₂ gases by post-annealing in air and lead to pore formation along the grain junctions. The pore formation significantly occurs at the high heating rate due to the large amount of the contaminant carbon phases. This suggests that if once the carbon contamination was formed in the materials, it is very difficult to remove the carbon phases from the materials.     

In situ binary sol–gel reaction of various trifunctional alkoxysilane in the silane‐grafted polyolefin matrix and its effect upon the mechanical properties

The vinyltrimethoxysilane‐grafted ethylene‐propylene copolymer/trifunctional methoxysilane (EPR‐g‐VTMS/RTMS) composites were prepared via in situ silica sol–gel reactions. Five trifunctional methoxysilane compounds (n‐hexyltrimethoxysilane, n‐decyltrimethoxysilane, n‐tetradecyltrimethoxysilane, n‐octadecyltrimethoxysilane, and phenyltrimethoxysilane) have been selected for this study. The water‐cross‐linked EPR‐g‐VTMS/RTMS composites were characterized by attenuated total reflectance‐Fourier transform infrared spectroscopy, gel content, solid‐state ²⁹Si CP/MAS NMR, wide‐angle x‐ray scattering, tensile strength, and field emission scanning electron microscopy measurements. The type of RTMS additive has a substantial influence on the nature of siloxane band networks and eventually the mechanical tensile properties. This finding suggests that the interaction and/or entanglement between the EPR‐g‐VTMS matrix and the substituent of the RTMS additives are crucial for the modifying mechanical properties. Moreover, for the water‐cross‐linked EPR‐g‐VTMS/CnTMS (n = 6, 10, 14, and 18) composites, the joint evidence provided by attenuated total reflectance‐Fourier transform infrared spectroscopy, ²⁹Si CP/MAS NMR, and wide‐angle x‐ray scattering results suggested the formation of ladder‐type poly(n‐alkyl silsesquioxane)s and the presence of the highly ordered structure with a thickness equal to the length of two n‐alkyl groups in all‐trans conformation. POLYM. ENG. SCI., 2011. © 2010 Society of Plastics Engineers.     

Broadband semi‐parametric estimation of long‐memory time series by fractional exponential models

This article proposes broadband semi‐parametric estimation of a long‐memory parameter by fractional exponential (FEXP) models. We construct the truncated Whittle likelihood based on FEXP models in a semi‐parametric setting to estimate the parameter and show that the proposed estimator is more efficient than the FEXP estimator by Moulines and Soulier (1999) in linear processes. A Monte Carlo simulation suggests that the proposed estimation is more preferable than the existing broadband semi‐parametric estimation.