Unsaturated polyester resin (UPR) reinforced with flax fibers,untreated and cold He plasma-treated: thermal,mechanical and DMA studies

Hemp, jute, flax, bagasse, coconut and bamboo fibers are some of the natural fibers that have attracted attention for the preparation of composite materials because of their low cost compared with synthetics fibers (glass, carbon). The performance of a natural fiber as reinforcement in composite materials is linked to its ability in term of adhesion with the synthetic matrix. This depends mainly on the quality of the fiber surface. In order to improve this adhesion, a thin reactive coating is generally used. In this study, cold He plasma treatments have been carried out on reinforcing flax fiber. Composites with unsaturated polyester resin (UPR) have been used with untreated flax fibers and plasma-treated fibers. The data characterizing the thermal, mechanical (dynamic and static) will be presented in order to analyze the efficiency of the He plasma treatment on the composite performances.     

Effect of Pb additive on crystallization kinetics of Se80In20 glassy matrix

The crystallization kinetics of bulk Se₈₀In_20−xPb_x (x=0, 5, 10 and 15) chalcogenide glasses have been studied using a differential scanning calorimeter (DSC) with different heating rates (5, 10, 15 and 20 K/min) under non-isothermal conditions. Various kinetic parameters of crystallization, such as crystallization temperature T_c, peak crystallization temperature T_p, activation energy for crystallization E_c and order parameters n, m have been determined to study nucleation and growth during crystallization. The reaction rate constant K and pre-exponential factor K₀ also have been determined. The composition dependence of these parameters may be explained on the basis of modification of chemical bonds present in the Se–In system due to addition of Pb content.     

HA纳米微粒对PEG-600低温保护剂反玻璃化结晶的影响

为了研究羟基磷灰石HA纳米微粒对低温保护剂反玻璃化结晶的影响,本文利用DSC和低温显微镜研究了含有不同粒径(20nm、40nm、60nm)和不同质量浓度(0.1%、0.2%、0.4%、0.8%)HA纳米微粒的PEG-600(50%,w/w)溶液反玻璃化过程中的结晶现象.试验结果表明:与未添加纳米微粒的PEG-600溶液相比,加入40nm、0.4%纳米微粒的HA-PEG600溶液的反玻璃化温度升高了7℃;加入20nm、0.4%和40nm、0.8%纳米微粒的HA-PEG600溶液的冰晶生长速率分别降低了35%和提高了50%;纳米低温保护剂溶液的冰晶形貌从大圆形变成了小圆形、枝晶或小圆形中夹带枝晶.     

β-环糊精衍生物与吡罗昔康的包合特性

采用荧光光谱、差热扫描和核磁共振法,研究了不同酸度下吡罗昔康（PX）与β-环糊精（β-CD）、羟丙基-β-环糊精（HP-β-CD）和磺丁醚-β-环糊精（SBE-β-CD）的包合特性。 结果表明,吡罗昔康与3种环糊精均形成了1∶2.5的包合物。 以包合常数为包合能力的量度,中性条件下,包合平衡常数分别为1.2×106、1.8×106、2.0×106,3种环糊精的包合能力为SBE-β-CD＞HP-β-CD＞β-CD。     

Spectroscopic and Structural Study of a New Conducting Pyrazolium Salt

The increase in conductivity with temperature in 1H-pyrazol-2-ium 2,6-dicarboxybenzoate monohydrate was analyzed, and the influence of the mobility of the water was discussed in this study. The electric properties of the salt were studied using the impedance spectroscopy method. WB97XD/6-311++G(d,p) calculations were performed, and the quantum theory of atoms in molecules (QTAiM) approach and the Hirshfeld surface method were applied to analyze the hydrogen bond interaction. It was found that temperature influences the spectroscopic properties of pyrazolium salt, particularly the carbonyl and hydroxyl frequencies. The influence of water molecules, connected by three-center hydrogen bonds with co-planar tetrameters, on the formation of structural defects is also discussed in this report.     

Melt-crystallization behavior and isothermal crystallization kinetics of crystalline/crystalline blends of poly(ethylene terephthalate)/poly(trimethylene terephthalate)

The melt-crystallization and isothermal melt-crystallization kinetics of poly(ethylene terephthalate)/poly(trimethylene terephthalate) blends (PET/PTT) were investigated by differential scanning calorimetry (DSC) and polarized optical microscopy. Although PET and PTT in the binary blends are miscible at amorphous state, they will crystallize individually when cooled from the melt. In the DSC measurements, PET component with higher supercooling degree will crystallize first, and then the crystallite of PET will be the nucleating agent for PTT, which induce the crystallization of PTT at higher temperature. On the other hand, in both blends of PET80/PTT20 and PET60/PTT40, the PET component will crystallize at higher temperature with faster crystallization rate due to the dilute effect of PTT. So the commingled minor addition of one component to another helps to improve the crystallization of the blends. For blends of PET20/PTT80 and PET40/PTT60, isothermal crystallization kinetics evaluated in terms of the Avrami equation suggest different crystallization mechanisms occurred. The more PET content in blends, the fast crystallization rate is. The Avrami exponent, n = 3, suggests a three-dimensional growth of the crystals in both blends, which is further demonstrated by the spherulites formed in all blends. The crystalline blends show multiple-melting peaks during heating process.     

Characterizations of self-combustion reactions (SCR) for the production of nanomaterials used as advanced cathodes in Li-ion batteries

In this work, self-combustion reactions (SCR) for the preparation of important cathode materials for rechargeable Li-ion batteries were investigated by thermal analytical tools (DSC, ARC, TGA), electron microscopy, XRD, various spectroscopies (MS, Raman, FTIR) and elemental analysis by ICP. The systems studied include solutions containing metal nitrates at the right stoichiometry and sucrose as a fuel, for the preparation of LiMn_0.5Ni_0.5O₂ (layered), LiMn_1.5Ni_0.5O₄ (spinel), LiMn_0.33Ni_0.33Co_0.33O₂ (layered), and LiMn_0.4Ni_0.4Co_0.2O₂ (layered). Similar products, which do not depend on the atmosphere of the processes (air or inert) were obtained by spontaneous SCR and the gradual heating of the same solutions by DSC, ARC, and TGA. The reactions involve the partial caramelization of sucrose, complicated by red-ox reactions with the nitrates that form solid products, whose organic part is finally decomposed around 400 °C. The presence of cobalt ions has a stabilizing effect, which is expressed by the low dissolution rates of Li ions from the solid products thus formed, into aqueous solutions. The reaction mechanisms are discussed herein.     

Investigation of the Interactions in Complexes of Low Molecular Weight Chitosan with Ibuprofen

Complexation between ibuprofen and low molecular weight chitosan (LMWC) was studied. LMWC was prepared from high molecular weight chitosan using the acid hydrolysis method. The complexes were investigated by using DSC, FT-IR and liquid-state ¹H-NMR. Molecular mechanics (MM) calculations were used to give insight into the stoichiometry of the interaction of chitosan with ibuprofen. The results showed that complexation of ibuprofen with LMWC involves ionic interaction between the ammonium group of LMWC and the carboxylate anion of ibuprofen. It was also shown that it is more efficient to prepare the complexes using lower concentration solutions of the polymer. These results were supported by molecular mechanics calculations. The experimental results may explain the discrepancies in the literature where, in many studies, the concentration of chitosan and its low average molecular weight were not considered to be important factors in the complexation process.     

An analysis of the thermal aging behaviour in high-performance energetic composites through the glass transition temperature

Differential scanning calorimetry (DSC) was used to analyze the thermal aging behaviour in energetic composite materials where a hydroxyl-terminated polybutadiene (HTPB)/isophorone diisocyanate elastomer is the polymeric matrix. Different parameters from the analysis of the glass transition, such as the glass transition temperature (T_g), were used in order to monitor this isothermal aging at 65 °C during a total time of 3000 h, finding an increasing and broadening T_g. In addition, the accelerated aging behaviour of these materials was also studied by a classical method, based on the change of mechanical properties such as those of Young's modulus or strain at break. The correlation between both methodologies was examined, demonstrating that an analytical technique such as DSC allows the evaluation of the actual state of composite solid propellants with a small sample and a straightforward measurement.     

Metastable phases in Gallium-Indium eutectic alloy particles and their size dependence

In this paper, submicrometer-sized Ga-In eutectic alloy particles were dispersed into polymethylmethacrylate (PMMA) matrix by ultrasonic vibration and sedimentation method. The solidification and melting processes of Ga-In eutectic alloy particles were studied by differential scanning calorimeter (DSC). Four endothermal peaks with the onset temperature located at 16, −11, −22, and −27 °C were observed in DSC heating curves, which corresponded to the melting process of the stable Ga-In phase α-Ga(In) and three metastable phases of β-Ga(In), δ-Ga(In) and γ-Ga(In), respectively. The stable phase α-Ga(In) can only be formed when the size of alloy particle was larger than 0.58 μm. Conversely, metastable phases β-Ga(In), δ-Ga(In) and γ-Ga(In) are mainly formed. The result shows that phase structures in Ga-In eutectic alloy are size dependent.