含(噁)唑环聚酰亚胺的制备及性能

以刚性棒状结构的2,6-二(对氨基苯)苯并[1,2-d;5,4-d’]二口恶唑为单体,采用两步法与三种不同结构的酸酐合成出了新型含口恶唑环聚酰亚胺薄膜。对聚酰亚胺的预聚体——聚酰胺酸的制备工艺的影响因素进行了详细的研究,聚酰胺酸的特性黏度均达到1.0dL/g以上,通过热环化处理得到了分子量较高的聚酰亚胺薄膜。经红外光谱测定,聚酰胺酸完全转化成聚酰亚胺。薄膜玻璃化温度均高于280℃,空气中热失重温度在520℃以上,表现出优异的热稳定性。     

TiAl–Nb melt interaction with pyrolytic boron nitride crucibles

This paper studies the chemical interaction on contact, and the related evolution of composition and microstructure of cast TiAl-based alloy, when using refractory oxygen-free pyrolytic boron nitride (pBN) crucibles/moulds instead of traditional oxide ceramic ones. We extend the research begun with AlN crucibles and reported in [4]. Three melting tests were performed in resistive SiC electro-furnace with Ti–46Al–8Nb (at%) alloy in 6N-purity pBN boat crucibles with fixed melt superheating times of 5, 12 and 25 min at 1670 °C and subsequent quenching with high-purity Ar gas flow. As-cast samples were examined by optical microscopy/metallography, X-ray diffractometry, SEM-BSE, EDX and EBSD micro-analyses, and compared to the initial material. Unlike the AlN it was shown that dissolved BN reacts with the melt, forming Ti₂AlN and (Ti,Nb)B micro-precipitates at the expense of selective destruction of the α₂-Ti₃Al major intermetallic phase in the solidified alloy: Ti₃Al + (Nb) + BN → Ti₂AlN + (Ti,Nb)B. The key features and temporal dynamics of this interaction are studied.     

NiMn2−xFexO4 prepared by a reverse micelles method as conversion anode materials for Li-ion batteries

Synthesis by reverse micelles was used to produce NiMn_2−xFe_xO₄ with nanometric particle sizes for their use as conversion anode materials for lithium ion batteries. The hydroxide precursor was characterized by infrared spectroscopy and the decomposition was followed by thermal analysis. Cation distribution in the spinel structure of pristine samples was evaluated by Mössbauer spectroscopy evidencing that octahedral Fe³⁺ is substituted by Mn³⁺ ions in NiMnFeO₄. Capacity values of 750 mA h g⁻¹ were retained for 50 cycles for NiMnFeO₄ and NiFe₂O₄, respectively. A good kinetic response was observed in NiMnFeO₄ at 2C.     

Crystal orientation dependence of the out-of-plane dielectric properties for barium stannate titanate thin films

The orientation-dependent out-of-plane dielectric properties of barium stannate titanate (Ba(Sn_0.15Ti_0.85)O₃ (BTS)) thin films prepared by sol–gel method were investigated. Films with (1 0 0), (1 1 0), and (1 1 1) orientation were grown on LaNiO₃-buffered (1 0 0), (1 1 0), and (1 1 1) LaAlO₃ (LAO) single-crystal substrates, respectively. The different temperature of the dielectric constant maximum (T_m) of the BTS thin films with different orientation was believed to be attributing to stress inside the films. Films with the (1 1 1) orientation had higher relative dielectric constant and tunability than (1 0 0)- and (1 1 0)-oriented films. This difference in dielectric properties in these three kinds of oriented BTS films may be attributed to change in the direction and magnitude of electric polarization in orientation engineered BTS films and stress in the films.     

On the size-dependent behavior of functionally graded micro-beams

In this paper, the size-dependent static and vibration behavior of micro-beams made of functionally graded materials (FGMs) are analytically investigated on the basis of the modified couple stress theory in the elastic range. Functionally graded beams can be considered as inhomogeneous composite structures, with continuously compositional variation from usually a ceramic at the bottom to a metal at the top. The governing equations of motion and boundary conditions are derived on the basis of Hamilton principle. Closed-form solutions for the normalized static deflection and natural frequencies are obtained as a function of the ratio of the beam characteristic size to the internal material length scale parameter and FGM distribution functions of properties. The results show that the static deflection and natural frequencies developed by the modified couple stress theory have a significant difference with those obtained by the classical beam theory when the ratio of the beam characteristic size to the internal material length scale parameter is small.     

Indium and gallium oxynitrides prepared in the presence of Zn by ammonolysis of the oxide precursors obtained via the citrate route

Ammonia nitridation of indium and gallium oxide precursors obtained through a soft solution route led to their oxynitrides [In_0.97□_0.03][N_0.92O_0.08] at 660 °C and [Ga_0.89□_0.11][N_0.66O_0.34] at 850 °C, respectively, where □ refers to a In or Ga vacancy. Cation vacancies in their wurtzite-type lattice were eliminated in similar preparations with the co-presence of Zn²⁺ by forming complete solid solutions of (InN)_1−x(ZnO)_x and (GaN)_1−y(ZnO)_y. The optical absorption edge shape was found to be relatively steep at the solid solution limits of x ≈ 0.23 and y ≈ 0.33 compared to the case without zinc.     

Anions of organic acids as gas suppressants in zinc-air batteries

One of the most important issues in the research related to Zn-air batteries is the hydrolysis of the aqueous solution. We have investigated the effectiveness of Zn ions and the anions of various acids as gas suppressants in the battery. Zn ions can function as a gas suppressant on a Pt surface, but they can stimulate additional gas production when they are deposited as Zn metal. On the other hand, the counter anions of weak acids behave as adsorbates to cover Zn metal effectively.     

Upconversion in Er-doped Gd2O3 nanocrystals prepared by propellant synthesis and flame spray pyrolysis

In this study, monoclinic luminescent Gd₂O₃ nanocrystals doped with different concentrations of Er³⁺ (0.1, 1, and 10 mol%) were produced by propellant synthesis and flame spray pyrolysis (FSP). A comparison of their optical and morphological properties is reported. Following 980 nm excitation, an increase of the emission intensity from the ²H_11/2, ⁴S_3/2 → ⁴I_15/2 and ⁴F_9/2 → ⁴I_15/2 transitions was observed with increasing Er³⁺ concentration in the Gd₂O₃ nanocrystalline samples prepared via both techniques. However, the overall upconversion emission intensity was greater for the samples obtained by FSP. Furthermore, as the Er³⁺ concentration was increased, the intensity of the red (⁴F_9/2 → ⁴I_15/2) emission was observed to increase more rapidly in comparison to the green (²H_11/2, ⁴S_3/2 → ⁴I_15/2) emission resulting in an overall enhancement of the red component in the upconversion emission. Although both synthetic routes yield average crystallite sizes in the nanoscale, the TEM and SEM images confirm a more homogeneous morphology and lower particle aggregation for the nanocrystals produced by FSP.     

Microhardness studies on calcium hydrogen phosphate (brushite) crystals

Vicker's and Knoop microhardness studies were carried out on grown calcium hydrogen phosphate dihydrate (CaHPO₄·2H₂O) crystals over a load range of 10-50 g. The Vickers (H_V) and Knoop (H_K) microhardness numbers for the above loads were found to be in the range of 94-170 kg/mm² and 28-35 kg/mm² respectively. It was also found that these numbers increased with increase in load. The Mayer's index (n) was found to be greater than 1.6 showing soft-material characteristics. The fracture toughness values (K_c), determined from measurements of crack length, were estimated to be 6 ± 0.5 × 10³ kg m^−3/2 and 4.5 ± 0.5 × 10³ kg m^−3/2 at 25 g and 50 g respectively. The brittleness indices (B_i) were found as 2.3 ± 0.1 × 10⁴ m^−1/2 for 25 g and 3.7 ± 0.1 × 10⁴ m^−1/2 for 50 g. Using Wooster's empirical relation, the elastic stiffness coefficient (c₁₁) has been calculated from Vicker's hardness values as 4.8 ± 0.5 × 10¹⁵ Pa for 10 g, 9.7 ± 0.5 × 10¹⁵ Pa for 25 g and 13.3 ± 0.5 × 10¹⁵ Pa for 50 g. The Young's modulus was calculated as 1.5 ± 0.1 × 10¹⁰ N m⁻² from Knoop microhardness values.     

Optical properties of silver sulphide thin films formed on evaporated Ag by a simple sulphurization method

Silver sulphide (Ag₂S) thin films were grown on the surface of silver films (Ag) deposited on glass substrate by using a simple chemical sulphurization method. According to X-ray diffraction analysis, the Ag₂S thin films display low intensity peaks at 34.48°, 36.56°, and 44.28°, corresponding to diffraction from (100), (112) and (103) planes of the acanthite phase (monoclinic). A model of the type Ag₂S/Ag/glass was deduced from spectroscopic ellipsometric measurements. Also, the optical constants (n, k) of the system were determined. Furthermore, the optical properties as solar selective absorber for collector applications were assessed. The optical reflectance of the Ag₂S/Ag thin film systems exhibits the expected behavior for an ideal selective absorber, showing a low reflectance in the wavelength range below 2 µm and a high reflectance for wavelengths higher than that value. An absorptance about 70% and an emittance about 3% or less were calculated for several samples.