Acidity and basicity of hydrotalcite derived mixed Mg-Al oxides studied by test reaction of MBOH conversion and temperature programmed desorption of NH3 and CO2

Mg-Al hydrotalcites intercalated with five different interlayer anions—CO₃²⁻, SO₄²⁻, Cl⁻, HPO₄²⁻ or terephthalate—were synthesized by either the coprecipitation or ion-exchange method. The structure of the as-synthesized samples and the presence of intended anions in the interlayer gallery of hydrotalcites were determined by X-ray diffraction and FTIR spectroscopy. On calcination at 600 °C the materials were transformed into mixed metal oxides. The kind of the counterbalancing anions present in the parent hydrotalcite influences strongly textural parameters of the obtained Mg-Al oxides. Both temperature-programmed desorption of NH₃ and CO₂, and test reaction of 2-methyl-3-butyn-2-ol (MBOH) conversion were used to determine the acidity and basicity of the samples. The hydrotalcite derived mixed Mg-Al oxides showed the presence of Brønsted and Lewis acid and base sites. However, the strong basic character of the solids caused that acetone and acetylene were observed as the major products of MBOH conversion.     

Fluorescence and IR characterization of epoxy cured with aliphatic amines

Cure reactions of the stoichiometric mixtures of diglycidyl ether of bisphenol A (DGEBA) and two very low molecular weight aliphatic polyether diamines (PED) were studied by using fluorescence and mid- and near-IR spectroscopic techniques. As the cure proceeded, the primary amine groups in PED are converted to the secondary and the tertiary amines. Near-IR spectral analysis was used to calculate the concentration of the three amine groups as a function of cure time. The decrease in the fluorescence intensity of DGEBA at about 307 nm was observed due to more effective quenching of the tertiary amine groups in PED, in comparison to the primary and the secondary amine groups. A large decrease in fluorescence intensity at 75 and 95 °C cure was observed. The amount of all the amine species was estimated from NIR spectra to shed light on the cure kinetics of PPO (polypropylene oxide) in comparison with PEO (polyethylene oxide) epoxy, as well as to explain their fluorescence behavior.The fluorescence intensity changes were correlated to the extent of epoxy reaction obtained by mid- and near-IR spectroscopy.     

An investigation into physicochemical characteristics of ash produced from combustion of oil palm biomass wastein a boiler

Ash derived from combustion of Malaysian oil palm biomass (empty fruit bunches consisting of fibers) was physically and chemically characterized in order to provide a comprehensive understanding of its specific properties in terms of toxicity, compositions and reusability. Principal analyses conducted include particle size distribution, scanning electron microscopy, elemental dispersive X-ray, elemental analysis, toxicity characteristic leaching procedure (TCLP) as well as thermogravimetric, X-ray diffractometry and Fourier-transform infrared analyses. TCLP result indicated that the oil palm ash (OPA) should not be classified as toxic wastes in terms of heavy metal leachability since leachable copper, cadmium, lead and nickel concentrations were detected below the stipulated leachability limits. It was determined that the OPA contained high amount of potassium as well as presence of silica which implied its suitability to be reused as crude fertilizer or cement replacement material.     

From Long Infrared to Very Long Infrared Wavelength Focal Plane Arrays Made with HgCdTe n + n ?/ p Ion Implantation Technology

This paper aims at studying the feasibility of very long infrared wavelength (VLWIR) (12–18 μm) focal plane arrays using n-on-p planar ion-implanted technology. To explore and analyze the feasibility of such VLWIR detectors, a set of four Cd _x Hg_1−x Te LPE layers with an 18 μ cutoff at 50 K has been processed at Defir (LETI/LIR–Sofradir joint laboratory), using both our “standard” n-on-p process and our improved low dark current process. Several 320 × 256 arrays, 30-μm pitch, have been hybridized on standard Sofradir readout circuits and tested. Small dimension test arrays characterization is also presented. Measured photonic currents with a 20°C black body suggest an internal quantum efficiency above 50%. Typical I(V) curves and thermal evolution of the saturation current are discussed, showing that standard photodiodes remain diffusion limited at low biases for temperatures down to 30 K. Moreover, the dark current gain brought by the improved process is clearly visible for temperatures higher than 40 K. Noise measurements are also discussed showing that a very large majority of detectors appeared background limited under usual illumination and biases. In our opinion, such results demonstrate the feasibility of high-performance complex focal plane arrays in the VLWIR range at medium term.     

Structural properties of phosphorous-doped polycrystalline silicon

The structural properties and hydrogen bonding of undoped and phosphorous doped polycrystalline silicon produced by step-by-step laser dehydrogenation and crystallization technique were investigated using Raman spectroscopy and hydrogen effusion measurements. At low laser fluences, E_L, a two-layer system is created. This is accompanied by the change in hydrogen bonding. The intensity of the Si–H vibration mode at 2000 decreases faster than the one at 2100 cm⁻¹. This is even more pronounced in phosphorous-doped specimens. The laser crystallization results in an increase of the hydrogen binding energy by approximately 0.2–0.3 eV compared to the amorphous starting materials.     

Formation and electronic structure of interface

In the present work the formation of the interface between polycrystalline silver and thin films of titanium oxide was studied with photoelectron spectroscopy (XPS, UPS) and time-of-flight secondary ion mass spectrometry (TOF-SIMS). Titanium oxide was deposited stepwise on 100 nm thick silver films by reactive magnetron sputtering allowing to study the evolution of the interface formation process. The process involves two steps: formation of thin layer of silver oxide and subsequent growth of the TiO₂ film. For better understanding of the silver oxidation process, pure silver films were exposed to a low temperature Ar/O plasma for different time intervals providing a possibility to investigate early stages of the oxide film growth.     

基于复数主成分分析的磁共振波谱信号衰减系数的自动校正

衰减系数的校正是磁共振波谱信号处理和分析过程中的一个关键难题。本文基于复数主成分分析，提出了一种自动的磁共振波谱衰减系数的校正方法，较成功地解决了这个难点问题。文中的模拟数据及其实现结果充分验证了该方法的有效性。     

铀表面初始氧化行为的电子能量损失谱研究

利用俄歇电子能谱仪获取了表面清洁的铀及其在氧化过程中的电子能量损失谱(EELS)，研究这些电子能量损失谱线显示：清洁表面铀的等离子损失的实验值与理论值较为符合；随着氧化程度的加剧，体等离子体(BP)、表面等离子体(SP)以及价带间跃迁所造成的电子能量损失峰发生了明显的连续偏移和强度的变化，表明室温下清洁表面铀暴露微量纯氧后，在铀表面上发生了U→UO→UO2初始氧化过程。同时，又采用了俄歇电子能谱(AES)和X射线光电子谱(XPS)对照分析了铀的初始氧化过程。     

A novel method for determination of polyester end-groups by NMR spectroscopy

An efficient, convenient and quantitative method for characterising polyester end-groups is described. We have found that trichloroacetyl isocyanate (TAI) reacts rapidly and quantitatively with both carboxyl [C(O)OH] and hydroxyl (OH) chain ends to form derivatives that can be readily determined by ¹H NMR spectroscopy. The TAI capped end-groups give rise to characteristic imidic NH resonances in a normally clear region of the ¹H NMR spectrum [δ∼10-11.5 for C(O)-O-C(O)-NH-C(O)CCl₃ from C(O)OH, δ∼8-9 for O-C(O)-NH-C(O)CCl₃ from OH]. The method has been successfully applied to quantitative determination of the end-groups of a wide variety of oligomeric polyesters. It has also been applied to higher molecular weight polyesters including commercial, bottle grade, poly(ethylene terephthalate) (PET) and PET based copolyesters (e.g. PETG).