Sensitivity of a solid Eu(III) complex towards acetonitrile vapor: Structural and spectroscopic characterization

The Eu(III) nitrate complex of the meso- N,N′-bis(2-pyridylmethylene)-1,2-(R,S)-cyclohexanediamine ligand was synthesized and characterized by single crystal and powder X-ray diffraction. The crystal lattice of the complex is capable of absorbing and desorbing selectively acetonitrile molecules, at 293 K upon an acetonitrile vapor pressure of ∼0.1 × 10⁵ Pa. This process, which is partially reversible, can be easily followed by both powder X-ray diffraction (P-XRD) and Eu(III) luminescence spectroscopy. The acetonitrile molecule, located in the outer coordination sphere of the metal ion, does not affect the radiative transition probability of ⁵D₀ level of Eu(III) and also it does not activate further non-radiative channels from this level. On the other hand, this molecule is capable of affecting the energy position and intensities of the crystal field components of the ⁵D₀→⁷F₂ transition. The complex in solid form can be considered a promising material for the optical sensing of acetonitrile vapors.     

Steel slag waste combined with melamine pyrophosphate as a flame retardant for rigid polyurethane foams

To explore the potential application of industrial waste, steel slag powder in combination with melamine pyrophosphate (MPP) was adopted to improve the flame retardancy of rigid polyurethane foam (RPUF). The incorporation of steel slag slightly reduced the thermal conductivity of the resulting flame-retardant RPUF samples. The addition of MPP and/or steel slag did not significantly alter the thermal stability in terms of T_-10% and T_max but did obviously increase the T_-50% value, suggesting the improved thermal resistance of the residues. The coaddition of MPP and steel slag into RPUF resulted in higher LOI values and lower peak heat release rates than the samples incorporating either MPP or steel slag alone. The superior flame retardancy could be attributed to MPP promoting char formation, which then acted as a barrier at the beginning of RPUF thermal decomposition; simultaneously, the thermally stable inorganics in the steel slag powder strengthened the thermal resistance of this char layer.     

The control of paracetamol particle size and surface morphology through crystallisation in a spray dryer

The parameters governing the crystallisation of paracetamol using various conventional techniques has been extensively studied, however the factors influencing the drug crystallisation using spray drying is not as well understood. The aim of this work was to investigate the crystallisation of an active pharmaceutical ingredient through evaporative crystallisation using a spray dryer to study the physicochemical properties of the drug and to use semi-empirical equations to gain insight into the morphology and particle size of the dried powder. Paracetamol solutions were spray dried at various inlet temperatures ranging from 60 °C to 120 °C and also from a series of inlet feed solvent compositions ranging from 50/50% v/v ethanol/water to 100% ethanol and solid-state characterisation was done. The size and morphology of the dried materials were altered with a change in spray drying parameters, with an increase in inlet temperature leading to an increase in particle Sauter mean diameter (from 3.0 to 4.4 µm) and a decrease in the particle size with an increase in ethanol concentration in the feed (from 4.6 to 4.4 µm) as a result of changes in particle density and atomised droplet size. The morphology of the dried particles consisted of agglomerates of individual crystallites bound together into larger semi-spherical agglomerates with a higher tendency for particles having crystalline ridges to form at higher ethanol concentrations of the feed.     

Structural and physicochemical properties of silver-rich Ag–Al alloys

The X-ray diffraction, Scanning Electron Microscopy, Differential Scanning Calorimetry, dilatometric and electrical conductivity measurements were used to study the structural and physicochemical properties of selected silver-rich alloys from Ag–Al system. All the studied alloys, containing from 10 to 37 at. % of Al (Ag₉₀Al₁₀, Ag₈₅Al₁₅, Ag₇₇Al₂₃, Ag₇₅Al₂₅, Ag₇₂Al₂₈, Ag₇₀Al₃₀, Ag₆₃Al₃₇), were prepared from high purity metals by melting in a glove-box filled with a high purity argon atmosphere. The obtained X-ray diffraction patterns and microstructure observation of alloys containing up to 15 at. % of Al suggested that in this range only solid solution of silver exists. The thermal analysis showed heat effects related to phase transitions in Ag–Al system. In addition, the thermal expansion studies revealed an anomalous behavior in expansion for some composition of alloys associated with the phase transition. The electrical conductivity values rapidly changed, which may be associated with the formation of different phase areas in the Ag–Al system.Based on the results obtained in this work and critically reviewed literature data a thermodynamic re-optimization of the binary Ag–Al system using CALPHAD method was proposed. A good agreement between calculation and experiment was found.     

Fatigue performance of friction stir welded Al2024 alloy in a different corrosive environment

The study examines the corrosion fatigue behavior of friction stir welded Al2024 alloy in the corrosive medium. The fatigue tests are conducted at a stress ratio of -1 in the different corrosive medium. The decrease in the fatigue life of welded joints in the corrosive environment is attributed to an increase in the crack initiation susceptibility in the presence of corrosive media. The fractured surfaces are investigated using the scanning electron microscopy (SEM). The formation of the corrosive compounds was studied using x-ray diffractometry.     

2219铝合金搅拌摩擦焊和钨极保护焊焊接件残余应力的中子衍射研究

利用中子衍射法对2219铝合金搅拌摩擦焊（FSW）和钨极保护焊（TIG）焊接件开展了三维残余应力测量，并对残余应力分布规律进行了分析。结果表明：焊接件的纵向残余应力数值较大；FSW焊接件残余应力整体较TIG焊接件的小；FSW和TIG焊接件的残余拉应力最大值分别为101 MPa和174 MPa，FSW焊接件残余拉应力最大值较TIG焊接件的小；FSW残余拉应力最大值处于轴肩边缘，且前进侧峰值大于后退侧峰值；TIG焊接件残余拉应力最大值处于焊缝边缘。通过中子衍射实验获得的焊接件残余应力分布，将可用于焊接工艺的优化与焊接件的寿命预测。     

Heat-treatable Mg-9Al-6Sn-3Zn extrusion alloy

Mg-9Al-6Sn-3Zn (wt%) alloy was extruded and heat treated in T5 and T6 conditions, and its mechanical properties and microstructures were investigated. The extruded product can be slightly strengthened by the T5 treatment as a result of sparse and heterogeneous precipitation. Significant increase in strength is achieved by the T6 treatment, and this is mostly attributed to the formation of lamellar discontinuous Mg₁₇Al₁₂ precipitates. The segregation of Al and Zn at grain boundaries is responsible for the discontinuous Mg₁₇Al₁₂ nucleation. The T6-treated alloy exhibits a tensile yield strength of 341 MPa and an ultimate tensile strength of 409 MPa, together with an elongation to fracture of 4%.     

Polypyrrole and platinum deposited onto carbon substrate to enhance direct methanol fuel cell electrodes behaviour

The aim of this work is to study the ability of polypyrrole to reduce the platinum load of low temperature methanol fuel cell electrodes. Platinum was deposited onto carbon paper and a layer of polypyrrole electrodeposited onto carbon paper, using electron beam evaporation and electrodeposition by pulses. Subsequently, the morphology and electrochemical behaviour of the synthesised samples were analysed in sulphuric acid solution, determining their electrochemically active surface area; and in a solution of sulphuric acid and methanol, to analyse their catalytic performance. The electrochemical measurements showed that the electrochemically active surface area and the catalytic performance of the electrodes prepared by evaporating platinum are increased when prepared on the polypyrrole film. Electrodes prepared using the pulse electrodeposition technique presented fairly homogeneous coatings that led to the reduction of the oxidation potential of methanol and the increase of their resistance to CO poisoning.     

The effect of synthesis conditions on the phase composition and structure of thorium bearing murataite ceramics

Samples of thorium-bearing ceramic with a target composition (wt%) 5 Al₂O₃, 10 CaO, 55 TiO₂, 10 MnO, 5 Fe₂O₃, 5 ZrO₂, 10 ThO₂ were produced by melting in glassy carbon crucibles in a resistive furnace and by cold crucible inductive melting (CCIM) at a vibration power of 10 kW and operation frequency of 5.28 MHz. All the samples contained 85–95 vol% murataite polytypes with 5- (5C), 8- (8C), and 3-fold (3C) elementary fluorite unit cell composing core, intermediate zone and rim of the grains, respectively, and minor crichtonite, perovskite, pyrochlore, rutile, etc. A feature of the ceramics obtained by melting in glassy carbon crucibles is formation of Fe (II) titanate whereas the inductive-melted ceramics contained traces of vitreous phase due to melt contamination with a cold crucible putty material. Melting rate in the cold crucible of up to 350 kg/(m² × h) has been achieved. The ceramics obtained have excellent chemical durability.