Hydrogen sorption behaviour of Mg-5wt.%La alloys after the initial hydrogen absorption process

In our earlier study, it has been shown that trace Na additions can improve the reaction kinetics of Mg–5%La (wt.%) alloys during the first absorption. However, the subsequent hydrogen desorption/absorption process of the Mg–5%La after the first absorption has not been investigated. In this study, we have investigated the hydrogen sorption behaviour of the Mg–5%La alloy after the first absorption in terms of phase evolution, and lattice expansion properties during desorption as function of temperature using in-situ synchrotron Powder X-ray Diffraction (PXRD) and in-situ High Voltage Transmission Electron Microscopy (HVTEM). Two distinct phase evolutions, a continuous phase transformation of LaH₃ → LaH₂ + ½ H₂ (from 250 °C) and decomposition of MgH₂ → Mg + H₂ (between 440 and 460 °C) were identified during the desorption. It is determined that this alloy is cyclable in the absence of Mg₁₂La intermetallic during the subsequent absorption/desorption cycling after the first hydrogen absorption.     

High temperature oxidation behavior of MoSi2–Al2O3 composite coating on TZM alloy

A novel MoSi₂–Al₂O₃ composite coating was prepared on Mo-based TZM alloy by slurry sintering method. The oxidation behavior of the coating was evaluated at 1600 °C in static air. Microstructure and phase composition of the as-prepared and oxidized coatings were characterized, and the antioxidant mechanism of the coating at high temperature was discussed. A three-layer structure was observed in the as-prepared coating, consisting of a ～2 μm thick Mo₅Si₃ diffusion layer, a ～65 μm thick MoSi₂ inner layer and a ～36 μm thick outer layer of mixture of MoSi₂ and Al₂O₃. After oxidation at 1600 °C for 5 h, all MoSi₂ phases were completely converted to intermediate silicide Mo₅Si₃ by solid-state diffusion, and the formed Mo₅Si₃ phase would be transformed into Mo₃Si phase with further extending the oxidation time. Furthermore, a dense oxide layer of SiO₂-mullite was formed on the specimen surface, which can effectively protect the material to further oxidation. The MoSi₂–Al₂O₃ coating could protect the substrate effectively at 1600 °C for 20 h without failure. The enhanced oxidation resistance of MoSi₂–Al₂O₃ coating is due to the formation of multi-layer structure containing a SiO₂-mullite composite oxide outer layer with high thermal stability and low oxygen permeability.     

Thermodynamic properties of sodium pyrovanadate (Na4V2O7) at high temperature (298.15–873 K)

The sodium pyrovanadate (Na₄V₂O₇) powder was synthesized by solid-state reaction using sodium carbonate (Na₂CO₃) and vanadium pentoxide (V₂O₅) as raw materials. X-ray powder diffraction (XRD), scanning electron microscope (SEM), and differential scanning calorimeter (DSC) were used to accurately characterize the synthesized sample. The solid-state phase transformation from α-Na₄V₂O₇ to β-Na₄V₂O₇ occurs at the temperature 696 K and the enthalpy is equals to 1.03 ± 0.01 kJ/mol, the endothermic effect at 931 K and the enthalpy is equals to 31.35 ± 0.31 kJ/mol, which is related to the melting of Na₄V₂O₇. The high-temperature heat capacity of Na₄V₂O₇ was measured using a Multi-high temperature calorimeter 96 line and DSC. The obtained high-temperature heat capacity of Na₄V₂O₇, as a function of temperature, was modeled as: Cp=314.62+0.05T-5494390T^-2 J·mol^-1·K^-1 (298.15-873 K). The temperature dependence on heat capacity was then used for computing changes in the enthalpy, entropy, and Gibbs free energy at the specific temperature internal.     

In-situ deflectometic measurement of transparent optics in precision robotic polishing

In the ultra-precision manufacturing of large optics, industrial robots have the potential to become an intelligent and economical choice of surface polishing. However, the transport of the workpieces between the polishing platform and the measurement instrument seriously limits the manufacturing efficiency. Therefore, an in-situ measurement system based on the monoscopic deflectometry is developed to determine the form quality of the optical lenses during rough polishing. Stray light reflected from the lower surface of transparent lenses may degrade the measuring quality, thus an effective absolute phase retrieval algorithm is developed to decouple the superposed fringes associated with the upper and lower surfaces. Then, the form of the upper surface under polishing can be reconstructed to guide the subsequent polishing. Experimental results demonstrate that the accuracy of the method is comparable to that of the coordinate measuring machine, consequently the manufacturing efficiency and reliability of large optical workpieces can be greatly improved.     

Effect of spatial constraints on the phase evolution of YFeO3-based nanopowders under heat treatment of glycine-nitrate combustion products

Formation and structural transformations of yttrium orthoferrite crystals have been studied using X-ray diffractometry, Mössbauer spectroscopy and transmission electron microscopy combined with electron microdiffraction. Said processes have been studied under heat treatment of glycine-nitrate combustion products. There have been identified formations of three structural yttrium orthoferrite modifications – amorphized hexagonal <h₁>-YFeO₃ (P6₃cm) and nanocrystalline hexagonal h₂-YFeO₃ (P6₃/mmc), as well as nanocrystalline orthorhombic o-YFeO₃ (Pbnm), which are selectively formed depending on available three-dimensional confinements. Based on the analysis of changes in the fluid and size composition formulation, it has been proposed mechanism for formation and transformation of YFeO₃ nanocrystals, including growth stage of h₂-YFeO₃ crystals due to amorphized phase of <h₁>-YFeO₃ up to critical size of about 15?nm and their subsequent transformation into orthorhombic form o-YFeO₃.     

Control of aluminum phosphate coating on mullite fibers by surface modification with polyethylenimine

Aluminum phosphate (AlPO₄) is a promising oxidation-resistant and weak interface for ceramic-matrix composites. In this research, AlPO₄ coating was deposited on mullite fibers by an improved liquid-phase method based on electrostatic attraction. A cationic polyelectrolyte, polyethylenimine (PEI), was used for surface modification of mullite fibers. The formation process, phase evolution and microstructure of the coating were studied. The zeta potential of AlPO₄ particles, PEI-adsorbed AlPO₄ particles, and PEI-adsorbed mullite particles was characterized to find the proper pH value for improving electrostatic attraction. The obtained AlPO₄ coating was porous and continuous, whose thickness could be controlled by multiple coating cycles. The relatively low calcination temperature (600 or 1000 °C) was a useful heat treatment method to develop bonding between coating and fiber as well as reduce the fiber strength degradation. The phase transformations of AlPO₄ have little volume change, and cristobalite AlPO₄ is thermal compatible with mullite. Therefore, the coating structure was preserved after calcining at 1200 °C. The technique is also applicable for other fibers contained mullite phase to fabricate high-performance AlPO₄ coated mullite/mullite composites.     

Phase Field Modelling Allotropic Transformation of Solid Solution

Based on multiphase field conception and integrated with the idea of vectorvalued phase field, a phase field model for typical allotropic transformation of solid solution is proposed. The model takes the non-uniform distribution of grain boundaries of parent phase and crystal orientation into account in proper way, as being illustrated by the simulation of austenite to ferrite transformation in low carbon steel. It is found that the misorientation dependent grain boundary mobility shows strong influence on the formation of ferrite morphology comparing with the weak effect exerted by misorientation dependent grain boundary energy. The evolution of various types of grain boundaries are quantitatively characterized in terms of its respective grain boundary energy dissipation. The simulated ferrite fraction agrees well with the expectation from phase diagram, which verifies this model.     

Design of an aeronautic pitot probe with a redundant heating system incorporating phase change materials

The aim of this work is the design of a pitot probe (PP) prototype in order to retard the cool down of the tip, in case of a heating element failure. The viability of operation in flight conditions is evaluated. The design consists of a redundant heating system incorporating phase change materials (PCM). Combining experimental observations of ice formation with the implementation of the conjugate heat transfer (CHT) model, with the addition of the heat release due to the phase change of the PCM, the numerical evaluation is developed. The modelling assumptions and numerical implementation of the phase change process are presented. Then, the selection an appropriate PCM is based on the low flammability and volume dilation and the quantitative effects of the material properties on the heat transfer. A commercial PCM solution based on salt hydrates was chosen as the most adequate for the design. The parametric design of the prototype, based on the design of experiment method and fractional factorial testing, is established. A multiple linear regression model was obtained in order to maximize the cooling retardation. The numerical simulations demonstrate that the prototype PP tip temperature remains 194 s longer above 0 °C than that of the conventional model analyzed.     

Generalized phase compensator of continuous time plants

This work proposes a novel design method for generalized order lead/lag compensators. With respect to the traditional lead/lag compensator, it introduces a new parameter, β, which is a non-integer number. A new design method of the compensator is introduced in order to quantify its design parameters. Compared to its integer order counterpart, the generalized order lead compensator facilitates with the unique solution of desired design specifications with maximum phase at the desired gain cross-over frequency to achieve reshaping of the loop frequency domain characteristics. On the other hand, generalized order lag compensator is designed so as to allow minimum phase lag at the new gain crossover frequency. Examples with simulation and real-time results are presented to validate the efficacy of the proposed approach.     

Re-examination of phase relations between solid solutions in R4Al2O9-R4Si2N2O7-R4Si2O10 (R=Y,Gd, Yb) systems

Samples in Si–Al-R-O-N (R = Y, Gd, Yb) systems were prepared by solid-state reactions using R₂O₃, Al₂O₃, SiO₂ and Si₃N₄ powders as starting materials. X-ray diffraction was done to investigate RAM-J(R) solid solutions [RAM = R₄Al₂O₉, J(R) = R₄Si₂N₂O₇] formation and their equilibrium with RSO (R₄Si₂O₁₀). Phase relations between RAM, J(R) and RSO at 1700 °C were summarized in a phase diagram. It was determined that a limited solid solution of RAM and RSO could be formed along RAM-RSO tie-line, while RAM and J(R) form a continuous solid solution along RAM-J(R) tie-line. In RAM-J(R)-RSO ternary systems, the RAM-J(R) tie-lines were extended towards the RSO corner to form a continuous solid solution area of JRAMss (R = Y, Gd, Yb). The established phase relations in the Si–Al-R-O-N (R = Y, Gd, Yb) systems may facilitate compositional selections for developing JRAMss as monolithic ceramics or for SiC/Si₃N₄ based composites using the solid-solutions as a second refractory phase.