Design guidelines for titania-silica-alumina ceramics with tuned anatase to rutile transformation

Titania-based ceramics with adjustable anatase-rutile fractions were obtained by milling of anatase, quartz and corundum precursors, uniaxial pressing and firing at 1100?°C. The influence of silica and alumina, combined with milling time and compaction pressure, was studied by design of experiments. The L9 orthogonal array with a three-level noise factor was employed. Firing of pure titania at 1100?°C yielded complete anatase to rutile transformation (ART), whereas stabilized samples show that an optimum amount of 9% silica and 33% alumina reduces phase transformation to only about 5?wt% rutile. An extended correlation matrix combined with analysis of variance (ANOVA) was applied to assess the combined effects of quartz, alumina, milling time and uniaxial compressing pressure on relative density, and anatase to rutile transformation. Results show absence of ART after milling, and controlled partial conversion of anatase to rutile after firing. Very good fitting was obtained by multivariate analysis on considering first and second order terms for dependence on silica contents and interactions between silica and each of the remaining factors, including milling time. This empirical dependence could be interpreted on a sound physicochemical basis, allowing the prediction of suitable compositions and processing conditions to obtain rutile-free samples by conventional ceramic processing, and to design ceramic samples with controlled fractions of anatase and rutile.     

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.     

Producing fully-lamellar microstructure for wrought beta-gamma TiAl alloys without single α-phase field

Fine-grained fully-lamellar (FL) microstructure is desired for TiAl components to serve as compressor/turbine blades and turbocharger turbine wheels. This study deals with the process and phase transformation to produce FL microstructure for Mo stabilized beta-gamma TiAl alloys without single α-phase field. Unlike the α + γ two-phased TiAl or beta-gamma TiAl with single α-phase field, the wrought multi-phase TiAl–4/6Nb–2Mo–B/Y alloys exhibit special annealing process to obtain FL microstructure. Short-term annealing at temperatures slightly above β-transus is recommended to produce the desired FL microstructure. The related mechanism is to guarantee the sufficient diffusion homogenization of β stabilizers during single β-phase annealing, and further avoid α decomposition by α → γ + β when cooling through α + β + γ phase field. The colony boundary β phase contributes to fine-grained nearly FL microstructure, by retarding the coarsening of the α phase grains.     

Mechanical properties of graphene films enhanced by homo-telechelic functionalized polymer fillers via π–π stacking interactions

Most researches on graphene/polymer composites are focusing on improving the mechanical and electrical properties of polymers at low graphene content instead of paying attention to constructing graphene’s macroscopic structures. In current study the homo-telechelic functionalized polyethylene glycols (FPEGs) were tailored with π-orbital-rich groups (namely phenyl, pyrene and di-pyrene) via esterification reactions, which enhanced the interaction between polyethylene glycol (PEG) molecules and chemical reduced graphene oxide (RGO) sheets. The π–π stacking interactions between graphene sheets and π-orbital-rich groups endowed the composite films with enhanced tensile strength and tunable electrical conductivity. The formation of graphene network structure mediated by the FPEGs fillers via π–π stacking non-covalent interactions should account for the experimental results. The experimental investigations were also complemented with theoretical calculation using a density functional theory. Atomic force microscope (AFM), scanning electron microscope (SEM), X-ray diffraction (XRD), nuclear magnetic resonance (NMR), thermal gravimetric analysis (TGA), UV–vis and fluorescence spectroscopy were used to monitor the step-wise preparation of graphene composite films.     

Structures and properties of chicken myofibrillar protein gel induced by microwave heating

Structures and properties of myofibrillar protein gel prepared at different power (300–800 W) were evaluated. Amino acid analysis demonstrated that changes in microwave power did not alter primary structure of gel. However, an increase in microwave power could change higher structures of gel. As microwave power increased, α-helix content decreased and β-sheet content increased. Increased microwave power probably facilitated protein to unfold and expose the internal groups, causing surface hydrophobicity and the formation of disulphide bonds were enhanced, which indicated changes in tertiary and quaternary structures of protein. At 500 W, gel had the best ultrastructure where surface morphology, springiness and water holding capacity reached the optimum. Our findings suggested that microwave at an appropriate power (500 W) could change higher structures of myofibrillar protein gel to achieve desired processing and quality protein gel characteristics.     

Thermo-physical properties of as deposited and aged thermal barrier coatings (TBC) for gas turbines: State-of-the art and advanced TBCs

In the perspective of fuelling the future generations of gas turbines by hydrogen rich syngas, the evaluation of the effect of a higher water vapour content into the flue gases on the TBC used, or potentially usable, is a need. For this purpose YPSZ APS TBC with two different microstructures have been exposed for 500?h at different temperatures in the range 1000?°C–1250?°C either in air and air +20% vol. H₂O. The comparison between the different testing conditions has been performed in terms of sintering kinetics and phase stability, as evaluated by thermal diffusivity measurements and Synchrotron X-Rays diffraction, respectively. Furthermore the characterisation of thermal properties of two innovative TBCs (GZO-YPSZ and YAG) potentially able to withstand the CMAS attack and erosive environments, respectively, has been carried out.No clear evidence of a different behaviour of TBC has been observed, at least in the considered aging time and temperature range.     

Binary Ti–Fe system. Part I: Experimental investigation at high pressure

The present work illustrates the effect of quasi-hydrostatic pressure on the positions and widths of the homogeneity ranges of the intermetallic phases TiFe and TiFe₂ at high temperatures. The experiments were performed with Ti–Fe diffusion couples that were heat treated in a multi-anvil press at 2.5 GPa. The solubility limits of the phases were derived from the concentration profiles that were measured using electron probe microanalysis. It was found that the homogeneity ranges of TiFe and TiFe₂ extend to higher titanium concentrations, if the pressure is applied. The positions of the phase boundaries of the intermetallics on the iron-rich side are not affected by the pressure. The accuracy of the experimental data including the homogeneity ranges and temperatures was verified by comparing the homogeneity ranges of β-Ti(Fe), α/δ-Fe(Ti) and γ-Fe measured in this study with the homogeneity ranges taken from literature. The pressure was calibrated using the pressure-induced phase transitions of bismuth.     

古建筑木结构透榫节点力学模型研究

为研究古建筑木结构透榫节点的M-θ力学模型，在分析透榫节点构造特征与受力机理的基础上，建立其数值模型，用透榫节点的试验数据验证了该数值模型的正确性，并分析了节点缝隙、木材横纹弹性模量和大榫头长度对透榫节点受弯承载力的影响。根据受力分析结果，建立以弹性点、屈服点与极限点为特征点的三折线多参数M-θ力学模型，其结果与多数的试验结果基本吻合，并将该力学模型应用于木构架的受力分析。研究结果表明：透榫节点的滞回耗能能力强，节点的变形主要集中在榫头处。当榫头与卯口之间的缝隙增大时，节点的受弯承载力降低。随木材横纹弹性模量的提高和大榫头长度的增加，节点的受弯承载力有一定提高。文章建立的M-θ力学模型能较好反映透榫节点的受力过程，适用于木构架的受力分析，其荷载 位移骨架曲线与试验结果基本吻合。研究成果可为古建筑木结构的维修与保护提供参考。     

Optimised phase compositions and improved microwave dielectric properties based on calcium tin silicates

The Ca_(1+2y)Sn_(1-x)Si_(1+y)O_(5-2x+4y) low-permittivity microwave dielectric ceramics were prepared through solid-state reaction at 1350–1450 °C for 5 h. The relations between microwave dielectric properties and phase compositions for non-stoichiometric Ca_(1+2y)Sn_(1-x)Si_(1+y)O_(5-2x+4y) ceramics have been investigated. A single CaSnSiO₅ phase with abnormally positive temperature coefficient of resonant frequency (τ_f = + 62.5 ppm/°C) was synthesised at 1450 °C. This composition was an effective τ_f compensator of CaSiO₃ and Ca₃SnSi₂O₉ phases with typically negative τ_f value. The CaSiO₃ second phase was related to the Sn deficiency in the CaSn_(1-x)SiO_(5-2x) (0 < x < 1.0) composition, whereas the Ca₃SnSi₂O₉ second phase was obtained by controlling the Ca:Sn:Si ratios on the basis of the Ca_(1+2y)SnSi_(1+y)O_(5+4y) (0 < y < 1.0) composition. A promising low-permittivity millimetre-wave ceramic with most excellent microwave dielectric properties (ε_r = 10.2, Q×f = 81,000 GHz and τ_f = −4.8 ppm/°C) was produced from the Ca_(1+2y)SnSi_(1+y)O_(5+4y) (y = 0.4) ceramic.     

影响煤层气开发效果的地质因素再认识

地质特征认识对煤层气开发效果起着重要作用。在资源特征相差不大的情况下,发现煤层气相邻井的产量差异仍较大。排除工程因素后,通过选取8类地质参数,细致比对了保德区块低产井与邻井的参数特征,筛查出其关键因素为煤层微幅构造与顶板封盖条件,其中以微幅构造为主。据此,重新认识并划分出区块新的次生褶皱背斜单元、向斜单元和斜坡单元,获得了不同次生褶皱构造单元的开发特征。结果表明,高、低产井分布与次生褶皱背斜、向斜相关性高达92%。其中:高产井主要分布在次生褶皱背斜变化较缓、呈隆起状的“平台”,且煤层顶板以泥岩、碳质泥岩为主,封盖性较好;低产井主要分布在次生褶皱向斜,同一井台各井开发效果差异表现为从向斜条带轴部—向斜条带内—向斜条带外的煤层气井平均单井产量不断增加,到向斜轴部的距离大于向斜曲率半径73.5%的范围为主力产气区,小于向斜曲率半径40.0%范围为产水主力区。这对煤层气新井部署、生产管理、开发调整等,具有一定的指导意义。