Formation of η and σ phase in three polycrystalline superalloys and their impact on tensile properties

The formation and phase transformation mechanism of η and σ phases in three experimental polycrystalline superalloys were studied. It was shown that a high (Ti + Al) content in the alloys would favor the formation of η and σ phases in the interdendritic region. Different as-cast microstructures resulted in different phase transformation processes during heat treatment and thermal exposure. Influence of η and σ phase on tensile properties had been investigated as well. The tensile properties of the alloys were sensitive to γ′ volume fraction of the alloys, as well as morphologies of η and σ phases in the interdendritic area. Formation of plate-like η phase had negative impact on the low and intermediate temperature tensile properties of the polycrystalline superalloy.     

Investigation of α platelet boundaries in a near-α titanium alloy

Transmission electron microscopy (TEM) of a bimodal near-α titanium alloy revealed the existence of retained β phase layers and silicide precipitates at the α platelet boundaries inside transformed β grains. The β to α phase transformation accompanied by the precipitation of silicide resulted in the formation of a large number of dislocations at α platelet boundaries. Orientation relationships between silicide, β phase and α phase were also identified. However high-resolution TEM (HRTEM) revealed crystal mismatches between these phases generating high strains at α platelet boundaries. The strengthening effects of the platelet boundaries are discussed in terms of dislocations slip across the boundaries. The mechanism that governs the β to α phase transformation is also discussed.     

High temperature creep of a hot-pressed β-sialon

The four-point bending creep properties of a hot-pressed β-sialon with Sm–melilite solid solution (denoted as M′) as intergranular phase have been studied in the temperature range 1250–1350°C in air. Creep rates plotted against stresses gave stress exponents of 1.45, 1.51 and 1.72 at 1250, 1300 and 1350°C, respectively, and Arrhenius plot between creep rate and temperature yielded a creep activation energy of 576 kJ mol⁻¹. Cavities were found to be mainly on the triple grain junctions. Diffusion coupled with grain boundary sliding and accompanied by the formation of wedge-shaped cavities was identified as the dominant creep mechanism.     

α-particle emission probabilities in the decay of U

²³⁵U decays by α-particle emission to ²³¹Th. The decay scheme of this nuclide is very complex, with more than 20 alpha branches. Recommended values for P_α of this nuclide are based on measurements carried out in 1975. This work presents the results of new measurements made with Si detectors and sources of enriched uranium in the frame of the EUROMET 591 cooperation project. The use of improved measurement techniques and numerical analysis of spectra allowed a new set of P_α values for 13 lines with improved uncertainties to be obtained.     

Simultaneous determination of Np, Pu and Am in HNO3 solution by combining extraction, liquid scintillation counting, and α spectrometry

α Spectrometry is one of the most important and sensitive techniques for the assay of α-emitting nuclides, but various complicated procedures are often required for preparation of uniform thin plate source. Liquid scintillation counting (LSC) with pulse shape analysis (PSA) combining extraction is much simpler, more rapid and accurate technique, but the extraction processes are often very long. By combining extraction, LSC with PSA, and α spectrometry, we proposed a new approach to determine ²³⁷Np, ^238–240Pu and ²⁴¹Am. The new approach includes an extraction process of three steps for blind samples or of only one step for those samples without tailing interference with α spectra. Moreover, no complicated procedure is required for α plate source preparation because even non-uniform plate source is feasible for the new approach. The approach has taken advantages of high counting efficiency (nearly 100%) of LSC for α-radiation, high energy resolution of α spectrometry and high recovery yield of actinides by trialkylphosphine oxide (TRPO) extraction. The approach with one step extraction can be expected to determine ²³⁷Np, ^238–240Pu, ²⁴¹Am and ²⁴⁴Cm simultaneously.     

Effects of hydrolysis on dodecyl alcohol modified β-CaSiO3 particles and PDLLA/modified β-CaSiO3 composite films

In this research, β-CaSiO₃ particles were surface modified with dodecyl alcohol, and Poly-(DL-lactic acid) (PDLLA)/modified β-CaSiO₃ composite films were fabricated with a homogenous dispersion of β-CaSiO₃ particles in the PDLLA matrix. The aim of the study was to investigate the properties of the composite films before and after hydrolytic treatment. SEM images showed retained homogenous dispersion of β-CaSiO₃ particles after hydrolysis and tensile test also showed maintained mechanical property. Simulated body fluid (SBF) incubation experiment suggested that hydrolytic treatment did not affect the formation of hydroxyapatite on the surface of the composite films. The hydrophilicity of the composites was greatly recovered (from 69.82° to 50.28°) after hydrolysis. In addition, cells cultured on composite films after hydrolysis presented the highest cell proliferation rate and differentiation level. All of these results suggested that the surface modification of silicate particles with dodecyl alcohol along with reversible hydrolytic treatment was an effective and feasible approach to fabricate polymer/silicate composite materials with improved properties.     

Tensile behaviors of fine-grained γ-TiAl based alloys synthesized by pulse current auxiliary sintering

Micro-grained γ-TiAl based alloy obtained via pulse current auxiliary sintering exhibits good room temperature ductility with the common influence of fine grain size and inner twinning microstructure. Superplastic behavior at relatively low temperatures is also observed. It is also noted that the tensile strength of the studied alloy manifests anomalous hardening from room temperature to approximately 600 °C as a result of the controlling of dislocations slip, and softening above 600 °C due to thermal activation. Based on calculation, the superplastic deformation mechanism in the present work is determined as the grain boundary sliding accommodated by grain boundary diffusion.     

Influence of subgrain orientation on martensitic transformation in β1–Cu–Zn–Al-single crystals

In β₁–Cu–Zn–Al single crystals the course of cyclic martensititic transformation ‘β₁ parent phase↔γ′₁ martensite’ induced by tensile stress were studied with use of X-ray topography, light microscopy and etch pits. Two groups of single crystals were studied. The first one (OR) contained single crystals of subgrain boundaries parallel to the direction of elongation [001], the second one (RA) consisted of single crystals of random subgrain boundaries orientations. Single crystals from the RA group cracked after about 300 cycles of martensitic transformation; single crystals from the OR group did not crack even after 1200 cycles. In OR single crystals changes of dislocation density inside the subgrains caused by cycling occurred much more slowly than in the RA single crystals. This has been related to the dislocation movement from inside the subgrains to their boundaries.     

Effect of Ni-modified α-Al2O3 prepared by sol–gel and solvothermal methods on the characteristics and catalytic properties of Pd/α-Al2O3 catalysts

In the present study, Ni-modified α-Al₂O₃ with Ni/Al ratios of 0.3 and 0.5 were prepared by sol–gel and solvothermal method and then were impregnated with 0.3 wt.% Pd. Due to different crystallization mechanism of the two preparation methods used, addition of nickel during preparation of α-Al₂O₃ resulted in various species such as NiAl₂O₄, mixed phases between NiAl₂O₄ and α-Al₂O₃, and mixed phases between NiAl₂O₄ and NiO. As revealed by NH₃-temperature programmed desorption, formation of NiAl₂O₄ drastically reduced acidity of alumina, hence lower amounts of coke deposited during acetylene hydrogenation was found for the Ni-modified α-Al₂O₃ supported catalysts. For any given method, ethylene selectivity was improved in the order of Pd/Ni–Al₂O₃-0.5 > Pd/Ni–Al₂O₃-0.3 > Pd/Ni–Al₂O₃-0  Pd/α–Al₂O₃-commercial. When comparing the samples prepared by different techniques, the sol–gel-made samples showed better performances than the solvothermal-derived ones.     

Optoelectronic properties of β-Fe2O3 hollow nanoparticles

The effect of hollow structure on the optoelectronic properties of β-Fe₂O₃ hollow nanoparticles (HNPs) was determined. Spectrophotometry showed that the optical transmittance of the β-Fe₂O₃ HNPs was less than 40% in the visible-light region. This opaqueness was suggested to be an optical characteristic, commonly found in the authors' previous studies of TiO₂ and δ-Al₂O₃ HNPs. In addition, β-Fe₂O₃ HNPs had a band gap (1.86 eV) between amorphous (1.73 eV) and polycrystalline (1.97 eV) β-Fe₂O₃ thin films, which was a 5–7 nm thick shell that embraced an intermediate volume of the crystal phase, in-between the two thin films.     

Characterisation of blends between poly(ε-caprolactone) and polysaccharides for tissue engineering applications

In this work, bioartificial binary blends between poly(ε-caprolactone) (PCL) and a polysaccharide (chitosan (CS) or starch (S)) with different contents of the natural polymer (5–30 wt.%) were produced. Melt-mixing and double-precipitation were the methods used for the obtainment of PCL/S and PCL/CS blends, respectively. Tubular scaffolds were produced from bioartificial blends by melt-extrusion. Physico-chemical characterisation was performed by differential scanning calorimetry analysis (DSC), thermogravimetry (TGA), scanning electron microscopy (SEM), infrared analysis (FTIR-ATR and micro-ATR mapping), atomic force microscopy (AFM) and stress–strain tests. Blends were not miscible, phase-separated systems, showing a homogeneous composition and morphology only at low polysaccharide content (≤ 10 wt.%). The biocompatibility of bioartificial guides was investigated by culturing NIH-3T3 mouse fibroblasts. Cells response showed the following order: PCL/S > PCL > PCL/CS. For each blend type, biocompatibility increased with decreasing the polysaccharide content. In vitro cell tests using S5Y5 neuroblastoma cells, carried out on the most biocompatible blends, assessed their absence of cytotoxicity towards these model cells of the nervous tissue. Results showed that blends with a low chitosan or starch content (≤ 10 wt.%) are promising for the regeneration of tissues requiring tubular scaffolds, such as the peripheral nerves.     

Relationship between soil bulk density and PVR of in situ γ spectra

This paper presents the specific relationship between soil bulk density and peak-to-valley ratio (PVR) of natural radionuclides in in situ γ spectra, by theoretical deduction, Monte Carlo simulation and experimental research. Results show that for an infinite half-space volume source, PVR is a constant independent of the diverse soil bulk density. But for a limited-scale volume source, PVR would decrease slowly with an increase in soil bulk density, and the smaller the source scale, the larger the PVR variation with soil bulk density. However, the PVR variation with bulk density is very small in general. For field measurements, the volume source thickness is uncontrollable in practice, and the volume source radius should not be as small as needed for the limitation of low detection efficiency. Hence the soil bulk density could not be determined through the information from PVR of field in situ γ spectra.     

A study of tensile properties in Al–Si–Cu and Al–Si–Mg alloys: Effect of β-iron intermetallics and porosity

The effect of β-iron intermetallics and porosity on the tensile properties in cast Al–Si–Cu and Al–Si–Mg alloys were investigated for this research study, using experimental and industrial 319.2 alloys, and industrial A356.2 alloys. The results showed that the alloy ductility and ultimate tensile strength (UTS) were subject to deterioration as a result of an increase in the size of β-iron intermetallics, most noticeable up to β-iron intermetallic lengths of 100 μm in 319.2 alloys, or 70 μm in A356.2 alloys. An increase in the size of the porosity was also deleterious to alloy ductility and UTS. Although tensile properties are interpreted by means of UTS vs. log elongation plots in the present study, the properties for all sample conditions were best interpreted by means of log UTS vs. log elongation plots, where the properties increased linearly between conditions of low cooling rate–high Fe and high cooling rate–low Fe. The results are explained in terms of the β-Al₅FeSi platelet size and porosity values obtained.     

Hydrothermal synthesis and characterization of monodisperse α-Fe2O3 nanoparticles

Monodisperse α-Fe₂O₃ nanoparticles have been successfully prepared by hydrothermal synthetic route using FeCl₃, CH₃COONa as reagents and reacted at 200 °C for 12 h. The morphology and structure of products were characterized by powder X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The results showed that the α-Fe₂O₃ nanoparticles were single-crystalline hexagonal structure and average diameters were about 80 nm. Magnetic properties have been detected by a vibrating sample magnetometer at room temperature. The nanoparticles exhibited a ferromagnetic behavior with the coercive force (Hc), saturation magnetization (Ms) and remanent magnetization (Mr) was 185.28 Oe and 0.494 emu/g, 0.077 emu/g.     

The effect of volume fraction of primary α phase on fracture toughness behaviour of Timetal 834 titanium alloy under mode I and mixed mode I/III loading

The effect of volume fraction of primary α phase on mode I and mixed mode I/III fracture toughness of Timetal 834 titanium alloy was investigated. The mode I and mixed mode I/III fracture toughness values for loading angle of 30° were found to initially decrease and subsequently increase with increase in volume fraction of primary α phase. On the other hand, mixed mode I/III fracture toughness for loading angle of 45° was found to monotonically decrease with increasing volume fraction of α phase. The fracture toughness was also found to marginally increase with increasing loading angle for the two lower primary α volume fractions, i.e. 6% and 15% whereas it marginally decreases with increasing loading angle for primary α volume fraction of 30%. The results were explained on the basis of the nature of stress field ahead of the crack tip under mixed mode I/III loading as well as the fracture mechanisms operative in this alloy for different α volume fractions.     

Preparation of composite nanofibers containing gold nanoparticles by using poly(N-vinylpyrrolidone) and β- cyclodextrin

We report a new method for preparing β-cyclodextrin/poly(N-vinylpyrrolidone) composite nanofibers containing gold nanoparticles by electrospinning. β-Cyclodextrin is mixed into fibers as a new material, and it acts as stabilized reagent and reducing reagent in the synthesis of gold nanoparticles. TEM observation confirms that the gold nanoparticles are completely encapsulated within the composite nanofibers.     

Physico/chemical characterization and preliminary human histology assessment of a β-TCP particulate material for bone augmentation

This study aimed to physico/chemically characterize and evaluate the in vivo performance of a β-TCP particulate grafting material. SEM/TEM, and EDS and XPS were used for morphology and chemistry assessment, respectively. FTIR was used to determine Ca–P phases characteristic bands. Rietveld refinement/XRD spectra was performed for secondary phase detection. Particle size distribution and specific surface were assessed by a scattering-laser based technique and BET, respectively. Mercury porosimetry was employed to determine pore-size distribution. For in vivo evaluation, the grafting material was used in 12 patients' sinus lifts, and biopsies were obtained at post-operative times of 3, 6, and 9 months. SEM/TEM revealed multigrained particles with interconnected pores. EDS showed Ca, P, and O, with stoichiometry close to theoretical values. XRD/Rietveld showed that the material presented crystalline β-TCP with ~ 9% β-Ca₂P₂O₇ secondary phase. FTIR did not detect the presence of bands related to α-TCP. Human histologic assessment showed that newly formed bone was present at 3 months, and degrees of bone organization increased as time elapsed in vivo. Human histology showed that the material is suitable for bone regeneration in a maxillofacial complex region.     

Investigation of the rotary swaging and heat treatment on the behavior of W- and γ-phases in PM 92.5W–5Ni–2.5Fe–0.26Co heavy alloy

The effects of rotary swaging and different heat treatment procedures on the W- and γ-phases behavior of PM 92.5W–5Ni–2.5Fe (wt.%) heavy alloy microalloyed with cobalt have been studied. The investigation was performed on sintered and cold rotary swaged samples deformed with area reduction from 5 to 30%. One batch of swaged samples was annealed in vacuum at 1473 K for 7.2 ks and then furnace-cooled to the room temperature, whereas another batch of swaged samples was previously deformed 30% and strain aged in argon and nitrogen in the temperature range between 473 and 1123 K for 3.6 ks. Strengthening of W- and γ-phases was investigated by applying microhardness measurements. Effects of the degree of deformation, parameters of heat treatment and strain aging on microstructural changes have been studied. Mechanical properties, hardness and microhardness of phases as a function of the degree of deformation and heat treatment were analyzed by applying statistical modeling. A correlation between deformation behavior of phases, effect of heat treatment and alloy properties was also discussed.     

Preparation and phase transformation behavior of χ-alumina via solvothermal synthesis

Solvothermal reaction of aluminum isopropoxide (AIP) in mineral oil at 250–300 °C over 2 h duration provides χ-alumina powder, which transforms directly to α-alumina after calcination at high temperature. The mechanism of the crystallization process appears to be the initial formation of a spherical complex which subsequently decomposes further to precipitate a solid. This mechanism is suggested by XRD, IR, TG/DTA, SEM and TEM characterization of the powder formed. χ-Alumina attains a critical crystallite size around 15 nm through accretion on calcination and then transforms directly to α-alumina through nucleation and growth process. Direct α-phase transformation of χ-alumina powders rather than passage through κ-alumina can be explained by the absence of the cation contamination and the higher crystallinity of χ-alumina in the AIP decomposition process.     

PPCO: polarization–polarization correlation from oriented nuclei

The correlation between linear polarization of one γ-ray quantum and polarization of the next γ-ray quantum emitted in a cascade from an oriented nucleus is discussed. This correlation forms the basis for developing the PPCO method which, in principle, can determine spins, parities and multipolarities. The method is particularly useful when γ rays are produced in heavy ion reactions, ensuring a high spin alignment. The paper presents an experimental test of the PPCO method and the results suggest, that this method can be applied with success in modern γ-ray spectroscopy in which a large number of detectors are sensitive to the polarization (e.g. the CLOVER detectors). When this method is combined with an angular correlation analysis, the number of the possibilities concerning spins, parities and multipolarity sequences can be reduced significantly.