Effects of microalloying with Cd and Ag on the precipitation process of Al–4Cu–0.3Mg (wt%) alloy at 200°C

The present work investigates the effects of individual and combined additions of Cd and Ag on precipitation processes in an Al–4Cu–0.3Mg (wt%) alloy. Analytical scanning transmission electron microscopy revealed that microalloying with Cd stimulates nucleation of θ′ phase on {001} planes and that Cd-rich particles form on the rim and broad facets of the θ′ platelets. We interpret these observations to suggest that Cd nucleates heterogeneously at the θ′– interface and that θ′ can also nucleate heterogeneously at the Cd– interface. In the quinary alloy, it was observed that Ag and Cd additions seem to work independently resulting in a fine and uniform dispersion of both Ω and θ′. Furthermore, the hardening effect of the {111} Ω phase appears to be more potent than other precipitates formed in this system since the hardness of the quinary alloy was intermediate between the Al–Cu–Mg–Ag and the Al–Cu–Cd alloys.     

A TEM study of precipitation in Al–Mg–Si alloys

A set of extrusion samples of Al–Si–Mg alloys (0.5 wt%Mg and 0.3–0.8 wt%Si) were, respectively, T1- and T4-heat-treated. Differential scanning calorimetry (DSC) was used to heat the samples to particular temperatures to promote the formation of precipitates for study by transmission electron microscopy (TEM). It was found that, apart from β″, β′, and B′, there were many precipitates showing rectangular lattices when viewed along the long axes of the precipitates. It is considered that the residual stresses (or dislocations) in the extrusion after the T1-treatment facilitated the nucleation and growth of the precipitates during the heating in the DSC.     

On the pp → ppη(η′) reactions near threshold

The production rate for η′ in pp → ppη′ at rest is calculated in a covariant one boson exchange model, previously applied to study π⁰ and η production in NN collisions. The transition amplitudes for the elementary BN → η′N processes with B being the meson exchanged (B = π, σ, η, , ω and a₀) are taken to be the sum of s- and u-channels with a nucleon in the intermediate states, and an a₀ meson pole in a t-channel. The couplings of the η′ to hadrons are a factor 0.4 weaker than the respective η-hadron couplings, as suggested by a quark model and a singlet-octet mixing angle θ = −23°. The model reproduces near threshold cross sections for the quasielastic processes π⁻p → nη(η′) and pp → ppη(η′) reactions.     

Fabrication and growth rate estimation of PrBa2Cu3O7−δ single crystal by the modified top seeded crystal pulling method

Recently, we succeeded in fabricating single crystals of PrBa₂Cu₃O_7−δ by a modified top seeded crystal pulling method called the SRL-CP (Solute Rich Liquid-Crystal Pulling) method. Y₂O₃ and MgO polycrystalline crucibles and a MgO single crystal crucible were used to grow the single crystals. The crystal growth temperature was set in the range of 968°C to 972°C. The grown crystals were identified as PrBa₂Cu₃O_7−δ by X-ray diffraction. In the case of using Y₂O₃ crucibles the composition of the grown crystals was Y_xPr_1−xBa₂Cu₃O_7−δ (0.48 < x < 0.57) and in the case of using MgO crucibles a relatively small amount of Mg contamination to the grown crystals occurred at a typical concentration of approximately 1 at.% of the sum of cations. According to the crystal growth model of the SRL-CP method [1–5], a maximum growth rate of 1.7 × 10⁻⁵ cm/s was calculated with the aid of the phase diagram studies we reported earlier [6]. This value is reasonably in agreement with the experimental results.     

Surface structure evolution during Sb adsorption on Si(1 1 1)–In(4×1) reconstruction

The Sb adsorption process on the Si(1 1 1)–In(4×1) surface phase was studied in the temperature range 200–400 °C. The formation of a Si(1 1 1)–InSb (2×2) structure was observed between 0.5 and 0.7 ML of Sb. This reconstruction decomposes when the Sb coverage approaches 1 ML and Sb atoms rearrange to and (2×1) reconstructions; released In atoms agglomerate into islands of irregular shapes. During the phase transition process from InSb(2×2) to Sb (θ_Sb>0.7 ML), we observed the formation of a metastable (4×2) structure. Possible atomic arrangements of the InSb(2×2) and metastable (4×2) phases were discussed.     

Effects of substitution of Ti for Fe in BiFeO3 films prepared by sol–gel process

Ti substituted BiFe_1−xTi_xO_3+δ films have been prepared on indium–tin oxide (ITO)/glass substrates by the sol–gel process. The films with x=0.00–0.20 were prepared at an annealing temperature of 600 °C. X-ray diffraction patterns indicate that all films adopt R3m structure and the films with x=0 and 0.10 show pure perovskite phase. Cross-section scanning shows the thickness of the films is about 300 nm. Through 0.05 Ti substitution, the 2P_r increases to 8.30 μC/cm² from 2.12 μC/cm² of the un-substituted BiFeO₃ film and show enhanced ferroelectricity at room temperature. The 2P_r values are 2.63 and 0.44 μC/cm² for the films with x=0.01 and 0.2, respectively. Moreover, the films with x=0.05 and 0.10 show enhanced dielectric property since the permittivity increases near 150 at the same measuring frequency. Through the substitution of Ti, the leakage conduction is reduced for the films with x=0.05–0.20.     

Contributions of atom probe tomography to the understanding of nickel-based superalloys

Atom probe tomography enables atomic level microstructural characterization to be performed on complex engineering materials such as superalloys. The technique provides information on the size, morphology and compositions of coexisting phases, the solute partitioning of the elements between the phases, and solute segregation to interfaces and grain boundaries. This information leads to a more complete understanding of nickel-based superalloys. The types of atomic level information that may be obtained with atom probe tomography are illustrated with examples of the formation of fine γ precipitates within the central region of the γ′ phase in PW 1480, the evolution of the dual γ′/γ″ nature of secondary precipitates in alloy 718, the interphase precipitation of the γ′ phase at the primary γ″–γ interface in alloy 718, and the quantification of the level and spatial extent of the boron segregation at grain boundaries in a nickel–molybdenum superalloy.     

Compton scattering by the proton through θcms = 75° and 90° in the Δ-resonance region

Differential cross sections for Compton scattering by the proton have been measured in the energy interval between 200 and 500 MeV at scattering angles of θcms = 75° and θcms = 90° using the CATS, the CATS/TRAJAN, and the COPP setups with the Glasgow Tagger at MAMI (Mainz). The data are compared with predictions from dispersion theory using photo-meson amplitudes from the recent VPI solution SM95. The experiment and the theoretical procedure are described in detail. It is found that the experiment and predictions are in agreement as far as the energy dependence of the differential cross sections in the Δ-range is concerned. However, there is evidence that a scaling down of the resonance part of the M1+3/2 photo-meson amplitude by (2.8 ± 0.9)% is required in comparison with the VPI analysis. The deduced value of the M1+3/2-photoproduction amplitude at the resonance energy of 320 MeV is: |M1+3/2| = (39.6 ± 0.4) × 10−3 mπ+−1.     

Fabrication of p-Si/β-FeSi2 balls/n-si structures by MBE and their electrical and optical properties

We report on the formation technique of single-crystalline β-FeSi₂ balls (<100 nm) embedded in a Si p–n junction region by Si molecular beam epitaxy (MBE). β-FeSi₂ films grown on Si (0 0 1) by reactive deposition epitaxy (RDE) aggregated into islands after annealing at 850°C in ultrahigh vacuum. The islands of β-FeSi₂ aggregated further into a ball shape by following the Si MBE overgrowth at 750°C. It was found from X-ray diffraction (XRD) patterns that the epitaxial relationship between the two materials, and single-crystalline nature were preserved even after the annealing and the Si overgrowth. Capacitance–voltage (C–V) characteristics and transmission electron microscope (TEM) images revealed that a lot of defects were introduced around the embedded β-FeSi₂ balls with an increase of embedded β-FeSi₂ quantity.     

Correlation between structural and optical properties of ion beam synthesized β-FeSi2 precipitates in Si

The structural and optical properties of β-FeSi₂ precipitates produced by ion beam synthesis have been investigated by transmission electron microscopy, photoluminescence (PL) analysis and near infrared transmission measurements. The PL spectrum of β-FeSi₂ precipitates in a dislocation free sample has been observed to consist of a sharp line at 1.54 μm and a weak peak at 1.46 μm. Optical transmission measurements showed a direct band gap about 0.8 eV smaller than in continuous β-FeSi₂ film. Calculation of the electronic bands of β-FeSi₂ for different values of the lattice parameters indicates that this reduction can be ascribed to band distortion provided by the lattice strain.     

Exploring the reaction mechanism of eta prime photoproduction

We examine theoretical implications of studying the differential cross-section and some key polarization observables in the η′ photoproduction reaction off protons, from its threshold to about 2 GeV of cm energy, the region of the so-called “missing baryon resonances”. We compare implications of different models all of which generate the observed peak in the total η′ photproduction cross section, but have very different differential cross section and polarization profields. Their measurements are thus crucial in distinguishing these reaction mechanisms, of interest to understanding QCD in its nonperturbative domain.     

Detection of Au precipitates in a Mg-based alloy using electronically simulated hollow cone illumination

Images from electronically simulated hollow cone illumination (or rotating dark field) conditions, obtained under plane wave (or weak) diffraction conditions, are generally assumed to approximate to the compositionally weighted sum of atomic number squared for sufficiently large momentum transfers. However, even for large momentum transfer encountered with a semi-angle of 5° and 300 keV electrons, appropriate numerical integration over condenser and objective aperture configurations indicates that some thermal scattering component is still present. A Mg–Al alloy with minor additions of Zn and Mn, and to which 0.1 at.% Au has been added, is shown to provide a good system for the detection of high Z (atomic number) precipitates within a low Z matrix and on which semi-quantitative calculations may be based. Correlation of absolute rather than relative intensities from small precipitates (3–10 nm diameter) with calculations based on an Einstein model for (incoherent) thermal diffuse scattering show that the small precipitates consist predominantly of Au, a conclusion subsequently supported by EDX analysis and electron diffraction measurements. It is also demonstrated that this incoherent contrast mechanism is ideal for stereographic imaging in the TEM.     

In vitro fibrillogenesis of the amyloid beta 1-42 peptide: cholesterol potentiation and aspirin inhibition

Understanding the formation of extracellular amyloid neurofibrillar bundles/senile plaques and their role in the development of Alzheimer's disease is of considerable interest to neuroscientists and clinicians. Major components of the extracellular neurofibrillar bundles are polymerized amyloid β (Aβ) peptides (1–40), (1–42) and (1–43), derived in vivo from the soluble amyloid precursor protein (sAPP) by proteolytic (β- and γ-secretase) cleavage. The Aβ_1–42 peptide is widely considered to be of greatest significance in relation to the pathogenesis of Alzheimer's disease. A well-defined ultrastructural characteristic within Alzheimer dense plaques is the presence of helical fibrils that are believed to consist of polymerized amyloid β, together with other associated proteins such as the serum amyloid P protein, apolipoprotein E isoform epsilon 4, 1-anti-chymotrypsin, catalase, glycoproteins, proteoglycans, cholesterol and other lipids. The spontaneous in vitro fibrillogenesis of chemically synthesized Aβ_1–42 peptide (rat sequence), following 20 h incubation at 37 °C, has been assessed from uranyl acetate negatively stained specimens studied by transmission electron microscopy (TEM). Amyloid β_1–42 peptide fibrillogenesis in the presence of cholesterol has been investigated using aqueous suspensions of microcrystalline cholesterol and cholesteryl acetate, globular particles of cholesteryl oleate, a soluble (micellar) cholesterol derivative (polyoxyethyl cholesteryl sebacate/cholesteryl PEG 600 sebacate), cholesterol–sphingomyelin liposomes and sphingomyelin liposomes. In all these cases, with the exception of cholesteryl oleate, considerable potentiation of long smooth helical fibril formation occurred, compared to 20 h 37 °C control samples containing the Aβ_1–42 peptide alone. The binding of polyoxyethyl cholesteryl sebacate micelles to helical Aβ fibrils/filaments and the binding of fibrils to the surface of cholesterol and cholesteryl acetate microcrystals, and to a lesser extent on cholesteryl oleate globules, indicates an affinity of the Aβ peptide for cholesterol. This potentiation of Aβ_1–42 polymerization is likely to be mediated at the molecular level via hydrophobic interaction between the amino acid side chains of the peptide and the tetracyclic sterol nucleus. Addition of cupric sulphate (0.1 mM) to the Aβ solution produced large disorganized fibril aggregates. Inclusion of 1 mM aspirin (sodium acetylsalicylate) in the Aβ peptide alone and as an addition to Aβ peptide solution containing cholesterol, cholesteryl acetate, soluble cholesterol, sphingomyelin and sphingomyelin–cholesterol liposomes, and to 0.1 mM cupric sulphate solution, completely inhibited fibrillogenesis. Instead, only non-crystalline diffuse, non-filamentous microaggregates of insoluble Aβ particles were found, free and attached to the sterol particles. The in vitro system presented here provides a way to rapidly monitor at the structural/TEM level other compounds (e.g. chelating agents, drugs, β-sheet breaking peptides and anti-oxidants) for their effects on amyloid β peptide fibrillogenesis (and on preformed fibril disassembly) in parallel with in vitro biochemical studies and in vivo studies using animal models of Alzheimer's disease as well as studies on man.     

Solid-state synthesis of potassium β- and β″-gallates

Direct synthesis of K-β- and β″-gallates by Ga₂O₃–K₂O solid-state reaction is described. The formation of K-β- or β″-gallates depends on the initial Ga₂O₃ phase. -Ga₂O₃ leads to K-β-gallate; β-Ga₂O₃ leads to K-β″-gallate. K-β″-Gallate is stable <1200°C. The high temperature stability of K-β″-gallate can be enhanced by doping with aliovalent ions.     

Study of the interfacial structure and chemistry of CVD κ-Al2O3/TiC multilayer coatings

This article describes the interfacial regions in CVD grown TiC/κ-Al₂O₃ multilayers. A number of microanalytical techniques were used including HREM, EDX and EELS. Occasionally, the first 50 nm of the alumina layers deposited on the intermediate TiC layers grew as a cubic alumina, heavily faulted, containing small amounts of sulphur (S), maybe as a stabiliser. The presence of slightly rounded TiC (111) facets may act as preferred nucleation sites for the cubic Al₂O₃ phase, with a ‘cube on cube’ orientation relationship. In this way the nucleation of κ-Al₂O₃ is less favourable. After some tens of nanometres the cubic phase cannot be stabilised any longer and the layer continues to grow as κ-Al₂O₃. A number of observations point towards the reaction zone (RZ) being η- and/or γ-Al₂O₃. The diffraction work and the FFT analysis of the HREM images show that the RZ is an fcc phase with a=7.9 Å, which matches with η- and γ-Al₂O₃. The EELS Al fine structure indicate more tetrahedral Al ions than in κ-Al₂O₃, as in η- and γ-Al₂O₃. The RZ contains small amounts of S, as has been reported for γ-Al₂O₃. Due to the structural similarities between η- and γ-Al₂O₃ it was not possible to determine which of these cubic phases is present in the RZ.     

Coexisting antiferromagnetism and ferromagnetism in mechanically alloyed Fe-rich Fe–Ni alloys: implications regarding the Fe–Ni phase diagram below 400°C

Fe–Ni alloys below the Invar region with compositions Fe_100−xNi_x (x=21, 24, and 27 at%) were prepared by high-energy ball milling technique (mechanical alloying). The as-milled samples, characterized by X-ray diffraction and Mössbauer spectroscopy, contain a mixture of (BCC) and γ (FCC) phases, whereas the samples annealed at 650°C for 0.5 h show a single γ (FCC) phase displaying a single line Mössbauer spectrum at room temperature (RT). At low temperature, the Mössbauer spectra of annealed Fe₇₆Ni₂₄ and Fe₇₃Ni₂₇ alloys show the existence of a magnetically split pattern together with a broad singlet, which are ascribed to a high-moment ferromagnetic Ni-rich phase and a low-moment Fe-rich phase, respectively. The Fe-rich phase in annealed Fe₇₆Ni₂₄ alloy, which is paramagnetic at RT, undergoes antiferromagnetic ordering at 40 K, estimated from the dramatic line broadening of its spectrum, giving rise to a small hyperfine field (e.g. 2 T at 6 K). The coexistence of these phases is attributed to phase segregation occurring in these alloys as a result of enhanced atomic diffusion. The stability of these alloys towards martensitic (FCC→BCC) transformation at low temperatures is discussed in connection with the Fe–Ni phase diagram below 400°C.     

The IR spectra of Mg5C(CO) complexes on the (0 0 1) surfaces of polycrystalline and single crystal MgO

The FTIR spectroscopy of carbon monoxide adsorbed on polycrystalline MgO smoke has been investigated as a function of the CO equilibrium pressure at constant temperature (60 K) (optical isotherm) and of the temperature (in the 300–60 K range) at constant CO pressure (optical isobar). In both cases the spectra fully reproduce those of CO adsorbed on the (0 0 1) surface of UHV cleaved single crystals [Heidberg et al., Surf. Sci. 331–333 (1995) 1467]. This result, never attained in previous investigations on dispersed MgO, contribute to bridging the gap which is commonly supposed to exist between surface science and the study of “real” (defective) systems. Depending on the surface coverage θ the main spectral features due to the CO/MgO smoke interaction are a single band shifting from 2157.5 (at θ→0) to 2150.2 cm⁻¹ (at θ=1/4) or a triplet, at 2151.5, 2137.2 and 2132.4 cm⁻¹ (at θ>1/4). These manifestations are due to the ν(CO) modes of Mg_5C²⁺· · · CO adducts formed on the (0 0 1) terminations of the cubic MgO smoke microcrystals. The formation of the CO monolayer is occurring in two different phases: (i) a first phase with CO oscillators perpendicularly oriented to the surface (2157–2150 cm⁻¹) and (ii) a second phase constituted by an array of coexisting perpendicular and tilted species (triplet at 2151.5, 2137.2 and 2132.4 cm⁻¹). A much weaker feature at 2167.5–2164 cm⁻¹ is assigned to Mg_4C²⁺· · · CO adducts at the edges of the microcrystals. The heat of adsorption of the perpendicular Mg_5C²⁺· · · CO complex in the first phase has been estimated from the optical isobar and results to be 11 kJ mol⁻¹.     

An evaluation of surface properties and frictional forces generated from Al–Mo–Ni coating on piston ring

Surface properties of the Al–Mo–Ni coating plasma sprayed on the piston ring material and the frictional forces obtained by testing carried out under different loads, temperatures and frictional conditions were evaluated.

Al–Mo–Ni composite material was deposited on the AISI 440C test steel using plasma spraying method. The coated and uncoated samples were tested by being exposed to frictional testing under dry and lubricated conditions. Test temperatures of 25, 100, 200, and 300 °C and loads of 83, 100, 200, and 300 N were applied during the tests in order to obtain the frictional response of the coating under conditions similar to real piston ring/cylinder friction conditions. Gray cast iron was used as a counterface material. All the tests were carried out with a constant sliding speed of 1 m/s.

The properties of the coating were determined by using EDX and SEM analyses. Hardness distribution on the cross-section of the coating was also determined. In addition, the variations of the surface roughness after testing with test temperatures and loads under dry and lubricated conditions were recorded versus sliding distance.

It was determined that the surface roughness increased with increasing loads. It increased with temperature up to 200 °C and then decreased at 300 °C under dry test conditions.

Under lubricated conditions, the roughness decreased under the loads of 100 N and then increased. The roughness decreased at 200 °C but below and above this point it increased with the test temperature.

Frictional forces observed under dry and lubricated test conditions increased with load at running-in period of the sliding. The steady-state period was then established with the sliding distance as a normal situation. However, the frictional forces were generally lower at a higher test temperature than those at a lower test temperature. Surprisingly, the test temperature of 200 °C was a critical point for frictional forces and surface roughness.     

Hardening nanostructures in an AlZnMg alloy

The formation of nanoscale and sub-nanoscale solute aggregates (clusters, Guinier–Preston zones and precipitates) in an AlZnMg alloy (Al–2.1 at.% Zn–1.5 at.% Mg) has been followed by a combination of experimental techniques with the aim of correlating the properties of the aggregates with their thermal history. The choice of thermal treatments was guided by the results of mechanical and calorimetric characterizations, supported by transmission electron microscopy for the identification of the morphology of the aggregates. Positron annihilation spectroscopy (using two variants of this technique, coincidence Doppler broadening and lifetime spectroscopy) was adopted for determining the local chemistry in the proximity of open volume defects. The geometrical parameters of the distribution (size, volume fraction, numerical density of the solute aggregates) were obtained by small-angle X-ray scattering. The results of the investigation provide new information regarding: two families of vacancy-rich clusters formed during or immediately after quenching; Guinier–Preston zones formed at 95°C after room-temperature pre-ageing; growth of η′ and?η?phases at 150°C; solute clusters formed at room-temperature in conditions of secondary ageing after preliminary heating at 150°C.     

Luminescence from γ-irradiated humic acid

This study was conducted to investigate the ultraweak delayed radiochemiluminescence (RCL) spectra, kinetics and spectroscopic properties of humic acids (HAs) after γ-radiation exposure (absorbed doses of 1−10 kGy, Co-60) in model systems.

The kinetics and spectral distribution of RCL (340–650 nm) were measured using the single photon counting (SPC) method and cut-off filters.

The intensity of fluorescence (λ_ex=390, 440, 490 and 540 nm) covering the spectral range 400–580 nm was heavily dependent on the λ_ex and slightly increased with the absorbed dose of γ-radiation.

Absorption spectra (the range 240−800 nm) and color coefficients E_2.6/4 and E_4/6 of irradiated solutions indicated that post-radiative degradation/polymerization processes take place in the HA, changing their macromolecule size or properties.

Comparison of FTIR spectra and elemental analysis proved an increased O and decreased C atoms in irradiated samples. The data indicate on the radiolysis-induced degradation of native HA into fulvic-like acids with higher hydrophilicity and lower molecular size.