Effect of superplastic deformation on the grain size and tensile properties of Al-6.2Zn-2.5Mg-1.7Cu (7010) alloy sheet

An Al-Zn-Mg alloy (7010) was cold-rolled and annealed to produce a small recrystallized grain size, and superplastically deformed in the temperature range 475 to 520° C at strain rates to 2.8×10^–3 sec^–1. At 500° C and sec^–1 superplastic elongations up to 350% were obtained, but above about 60% elongation the residual room-temperature tensile properties after heat treatment decreased due to increasing grain-boundary cavitation. Grain growth rates were increased by superplastic strain.     

Superconductivity of YBa2?xNdxCu3Oy Solid Solution

The solubility of Nd at the Ba sites and the superconductivity of YBa_2–x Nd _x Cu₃O _y were investigated by X-ray powder diffraction and measurements of the electrical resistance and ac susceptibility. The single Re123 phase was obtained for x0.30. The onset transition temperature is insensitive to the Nd content x in the region of x0.40. All are higher than 95 K. The zero resistance transition temperatures , however, exhibits two-step variation with the increase of x. For x0.25, are all above 92 K. The highest of 94 K was obtained for x=0.25. For x0.3 drops sharply to about 84 K. Finally falls to 30 K and is below 10 K for x=0.5. The two-step variation of T _c might be an indication of the existence of two trap levels for holes.     

Size effects and ductile-brittle transition of polypropylene

The influence of specimen width on fracture parameters has been investigated. The range examined was sufficiently large to obtain ductile and brittle fractures. With reference to previously published work, the phenomenology has been analysed by combining BCS model and Carpinteri's brittleness number approach.Nomenclature a crack length - f(a/W) shape function according to ASTM specification [16] - F(a/W) shape function according to Tada Paris notation [21] - E elastic modulus - K _IC plane strain fracture toughness - K _IC ^f fictitious plane strain fracture toughness - K _IC2 plane stress fracture toughness - J _IC ^f J-integral at maximum load - L span - weight average molecular weight - number average molecular weight - polydispersity - P _M maximum load - P _F load of brittle fracture - p _P load of plastic collapse - s brittleness number - V machine cross speed - W specimen width - _y yield stress - strain rate     

Three oxidation states and atomic-scale <Emphasis Type="Italic">p–n</Emphasis> junctions in manganese perovskite oxide from hydrothermal systems

Perovskite oxides have provided magical structural models for superconducting and colossal magnetoresistance, and the search for nano-scale and/or atomic-scale devices with particular property by specific preparations in the same systems has been extensively conducted. We present here the three oxidation states of manganese (Mn³⁺, Mn⁴⁺, Mn⁵⁺) in the perovskite oxide, La_0.66Ca_0.29K_0.05MnO₃, which most interestingly shows the rectifying effect as atomic-scale p–n junctions (namely FY-Junctions) of single crystals and films. The family of cubic perovskite oxides were synthesised by the so-called hydrothermal disproportionation reaction of MnO₂ under the condition of strong alkali media. The new concept of the atomic-scale p–n junctions, based on the ideal rectification characteristic of the p–n junctions in the single crystal, basically originates from the structural linkages of [Mn³⁺–O–Mn⁴⁺–O–Mn⁵⁺], where Mn³⁺ and Mn⁵⁺ in octahedral symmetry serve as a donor and an acceptor, respectively, corresponding to the localized Mn⁴⁺ .     

Rigid body translation in the (\bar 211) twin boundary in silicon

The rigid body translation accompanying a ( 11) twin boundary in silicon has been studied by transmission electron microscopy. From a detailed analysis of theα-type fringe systems in the 111, 311 and 2 0 common reflections, the following translation vector is deduced: [011], which is equivalent to [411] in the other crystal element. A slight deviation of this orientation is possible.     

Luminescence of SrAl<Subscript>2</Subscript>O<Subscript>4</Subscript>:Cr<Superscript>3+</Superscript>

Samples of SrAl₂O₄ and SrAl₂O₄:Cr³⁺ were prepared by mixing the powder materials SrCO₃, Al₂O₃, and Cr₂O₃. The crystal structures of the undoped and doped samples were analyzed by X-ray diffraction (XRD) measurements. The diffraction patterns reveal a dominant phase, characteristic of the monoclinic SrAl₂O₄ compound and another unknown secondary phase, in small amount, for doped samples. The data were fitted using the Rietveld method for structural refinements and lattice parameter constants (a, b, c, and β) were determined. Luminescence of Cr³⁺ ions in this host is investigated for the first time by excitation and emission spectroscopy at room temperature. Emission spectra present a larger band and a smaller structure associated to the and electronic transitions, respectively. The obtained results are analyzed by crystal-field theory and the crystal-field parameter, Dq, and Racah parameters, B and C, are determined from the excitation measurements.     

Determination of standard Gibbs energies of formation of ternary oxides in the system Co-Sb-O by solid electrolyte emf method

An isothermal section of the phase diagram of the system Co-Sb-O at 873 K was established by isothermal equilibration and XRD analyses of quenched samples. The following galvanic cells were designed to measure the Gibbs energies of formation of the three ternary oxides namely CoSb₂O₄, Co₇Sb₂O₁₂ and CoSb₂O₆ present in the system.

Interface structure and strain development during compression tests of Al2O3/Nb/Al2O3 sandwiches

The interface structure of an Al₂O₃/Nb/Al₂O₃ sandwich produced by solid-state diffusion bonding was investigated in detail by various transmission electron microscopy (TEM) methods. The joint possessed at one interface a , , and on the other interface a and orientation relationship. At both interfaces, misfit dislocations formed to compensate the lattice mismatch as found by high-resolution transmission electron microscopy (HRTEM). Electron energy-loss near edge structure (ELNES) studies revealed that the interface is terminating with an Al layer resulting in Al–Nb bonds. Identical sandwiches were investigated on the meso- and macroscopic scale by performing compression tests and simultaneously monitoring the strain development at (001)_Nb and crystal faces. The full-field optical strain measurements (FFOM) revealed that the strain is localized at the interfaces when observed at the (001)_Nb face while it is along the maximum shear directions of 36–54° inclined to the interface when observed at the face. The strain localization along a specific maximum shear direction results in the cleavage of Al₂O₃, always initiating from the interface possessing the and orientation relationship.     

Structural properties of nickel manganite Ni x Mn3−x O4 with 0.5 ⩽x ⩽ 1

Single-phase nickel manganite spinels, Ni _x Mn_3–x O₄, with 0.5 x 1, were prepared by a careful thermal processing of nickel-manganese coprecipitated oxalate precursors. Powder X-ray diffraction analysis of the spinel revealed the presence of cubic single spinel phase with parametera which decreases with nickel content. The lattice parameter variation can be explained in terms of the distribution of Ni²⁺ ions on the octahedral sites. Therefore, a fine analysis of data shows that some Ni²⁺ ions (forx>0.56) are located in tetrahedral sites. The percentage of nickel in A-sites increases with nickel content (x) following the relation % Ni²⁺ in A sites =P = – 82.1x ²+192.4x–81.5 and thus the general formula for cation distribution is

Effect of gas composition on Si2N2O formation in the Si-C-N-O system

Formation of silicon oxynitride was observed during silicon nitride whisker synthesis from silica, carbon and nitrogen. The silicon oxynitride formation was limited to a bottom area of the charged powders and found both in whisker and powder. The possible reason for this localized Si₂N₂O formation is analysed, based on the effect of gas phase composition on the phase stability among β-Si₃N₄, β-SiC and Si₂N₂O. The phase stability is closely related to the ratio in the gas phase. To suppress Si₂N₂O formation, the ratio must be lower than that of the phase boundary in the Si₂N₄/Si₂N₂O equilibrium, whereas it must be higher than that of the phase boundary in the SiC/Si₂N₂O equilibrium. The formation of silicon oxynitride during silicon nitride whisker formation was caused most likely by fluctuation in the ratio in the gas phase surrounding the lower area.     

The interface microstructure in alumina (FP) fibre/magnesium alloy composite

The objective of this work was to characterize the interfacial reaction zone in the metal matrix composite system-Al₂O₃(FP)/Mg (ZE41A). The composite was fabricated by liquid infiltration method. The reaction zone, a result of the reaction between magnesium in the alloy and the alumina fibres, was analysed for its morphology, chemistry, and crystallographic orientation using transmission electron microscopy. The results of this study showed the reaction zone to be, on average, 100nm wide and composed of MgO. The grains of the reaction zone ranged from less than 10 nm at the fibre/reaction zone interface to greater than 100nm at the matrix/reaction zone interface. It is proposed that the growth of the reaction zone was controlled by a seepage mechanism involving infiltration of liquid magnesium between MgO crystalS. Finally, it was observed that the MgO grains have the following crystallographic orientation relationship with the alumina grains from which they grew:

Electrical, magnetic and Mössbauer properties of cadmium - cobalt ferrites prepared by the tartarate precursor method

Six samples of the system Cd_1–x Co _x Fe₂O₄ were prepared by the tartarate precursor method with x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0. The formation of ferrispinels were studied by X-ray powder diffraction, infrared spectroscopy, electrical conductivity, thermoelectric power, magnetic hysteresis, initial magnetic susceptibility and Mössbauer spectroscopy. The data of the temperature variation of the direct current electrical conductivity showed a definite kink (390°C) except x = 0.0 and 0.2, which corresponds to the ferrimagnetic to paramagnetic transitions. Magnetic properties of the samples with x 0.6 showed definite hysteresis loops. The observed low magnetic moment can be explained in terms of the non collinear spin arrangement. A well defined hyperfine Zeeman spectra are observed for samples with x 0.6 at room temperature and resolved into two sextets corresponding to octahedral and tetrahedral sites. The electrical, magnetic and Mössbauer properties suggest that, a canted spin arrangement upto x = 0.8 and Néel's configuration above this composition. The probable ionic configuration for the system is suggested as

Electrical conductivity in non-stoichiometric titanium dioxide at elevated temperatures

The electrical conductivity of polycrystalline titanium dioxide prepared by a liquid mix technique was measured for the oxygen partial pressure range of 10° to 10^–19 atm and temperature range of 850 to 1050° C. The data were found to be proportional to the –1/6 power of oxygen partial pressure for the oxygen pressure range 10^–19 to 10^–15 atm, and proportional to for the oxygen pressure range >10^–15 atm. The region of linearity where the electrical conductivity varied as the –1/4 power of increased as the temperature was decreased. There was evidence of p-type behaviour for 10^{ - 2}$$ " align="middle" border="0"> atm in the temperature range 950 to 850° C, although the measured data were insufficient to assign a pressure dependence. Electrical conductivity minima in the log against log plot moved to lower as the temperature was decreased in the range 950 to 850° C. The measured oxygen pressure dependence of electrical conductivity in the lowest region supports the oxygen vacancy defect model. The observed data are consistent with the presence of very small amounts of acceptor impurities. A binding energy of 0.67 eV between the acceptor impurity and its compensating oxygen vacancy was also determined.     

Effect of non-stoichiometry on the sintering of doped TiO2

The sintering of TiO₂ has been studied with respect to oxygen partial pressure ( ) and doping content. From the microstructural evolution, it is obvious that a decrease of the oxygen pressure promotes the densification with a comparatively smaller grain growth than in air sintering. This fact has been related with the influence of defects on the sintering. Both effects of and tantalum doping have been studied. They are interpreted on the basis of a model involving interstitial titanium, electron holes, titanium vacancies and complexes associating titanium vacancies with tantalum substituted titanium. This latter complex is probable according to previous microscopic studies of defects in TiO_2–x and may be important in highly doped compounds. The formation of such associates reduces the mobile defect concentration, however a decrease of the favour their dissociation. The titanium vacancies which are thus released allow the titanium ions to migrate, a necessary condition for the sintering.     

Study on the behavior of elastic-plastic fracture under mixed I+II mode loading in aluminum alloy Ly12-J-integral analysis

The elastic-plastic fracture behavior of aluminum alloy Ly12 under mixed I+II mode loading was studied by finite element method and fracture test. A mixed mode elastic-plastic fracture criterion of J-integral was proposed by using the J-resistance curve, and the maximum fracture effective plastic strain _p max of different mixed ratios at crack tip were also calculated. The results show that(1) the initiation J-integral values of different mixed ratios have the equation

Effect of magnetic iron impurity on the superconducting properties of an amorphous Nb50Zr35Si15 alloy

The effect of magnetic iron impurity on the superconducting properties of amorphous Nb₅₀Zr_35−x Si₁₅Fe _x (x⩽4 at %) alloys was examined. Doping with an iron impurity resulted in a linear depression ofT _c andH _c2(T) and a decrease in andρ _n after reaching a maximum value at 0.5 to 1.0 at % iron. The observed decrease was about 35% forT _c, 85% forH _c2 at 2.0 K, 16% for and 21% forρ _n. Although the decrease in occurs through the decrease inρ _n as expected from the GLAG theory, the depression inT _c caused by magnetic impurity could not be explained in terms of the GLAG theory which is applicable to Nb-Zr-Si amorphous alloys without magnetic impurity, but was interpreted as arising from the pair-breaking effect in the superconducting nature due to magnetic scattering. However, the pair-breaking effect was found to be smaller by about one-tenth for the present amorphous superconductors than for crystalline superconductors, indicating the high stability of the superconductivity of the Nb-Zr-Si-Fe alloys against the magnetic scattering arising from the magnetic impurity. The reduced magnetic field at which the reduced fluxoid pinning force exhibits a maximum value increased with iron concentration, indicative of an enhancement of fluxoid pinning force. The enhancement in fluxoid pinning force was interpreted as arising from the increase in compositional, electronic and/or magnetic fluctuations by the dope of iron impurity.     

Stability and direct conversion of mineral barite crystals in carbonated hydrothermal fluids

The pseudomorphic replacement of mineral barite (BaSO₄) crystals into barium carbonate was investigated in the present work by using carbonated alkaline hydrothermal fluids. Hydrothermal treatments were carried out over the temperature range from 150 up to 250 °C for intervals between 1 and 192 h, with different filling ratios (40–70%), and molar ratios of 1, 5, and 10. The reaction products were characterized by XRD and SEM techniques. The chemical reactivity of mineral barite crystals was markedly limited at temperatures below 200 °C, and only a tiny BaCO₃ layer on the surface of the original BaSO₄ crystal was formed on the crystal treated for 192 h. The rate of the pseudomorphic conversion of BaSO₄ into BaCO₃, was accelerated by increasing the reaction temperature and the molar ratio . Powder X-ray diffraction results showed that under hydrothermal conditions the replacement of ions by ions, in barite crystals was completed at 250 °C with a molar ratio = 10 for an interval of 192 h, resulting in the Witherite structure. The morphology of the completely converted BaCO₃ at 250 °C in a Na₂CO₃ solution for 192 h, showed that the conversion proceed without severe changes of the original shape and dimension of the original crystal, similar to that observed in mineral pseudomorphic replacement process.     

Creep and densification during anisotropic sintering of glass powders

The isothermal sintering behaviour of a barium magnesium aluminosilicate glass powder at 930°C was investigated using a heating microscope. The cylindrical samples exhibited a variable shrinkage anisotropy during sintering. The shrinkage anisotropy ratio, defined as the ratio of the relative change of height and diameter, varied linearly between 0.3 and 0.98 with the relative volume shrinkage during densification. Shrinkage anisotropy caused creep deformation of the samples. The creep rate varied exponentially with the densification rate and the ratio of creep to densification rates, , decreased as densification proceeded. This is in disagreement with most previous studies, which show a constant value of during the densification. Overall, the study points out the relevance of variable shrinkage anisotropy and how it affects the densification behaviour of glass powders.     

Phonon Thermal Conductivity of Stripe Ordering La2–x Sr x NiO4

We have studied the thermal conductivity of stripe ordering La _2–x Sr _x NiO ₄. In particular, long range stripe order is well established for x = 1/3. For this composition is enhanced in the charge ordering phase and exhibits a clear maximum at low T. Even small deviations from this stochiometry cause a strong change of : the low T-maximum is suppressed and no anomaly is observed at high T. Our data confirm that the stripe phase is most stable for x = . Moreover, we find clear differences in the thermal conductivity for x > and for x < , respectively, which indicates different properties of the stripe ordered phase in these two regions of the phase diagram.     

Prediction of Fracture Toughness of Reactor Pressure-Vessel Steels Using the “Master Curve” Concept and Probabilistic Model

Using a probabilistic model and the Master curve approach, the temperature dependence of the brittle fracture toughness of reactor pressure-vessel steel 15Kh2NMFA in the initial state and highly embrittled state is predicted from the results of fracture toughness testing of a cracked Charpy-type specimen at a given temperature. A comparative analysis has shown that for the steel in the initial state the curves calculated by the probabilistic model and by the Master-curve approach are in good agreement. By testing compact-tension specimens of embrittled 2T-CT steel in a wide temperature range the authors have obtained experimental fracture toughness values and compared them with the calculated curves. It is demonstrated that, in the case of the embrittled steel, the curve as calculated by the Master-curve approach fails to describe adequately the experimental results, while the curves plotted by the probabilistic model agree well with the experimental fracture toughness values.