Elastic anisotropy and the grain size dependence of ceramic fracture energies

A literature review of fracture energy ()-grain size (G) trends of cubic ceramics, and an analysis based on adaptation of a model for thermal expansion anisotropy effects are made to evaluate effects of elastic anisotropy (EA) on . Although the model does not give the specific, typically limited, —G dependences suggested by experimental data, it does predict the level of the maxima indicated at intermediateG in some materials, and the lower values at large against smallG. Further, both of these deviations from constant are shown to be dependent on crack size and hence consistent with their being more frequently and extensively seen with notch beam (NB) as against most other measuring methods.     

Effect of annealing upon decomposition of electrodeposited iron-zinc alloy coatings

As-deposited electrodeposited iron-zinc alloy coatings containing phase, decompose upon heating through a sequence of metastable phases. The h c p phase transforms to b c c G, or -like phase via a rapid diffusional phase transformation in the vicinity of 150 °C. For bulk iron contents of 8–13 wt%, transforms to 100% G phase. The G phase subsequently transforms at 240 °C to phase, which in turn transforms to or ₁ phase near 300 °C by depletion of iron from the surrounding matrix. The decomposition process may be driven by supersaturation of with iron.     

Discrete β-Ta2O5 crystallite formation in reactively sputtered amorphous thin films

The crystallization of thin amorphous TaOx films formed by d.c. reactive sputtering was investigated at temperatures from 500–700 °C. The films remained amorphous for times up to 100 h at 500 °C. The formation of discrete, single crystallites of the orthorhombic -Ta2O5 phase was observed after annealing at 600 °C for times from 8–108 h. The crystallites were 0.35 m×0.35 m after 8 h and grew to approximately 2.5 m×2.0 m after 108 h. A (2 0 0) fibre texture with a 6° spread was observed. More rapid in-plane growth in the [0 1 0] direction resulted in a near-rectangular shape and is attributed to a ledge growth mechanism. Higher temperature anneals at 650 and 700 °C produced less-textured polycrystalline films with remnant amorphous regions. © 1998 Kluwer Academic Publishers     

Mechanical and Corrosion Characteristics of Zr + 2.5% Nb Zirconium Reactor Alloy

The results of structural and phase hardening of pipes made of Zr + 2.5% Nb alloy show that ultrahigh-frequency thermal treatment of pipes (fast heating to the temperature of existence of the -phase followed by sharp cooling and annealing in the high-temperature range of the -phase) destroys the texture and forms a fine-grained structure (the grain diameter is about 1 m) with numerous transitional twins and a high density of precipitations of the secondary -niobium phase ( 10¹⁶cm^–3). In this state, the alloy is rather strong and plastic (at room temperature, _u 650 MPa, _0.2 550 MPa, and 20% both in the longitudinal and transverse directions). The efficiency of hardening by ultrahigh-frequency thermal treatment is not reduced with increase in the temperature of testing up to 500°C. Corrosion tests of channel pipes made of Zr + 2.5% Nb alloy subjected to ultrahigh-frequency thermal treatment in water containing various amounts of oxygen (from 0.1–0.3 to 600 mg/kg) at temperatures of 285–350°C for 700–6600 h under static conditions and in reactor water of the Ignalina Nuclear Power Plant for 5000 h under dynamic conditions showed that the corrosion resistance of this alloy is on a par with the corrosion resistance of the material of assembly channels of high-power channel reactors subjected to a standard treatment.     

Dielectric relaxation in glassy Se80?xTe20Gex

Dielectric relaxation studies have been made in glassy Se_80–xTe₂₀Ge_x alloys where 0 x 20. The measurements of dielectric constant () and dielectric loss () are made in the audio frequency range (1 kHz to 10 kHz) at various temperatures from 30°C to 150°C. The results indicate that the dielectric dispersion occurs in the above frequency and temperature range. An analysis of the results shows that the dielectric losses are dipolar in nature and can be understood in terms of hopping of charge carriers over a potential barrier.     

Effect of temperature and strain rate on tensile mechanical properties of ARALL-1 laminates

The combined effect of temperature and strain rate of the mechanical properties for unidirectional 3/2 ARALL^®-1 laminates was studied. In this paper, the effect of strain rates from 0.00083–0.833 min^–1 on tensile behaviour at temperatures up to 250°F (121 °C) has been conducted. It is demonstrated that tensile strength, tensile modulus, and fracture strain are found to depend on temperature and strain rate. However, the effect of strain rates at 75 °F (24 °C) and 180 °F (82 °C) was found to be insignificant except the lowest strain rate at 180 °F. It was also observed that the tensile yield strength decreased as the strain rate decreased. The tensile properties were moderately reduced at high temperatures and were higher at high strain rates than at low strain rates. The temperature effect is more significant than that due to the strain rate. Scanning electron photomicrographs of the fracture surfaces observed in the aramid/epoxy layer of ARALL-1 laminates at the lowest strain rate are shown to be significantly different only at 250 °F (121 °C). But this phenomenon is not obvious when the highest strain rate is employed.     

Effect of prior cold rolling and test temperature on stress-strain rate behaviour of a Zr-2.5Nb alloy

Zr-2.5 wt% Nb alloy sheet, obtained by unfolding and straightening a pressure tube, was further cold rolled upto 39% reduction in thickness to investigate the effect of cold working on the stress ()-strain rate () behaviour over a strain rate range of 2 × 10–5 to 5 × 10–3 s–1 and a temperature range of 625 to 700 °C. Irrespective of the amount of rolling, the log vs log plots exhibit superplastic behaviour with strain rate sensitivity index, m, as high as 0.8, which decreases to 0.2 at higher strain rates. On the other hand, the activation energy for deformation, Q, increases from 171.1 kJ/mol for superplastic deformation to 249 kJ/mol in Region III. The tendency for improved superplasticity (m) is seen upon cold working by 22% or more at the test temperatures 675 and 700 °C.     

X-ray studies on the thermal expansion of tellurium dioxide

Using a Unicam 19 cm high temperature powder camera, the precision lattice parameters of tellurium dioxide have been determined at different temperatures in the range 30 to 461 °C. Using this data, the coefficients of thermal expansion, and parallel and perpendicular to the principal axis respectively, have been evaluated. The temperature dependence of the coefficients of thermal expansion is represented by the following equations: =29.673×10^–6+1.552sx10^–8 T+1.069sx10^–10 T ² =9.875sx10^–6–5.440sx10^–9 T+4.572sx 10^–12 T² HereT is the temperature in °C. The thermal expansion of tellurium dioxide has been explained in terms of the interionic distances.     

Anisotropy in the hardness and friction of calcium fluoride crystals

Anisotropy in the Knoop indentation hardness and the friction of diamond cones on calcium fluoride crystals has been investigated at experimental temperatures from 20 to 300° C. It is shown that the directions of minimum and maximum indentation hardness, on the (001) plane, are 110 and 100 respectively whilst the 1¯10 are harder than the 11¯2 directions on the (111) plane. Also, the sliding friction in the (001) plane is greatest in the 110 directions and least in the 100 and, on the (111) cleavage plane, [¯1¯12] sliding leads to higher friction than [11¯2]. The nature of anisotropy, for both hardness and friction measurements, does not change over the experimental temperature range covered in this work. Observations on the resultant deformation are made and these anisotropic properties are explained in terms of the effective resolved shear stresses developed on the {100} 011 primary slip systems at all experimental temperatures.     

Morphology and phase transition of high melt temperature crystallized poly(vinylidene fluoride)

When PVDF is crystallized at temperatures above 155°C it presents a multiform morphology composed of ringed, non ringed and mixed spherulites. Infrared spectroscopy showed that the ringed spherulites are formed exclusively by the phase when crystallization takes place at temperatures below 155°C. Higher temperatures induce a solid-state phase transformation in these structures, increasing the amount of phase with crystallization time. The rate at which this transformation takes place increases with crystallization temperature. The non ringed spherulites, only formed at crystallization temperatures above 155°C, consist predominantly of the phase, crystallized from the melt, with small phase inclusions. The melt process of the different spherulites, observed by optical microscopy and calorimetric measurements (DSC) showed that the melt temperature of the phase, originated from the phase transition, is 8°C higher than that crystallized directly from the melt. Optical micrographs of samples heated up to 186°C and quickly cooled allowed visualization of the ringed spherulite regions which underwent the phase transformation at different crystallization times and temperatures.     

Solid state phase transformation of BaB2O4 during the isothermal annealing process

Solid-state phase transformation of BaB₂O₄ during the isothermal annealing process for both to and to were investigated using a platinum crucible. For the -phase crystal at the -phase stable temperature (> 925 °C), the phase transforms to the phase perfectly below the melting temperature of 1100 °C. Meanwhile, for the -phase crystal at the -phase stable temperature (< 925 °C), the phase transforms to the phase perfectly above 800 °C. There is some difference in phase transformation behaviour between bulk-shape crystals and the powder, caused by thermal stress.     

Standard Gibbs' energies of formation of BaCuO2, Y2Cu2O5 and Y2BaCuO5

The Gibbs' energies of formation of BaCuO₂, Y₂Cu₂O₅ and Y₂BaCuO₅ from component oxides have been measured using solid state galvanic cells incorporating CaF₂ as the solid electrolyte under pure oxygen at a pressure of 1.01×10⁵ Pa BaO + CuO BaCuO₂ G _f,ox ^o (± 0.3) (kJ mol^–1)=–63.4–0.0525T(K) Y₂O₃ + 2CuO Y₂Cu₂O₂ G _f,ox ^o (± 0.3) (kJ mol^–1)=18.47–0.0219T(K) Y₂O₃ + BaO + CuO Y₂BaCuO₅ G _f,ox ^o (± 0.7) (kJ mol^–1)=–72.5–0.0793T(K) Because the superconducting compound YBa₂Cu₃O_7– coexists with any two of the phases CuO, BaCuO₂ and Y₂BaCuO₅, the data on BaCuO₂ and Y₂BaCuO₅ obtained in this study provide the basis for the evaluation of the Gibbs' energy of formation of the 1-2-3 compound at high temperatures.     

Microstructure and annealing behaviour of cold-drawn isotactic polypropylene

Isotactic polypropylene tensile bars were cold-drawn at room temperature and subsequently annealed for various times at temperatures ranging from 50 to 155° C. The material was examined at room temperature in the as-drawn state at several stages of annealing. SAXS, density and mechanical loss data were obtained. Furthermore, thin films were cast. These films were drawn at –196° C and subsequently examined in the electron microscope at –120° C and at higher annealing temperatures. SAXS results for lower temperature annealing showed increases in the intensity of the small-angle Bragg hump with no change in position. High temperature annealing produced a very large intensity increase. In no case did the density of the material show a large increase. Electron microscopy indicated a microstructureless material in the as-drawn state. Annealing at low temperatures produced a fibrous morphology with no observable density modulation in the draw direction. High temperature annealing produced a lamellar microstructure with normal, stepwise density modulation. Dynamical mechanical loss curves exhibited no or little relaxation, except after high temperature annealing. On the basis of these observations, a microstructural model is proposed. The model suggests a very highly defective crystal or paracrystal in the as-drawn state. Low temperature annealing promotes a fibrillar, fringed micellar morphology, in which crystalline and amorphous regions are not clearly delineated. At higher annealing temperatures, a lamellar, two-phase microstructure is produced.On leave from Universität des Saarlandes, 66 Saarbrücken, West Germany.     

Phase transformations and structure characterization of calcium polyphosphate during sintering process

Calcium polyphosphate (CPP) may be a promising bone substitute with controllably degraded ability. In this investigation, the effects of sintering temperatures on CPP's phase transformations and microstructure parameters, such as the distribution of crystallite size and micro-strain, were investigated by X-ray diffraction (XRD). The qualitative phase analysis and quantitative phase analysis based on reference intensity ratio (RIR) method were conducted for the CPP sintered at 585, 600, 650, 700, 750, 800 and 900°C. The distribution of crystallite size and micro-strain were calculated with the Warren-Averbach Fourier Transfer method. The results demonstrated that the transformation of amorphous CPP to semi-crystalline CPP occurred below 585°C, and semi-crystalline CPP to -CPP at temperature of 585–600°C; -CPP to -CPP at 585–700°C. CPP sintered between 600–700°C were composed of both -CPP and -CPP, and the mass fraction of -CPP increased with rising of temperature. Above 700°C, the sintered CPP only contained -CPP. At different ranges of the sintering temperature, the average crystallite size (D) and micro-strain () showed significant difference, for example, D and is about 2.9 nm and 1.68% at 585°C, but D and was 8.0 to 8.7 nm and 0.159 to 0.134% at 600 and 700°C, respectively. The results of the phase transformations and the variations of microstructure parameters in the present study may be able to provide some fundamental data for explaining CPP degradation phenomena.     

Characterization of a δ/γ duplex stainless steel

A duplex stainless steel was investigated in both as-received sheet and after annealing at temperatures ranging from 850 to 1100°C. The sheet presents a deformation texture in both phases, austenite and ferrite, induced by cold rolling. Microstructure in the as-received material consists of island-like austenitic grains in a ferrite matrix. These austenitic grains are elongated with an average size of 6, 20 and 40 m along the normal (ND), transversal (TD) and rolling direction (RD). Quantitative texture measurements demonstrated that texture components are distributed mainly along the -fiber (ND ‹100›) and -fiber (RD ‹110›) for the ferrite and the -fiber (ND ‹110›) for the austenite. After recrystallization, a decrease in the intensity of the mean fibers and an increase in the minor components was observed in both, ferrite and austenite. Therefore, a similar texture was reached in both phases after annealing at 1050°C. Microstructural characterization after annealing at temperatures above 850°C showed that the elongated austenitic grains transform in colonies of equiaxic grains of about 10–15 m in size. These colonies are surrounded by a ferritic matrix at annealing temperatures above 1000°C or by a laminar microstructure at temperatures below 950°C. This laminar microstructure includes sigma phase and austenite formed from delta ferrite, and untransformed delta ferrite.     

Off-axis creep of a ceramic-matrix/continuous-ceramic-fiber composite: Experimental evaluation

The compression creep of a unidirectionally reinforced, SiC continuous fiber/calcium aluminosilicate (anorthite) glass-ceramic matrix composite was evaluated experimentally. Experiments covered the stress (–₁) and temperature (T) ranges of 20–40 MPa and 1300–1320°C, respectively. The experiments also emphasized characterization of the rheology as a function of the angle of misorientation () between the applied compressive load and the direction of reinforcement. For any given , T condition, the highest steady-state strain rate occurred for 50° (up to an order of magnitude faster than in the transverse, = 90°, case); overall composite strain in this case included a substantial contribution from displacement across the fiber-matrix interface. The data reveal that the interfacial rheology responsible for the displacement is distinctly temperature sensitive. Evaluation of the composite flow through its comparison to numerical/rheological models that scrutinize the interfacial effect implies that the interface is characterized by a non-Newtonian viscous rheology; this suggests that the interface response involves specifically the flow of the thin amorphous silica interphase that comprises a portion of the fiber-matrix interface in this material. The overall plastic response of the unidirectionally reinforced material is nevertheless rate-limited by plastic flow of the matrix and can be described by the superposition of three modes of strain, the magnitude of each being dependent specifically on .     

Electron diffraction study of superlattices and orientation variants in Ca3SrAl6SO16

Samples having the nominal composition of Ca₃SrAl₆SO₁₆ were sintered at 1380 °C and analysed by electron diffraction. The frequent appearances of forbidden and satellite reflections in this compound imply the presence of a number of basal and nonbasal superlattices so that the microstructure of this cement clinker was characterized by various superstructures including one-, two- and even three-dimensional superstructures along the 0 0 1, 1 1 0, 1 1 2, 1 1 4 or 2 2 1, 0 1 3 and 1 2 3 directions with repeat periods of two or three times of that of basic one, respectively, and intergrowth of these. Various domain structures with 90°, 120° and 48.2°, etc., orientation relationships were also detected in these superstructures and the total number of these orientation variants related to the symmetry elements lost in the process of phase transformation, can be predicted according to the conclusions of Van Tendeloo and Amerlinckx, or they are equal to the number of those unique planes in the matrix.     

Thermal expansion of interlayer spacing and thermal vibrational displacement of carbon atoms in petroleum coke

On petroleum coke heat-treated at various temperatures in the range from 1600 to 3000°C, thermal expansion of the interlayer spacing and the mean-square displacement along the c-axis due to thermal vibration of carbon atoms were measured from room temperature to 1050°C by means of X-ray diffractometry. The static mean-square displacement due to imperfect crystallization was also estimated for each sample.The c-axis spacing increases linearly with temperature and the slopes had almost the same values (1.85×10^–4 to 1.89×10^–4Å/°C) for all samples. The mean-square thermal vibrational displacements of carbon atoms increased almost linearly from 0.012Ų at room temperature to 0.047Ų at 1000°C for all samples, except for the sample heat-treated at 1640°C.A mean free space between the layer planes, that is the interlayer spacing minus twice the total root-mean-square displacement of carbon atoms along the c-axis direction, was obtained in consideration of the mean-square thermal vibrational displacement and the mean-square static displacement. The mean free space increases abruptly with decrease of c-spacing from 6.86 to 6.85Å (heat-treatment temperatures of 1640 and 2100°C respectively), then decreases slowly and eventually again begins to increase with further decrease of c-axis spacing to 6.73Å.     

Magnetic Co2Y ferrite, Ba2Co2Fe12O22 fibres produced by a blow spun process

Gel fibres of Co2Y,Ba2Co2Fe12O22, were blow spun from an aqueous inorganic sol and calcined at temperatures of up to 1200°C. The ceramic fibres were shown by X-ray diffraction to form crystalline Co2Y at 1000°C, and surface area and porosity measurements indicated an unusually high degree of sintering at this temperature. The fibres also demonstrated a small grain size of 1–3 m across the hexagonal plane and 0.1–0.3 m thickness at 1000°C. This only increased to 3 m in diameter and 1 m thickness even at temperature up to 1200°C. The fibrous nature combined with the improved microstructures could be an important factor in improving the magnetic properties of this material.     

The dielectric properties of aluminium nitride substrates for microelectronics packaging

The dielectric behaviour of sintered polycrystalline aluminium nitride substrates has been examined over the frequency range 500 Hz to 10 MHz and correlated with composition and microstructure. For pure, white AlN at 20 ° C both the permittivity () and dielectric loss () are frequency independent giving = 9.2±0.05 and tan = (2.1±0.1) × 10^–3. The permittivity is less than for pure alumina substrates ( = 10.2) but tan compares favourably, with that (1.4 × 10^–3) of alumina, which though used more widely has a thermal conductivity some eight times less than that of AlN. The addition of impurities, particularly iron, to give opaque black AlN causes large, frequency dependent increases in ; at 500 Hz the loss is seven times that of pure white AlN and is two times greater above 100 kHz. The temperature coefficient of permittivity [( – 1)( + 2)]^–1 [/T]_p between –180 and +180 ° C for pure white AlN is 1.05×10^–5 K^–1 which is similar to the value of 9×10^–6 K^–1 for pure Al₂O₃. For impure black AlN the coefficient below 20 ° C is the same but above 20 ° C there is a rapid, non-linear increase of with temperature. Below 180 ° C for pure white AlN and 20 ° C for impure black AlN the values of temperature coefficient are frequency independent at least up to 200 kHz.