The reaction hot-pressing of compositions in the system Al-Si-N-O corresponding to β′-sialon

The reaction hot-pressing at 1700 and 1750° C of a number of compositions in the system Al-Si-N-O corresponding to points spanning the-sialon phase line in the region of z=0.8 has been studied. Measurements have been made of densification rate and of the rate of conversion of-Si₃N₄ to-sialon. The densification process for these compositions may be described in terms of a liquid-phase assisted fast particle rearrangement process succeeded by Coble creep. The rates of these processes are sensitive to the volume of grain-boundary liquid phase present, which in turn is determined by the position of the compositional point in relation to the-sialon line. For systems containing very little grain-boundary phase, the vapour-phase transport of material may become important.     

Self-reinforcement in li-α-sialon ceramics

Self-reinforcement of Li--sialon ceramics by in situ growth of elongated and -sialon grains has been explored and analysed. Properties of Li--sialon ceramics are mainly determined by the overall starting composition and the crystalline modification of the starting Si₃N₄ powder which in turn determine the final microstructure of the materials. Both the morphology and crystalline phase of the elongated sialon grains have strong effects on the toughening mechanism. The results indicate that -sialons reinforced by elongated -sialon grains have advantages over similar materials reinforced by elongated -sialon grains because of the type of crack deflection toughening mechanism involved.     

Phase decomposition of liquid-quenched β-type Ti-Cr alloys

Phase decomposition behaviour of liquid-quenched (bcc) type Ti-Cr alloys was investigated by means of transmission electron microscopy and hardness measurements. It was found that decomposition of to ₁ (Ti-rich, bcc) + ₂ (Ti-lean, bcc) takes place in the intermediate composition range of the Ti-Cr system. This experimental result proves the theoretical prediction made by Menon and Aaronson, but the observed ₁ + ₂ two-phase field expands towards higher temperatures than the predicted binodal line. The coherent ₁ + ₂ two-phase state exhibits the so-called 100 modulated structure and it was concluded that the formation of such a structure is a result of spinodal decomposition of the -phase. We obtained time-temperature-transformation (TTT) diagrams of -type Ti-30, 40 and 50 at % Cr alloys. A typical sequence of structural change is coherent ₁ + ₂ incoherent ₁ + ₂ incoherent ₁ + ₂ + grain boundary precipitates stable state of + TiCr₂ or + TiCr₂. Not all the states in the above sequence appear, depending on alloy composition, liquid-quenching rate and ageing temperature.     

Ultrasonic study of the temperature and pressure dependences of the elastic properties of β-silicon nitride ceramic

Ultrasonic wave velocity measurements have been used to determine the elastic stiffness moduli and related elastic properties of high-purity, dense -Si₃N₄ ceramic samples as functions of temperature in the range 150–295 K and hydrostatic pressure up to 0.2 GPa at room temperature. Due to its covalently bonded, rigid structural framework -Si₃N₄ is an elastically stiff material; the elastic stiffness moduli of the ceramic at 295 K are: C _L = 396 GPa, = 119 GPa, B ^S = 238 GPa, E = 306 GPa, Poisson's ratio = 0.285. The longitudinal elastic stiffness C _L increases with decreasing temperature and shows a knee at about 235 K; the decrease in slope below the knee indicates mode softening. The shear elastic stiffness shows mode softening which results in a plateau centred at about 235 K and an anomalous decrease with further reduction in temperature. The hydrostatic-pressure derivatives of elastic stiffnesses at 295 K are (C _L/P) _P=0 = 4.5 ± 0.1, (B ^S/P) _P=0 = 4.3 ± 0.1 and (/P) _P=0 = 0.17 ± 0.02 (pressure < 0.12 GPa). An interesting feature of the nonlinear acoustic behaviour of this ceramic is that, in the pressure range above 0.12 GPa, the values obtained for (/P) _P=0 and the shear mode Grüneisen parameter (_S) are small and negative, indicating acoustic-mode softening under these higher pressures. Both the anomalous temperature and pressure dependences of the shear elastic stiffness indicate incipient lattice shear instability. The shear _S(=0.005) is much smaller than the longitudinal _L(=1.18) accounting for the thermal Grüneisen parameter ^th(=1.09): since the acoustic Debye temperature _D(=923 ± 5 K) is so high, the shear modes play an important role in acoustic phonon population at room temperature. Hence knowledge of the elastic and nonlinear acoustic properties sheds light on the thermal properties of ceramic -Si₃N₄.     

Microstructural studies on silicon nitride

Thin specimens of reaction sintered and hot pressed silicon nitride have been prepared by ion beam thinning and examined in the Harwell million volt microscope. It has been found that reaction sintered material consists of large grains, which are mostly-Si₃N₄, in a fine grained matrix of-Si₃N₄. Fibres are frequently observed within the pores, the type of fibre depending on the size of the pore. The hot pressed material consists largely of two types of grain, small angular grains of-Si₃N₄ and larger irregular grains. There is also some non-crystalline material between the angular grains and there are numerous small unidentified inclusions.The grains of-Si₃N₄ generally contain dislocations and examination of these shows that most have a 0001 Burgers vector. The remaining dislocations appear to be more complex, frequently occurring as multiple images, and have not been unambiguously identified. An analysis of dislocations in-Si₃N₄ shows that 0001 dislocations are the most stable and are also likely to be most mobile with {10¯10} as the primary slip plane.     

Phase relationship between β′- and O′-sialon at 1623 K

-sialon whiskers and co-products of synthesis, such as -sialon powders and O-sialon powders, were annealed at 1623 K for 8 h in a closed graphite reaction tube under 1 atm nitrogen. Phase stabilities, Si/Al ratios, and crystallographic features were investigated. The O-sialon phase, which formed in the early stage of synthesis when oxygen partial pressure was relatively high, became less stable in the present annealing condition and decomposed. The majority of released aluminium and possibly oxygen from the decomposed O-powder was incorporated into -sialon whiskers with little change in its lattice parameters, when the -sialon whiskers were included in annealing. The aluminium contents were always lower in the -whiskers than in the powders even after increasing its aluminium content during 8 h annealing. The lattice parameters of both -whiskers and powders increased with increasing aluminium content and became closer after annealing. The lattice parameters of -whiskers remained the same before and after annealing despite the increased aluminium content, while the lattice parameters of -powders decreased despite its aluminium content remaining unchanged. The lattice parameters of O-sialon increased with increasing aluminium content, and the increase in thea direction is the largest when compared with other parameters.     

Nonlinear asymptotic theory of hypersonic flow past a circular cone

Summary The hypersonic small-disturbance theory is reexamined in this study. A systematic and rigorous approach is proposed to obtain the nonlinear asymptotic equation from the Taylor-Maccoll equation for hypersonic flow past a circular cone. Using this approach, consideration is made of a general asymptotic expansion of the unified supersonic-hypersonic similarity parameter together with the stretched coordinate. Moreover, the successive approximate solutions of the nonlinear hypersonic smalldisturbance equation are solved by iteration. Both of these approximations provide a closed-form solution, which is suitable for the analysis of various related flow problems. Besides the velocity components, the shock location and other thermodynamic properties are presented. Comparisons are also made of the zeroth-order with first-order approximations for shock location and pressure coefficient on the cone surface, respectively. The latter (including the nonlinear effects) demonstrates better correlation with exact solution than the zeroth-order approximation. This approach offers further insight into the fundamental features of hypersonic small-disturbance theory.Notation a speed of sound - H unified supersonic-hypersonic similarity parameter, - K hypersonic similarity parameter, M - M freestream Mach number - P pressure - T temperature - S entropy - u, v radial, polar velocities - V freestream velocity - shock angle - cone angle - density - density ratio, /() - ratio of specific heats - polar angle - stretched polar angle, / - (), (), () gage functions     

The Interplay of Electronic and Nuclear Magnetism in PtFe x at Milli-, Micro-, and Nanokelvin Temperatures

We have measured ac susceptibility, nuclear magnetic resonance, and nuclear heat capacity of two PtFe _x samples with concentrations of magnetic impurities x = 11 ppm and 41 ppm at magnetic fields (0 ± 0.05) mTB248 mT. The susceptibility data have been measured at temperatures of 0.3 KT100 mK, no hint for nuclear magnetic ordering could be detected to a temperature of 0.3 K. The nuclear heat capacity data taken at 1.4 KT10 mK show enhanced values which scale with x at low polarization. This effect is described by a model assuming an internal magnetic field caused by the impurities. No indication for nuclear magnetic ordering could be detected to 1.4 K. The nuclear magnetic resonance experiments have been performed on these samples at 0.8 KT0.5 mK and 2.5 mTB22.8 mT as well as on three other samples with x = 5, 10, 31 ppm in a different setup at 40 KT0.5 mK and at 5.4 mTB200 mT. Spin-lattice and effective spin-spin relaxation times ₁and ₂ ^* of ¹⁹⁵ Pt strongly depend on x and on the external magnetic field. No temperature dependence of ₁and ₂ ^* could be detected and the NMR data, too, give no hint for nuclear magnetic ordering to 0.8 K.     

Gas pressure sintering of β-silicon nitride

The sintering behaviour of -Si₃N₄ powder was investigated in 980 kPa (10 atm) nitrogen at 1800–2000 °C. It is shown that -Si₃N₄ has a higher sinterability than the finer -Si₃N₄. The solution of small grains and reprecipitation on large grains occurred during sintering at >1600 °C. The rate-determining step in the liquid-phase sintering is believed to be the diffusion of material through the liquid phase at grain boundaries. There was no abnormal grain growth during gas pressure sintering of -Si₃N₄. The microstructures of gas pressure sintered materials from -Si₃N₄ were more uniform than those from -Si₃N₄. The densification mechanism of -Si₃N₄ is discussed in relation to that of -Si₃N₄.     

Breakup of an anomolously viscous liquid film in a centrifugal force field

An equation is obtained for the breakup radius with consideration of tipping moments and Laplacian pressure forces acting on the liquid ridge at the critical point.Notation K, n rhenological constants - density - surface tension - r current cup radius - R maximum cup radius - r_c critical radius for film breakup - ¯r=¯r=r/R dimensionless current radius - ¯r_c=r_c/R dimensionless critical radius - ₀, _c actual and critical film thicknesses - current thickness - R_r ridge radius - h₀ ridge height - h current ridge height - ₀ limiting wetting angle - current angle of tangent to ridge surface - angle between axis of rotation and tangent to cup surface - angular velocity of rotation - q volume liquid flow rate - v₁ and v meridional and tangential velocities - =4vv _lm/r,=4v_m/r dimensionless velocities - M moments of surface and centrifugal forces - M_v moment from velocity head - p_r pressure within ridge - P_vm pressure from velocity head - p_m, p_pm pressures from centrifugal force components tangent and normal to cup surface - deviation range of breakup radius from calculated value - ¯r_max, ¯r_min limiting deviations of breakup radius - _c angle of tangent to curve _c/°₀=f(¯r) at critical point - t random oscillation of ratio _c/_c Translated from Inzhenerno-Fizicheskii Zhurnal, Vol. 39, No. 1, pp. 51–56, July, 1980.     

Influence of microstructure on strength and fracture toughness ofβ-Sialon

-Sialon (Si_6–z Al _z O _z N_8–z ) withz = 0.5 was fabricated by hot-pressing of a spray dried mixture of –Si₃N₄ and aluminium-isopropoxide solution. Phase composition, flexural strength and microstructure of a sintered body were investigated. Phases identified by XRD were -Sialon and a small amount of O-Sialon. The flexural strength (three-point bending) was about 1500 MN m^–2. This value, about three times higher than that of -Sialon fabricated from -Si₃N₄ and -Al₂O₃ powder, was mainly due to the homogeneous microstructure without large defects such like clusters of large grains. -Sialon was heat treated at 2000 °C for 2 h in 4 M Pa N₂ to develop elongated -Sialon grains with high aspect ratio. Microstructure, flexural strength and fracture toughness (K _Ic) of it were investigated. Both strength andK _Ic were lower than those of hot-pressed sample, even though an elongated microstructure was achieved. This fact showed that the toughening of -Sialon with elongated grains could not be achieved without grain boundary phase which resulted in a crack deflection.     

The age hardening effect in Ti-6 Al-4 V due to ω and α precipitation in the β grains

The structure at room temperature of a quenched TA6V titanium alloy has been investigated. This structure is + or + according to the treatment temperature; it is always metastable. During ageing the grains decomposed by the reaction + + +; this decomposition was accompanied by a large increase of the 0.2% yield stress. No structural modification was observed in. The and phase of TA6V were separately investigated in the form of single-phase alloys. The hardness of was insensitive to ageing, while was considerably hardened by and; we deduced that the strengthening of the minor phase during ageing is mainly responsible for the hardening of TA6V.     

Distribution of α-AlFeSi and β-AlFeSi particles in surface layer of AA6063 alloy billets after heat treatment

We developed the EPMA mapping method of small -AlFeSi(Al_8.3Fe₂Si) and -AlFeSi(Al_8.9Fe₂Si₂) particles in the billets of Al-Mg-Si alloys such as AA6063 alloys. To discriminate between -AlFeSi and -AlFeSi particles we used the relative X-ray intensities of Fe/Si ratio, the I _Fe/I _Si ratio, instead of the Fe/Si mass ratio. To obtain the I _Fe/I _Si ratio, we used a Monte Carlo method. In this study, using this method the mapping of -AlFeSi and -AlFeSi particles in the surface layer of AA6063 billets after the heat treatment (for 2 h at 580°C) was done. Namely, the distribution of -AlFeSi and -AlFeSi particles of zones from the billet surface to a depth of 800 m was measured. Results showed the zone from the surface to a depth of 200 m was occupied mainly by -AlFeSi particles and the zone from a depth of 200 m toward the center was occupied mainly by -AlFeSi particles. From these results, it was found that if we remove zones from the surface to a depth of 200 m, we can remove the majority of the -AlFeSi particles, and thus improve the quality of anodizing performance of Al-Mg-Si alloys extrusions.     

Mössbauer studies of α″-Fe16N2 and α′-Fe8N films

Conversion-electron Mössbauer spectra of epitaxial -Fe₁₆N₂ and -Fe₈N films have been studied and their differences are discussed in detail. The Mössbauer spectrum of -Fe₁₆N₂ can be decomposed into three subspectra, which correspond to the 4d, 8h and 4c sites. The Mössbauer spectrum of -Fe₈N can be fitted using four spectra based on a nitrogen-atom-random-distribution model. The average hyperfine field is larger (3%) for -Fe₁₆N₂ than for -Fe₈N, which is approximately consistent with a 4.1% enhancement of the magnetic moments for -Fe₁₆N₂. The iron moments tend to locate in the film plane for -Fe₁₆N₂ and to arrange perpendicularly to the film plane for -Fe₈N.     

Oxidation behaviour of Β-sialon fabricated from α-Si3N4 and aluminium iso-propoxide

-sialon with z=0.5 was fabricated by hot pressing of a spray-dried mixture of -Si₃N₄ and aluminium iso-propoxide solution. The oxidation behaviour of this -sialon was investigated, comparing it with commercial -sialon containing Y₂O₃ as a sintering aid. Oxidation tests were carried out at 1200 and 1400C for 25 to 200 h in air. The oxide layer of aluminium isopropoxide-derived -sialon was thin, dense, smooth and homogeneous without bubbles and cracks. The strength after oxidation at 1400C for 200 h was about 800 MN m^–2, almost the same value as before oxidation. The oxide layer of Y₂O₃-doped -sialon was thick and inhomogeneous, containing many bubbles, cracks and grown needle-like crystallites (Y₂Si₂O₇). The strength after oxidation at 1200C for 200 h fell to 1/2(440 MN m^–2) because of pit formation in the oxide layer, and at 1400C for 200 h fell to 1/4(200 MN m^–2) because of severe swelling and flaking of the oxide layer. The high oxidation resistance of aluminium iso-propoxide derived -sialon was mainly due to its homogeneous microstructure and freedom from foreign constituents such as Y₂O₃.     

Flow of a heated ferrofluid over a stretching sheet in the presence of a magnetic dipole

Summary The flow of a viscous ferrofluid over a stretching sheet in the presence of a magnetic dipole is considered. The fluid momentum and thermal energy equations are fomulated as a five-parameter problem, and the influence of the magneto-thermomechanical coupling is explored numerically. It is concluded that the primary effect of the magnetic field is to decelerate the fluid motion as compared to the hydrodynamic case, thereby increasing the skin friction and reducing the heat transfer rate at the sheet.Nomenclature a distance - c constant - c _p specific heat at constant pressure - C _f wall friction coefficient - e 2.71828 ... - f dimensionless stream function - H magnetic field - k thermal conductivity - K constant - M magnetization - Nu _x local Nusselt number - p pressure - P dimensionless pressure - Pr Prandtl number, c _p/k - Re _x local Reynolds number, cx ²/ - T temperature - u velocity component along the sheet - v velocity component normal to the sheet - x coordinate along the sheet - y coordinate normal to the sheet - dimensionless distance - ferrohydrodynamic interaction parameter - constant - dimensionless Curie temperature - dimensionless coordinate - dimensionless temperature - viscous dissipation parameter - dynamic viscosity - ₀ permeability - dimensionless coordinate - density - shear stress - magnetic potential - stream function     

Carbothermal production of β′-sialon from alumina,silica and carbon mixture

Mixtures of pure nanometer-sized amorphous silica and -alumina with the atomic ratio SiAl=1 were reduced by a stoichiometric amount of carbon between 1100 and 1450 °C in flowing nitrogen in order to produce -sialon powder. Using aqueous suspensions of starting materials, compacts with different microstructures were prepared for reaction. Silica reduction to SiO occurred at a temperature as low as 1300 °C and part of it was removed with flowing nitrogen. Carbothermal reaction involving nitrogen stated at 1350 °C and Si₂N₂O was found as an intermediate together with SiC, resulting in -sialon formation. Loss of silica from the system led to AlN formation. Decomposition of -sialon into sialon polytypoids (15R, 12H) was observed as a result of sialon and AlN reaction at 1450 °C. The reaction rate of sialon formation was slowed down compared to the carbothermal reduction of kaolin because of the lack of impurities. The microstructure of the reacted pellets influenced the reaction products, and the narrow pore size distribution as well as good homogeneity enhanced -sialon formation.On leave, from Silesian Technical University, Krasiskiego 8, 40-019 Katowice, Poland.     

Effect of crystalline phase, orientation and temperature on the dielectric properties of poly (vinylidene fluoride) (PVDF)

The effect of crystalline phase, uniaxial drawing and temperature on the real () and imaginary () parts of the relative complex permittivity of poly (vinylidene fluoride) (PVDF) was studied in the frequency range between 10² and 10⁶ Hz. Samples containing predominantly and phases, or a mixture of these, were obtained by crystallization from a DMF solution at different temperatures. phase samples were also obtained from melt crystallization and from commercial films supplied by Bemberg Folien. Different molecular orientations were obtained by uniaxial drawing of and phase samples. The results showed that the crystalline phase exerts strong influence on the values of and , indicating that the _a relaxation process, associated with the glass transition of PVDF, is not exclsively related to the amorphous region of the polymer. An interphase region, which maintains the conformational characteristics of the crystalline regions, should influence the process decisively. The molecular orientation increased the values of for both PVDF phases and modified its dependence with temperature over the whole frequency range studied. The influence of the crystallization and molecular orientation conditions on the dc electric conductivity (_dc) were also verified. The value of _dc was slightly higher for samples crystallized from solution at the lowest temperature and decreased with draw ratio.     

Equation of state of3He near its liquid-vapor critical point

We report high-resolution measurements of the pressure coefficient (P/T) for³He in both the one-phase and two-phase regions close to the critical point. These include data on 40 isochores over the intervals–0.1t+0.1 and–0.2+0.2, wheret=(T–T _c )/T _c and =(– _c )/ _c . We have determined the discontinuity (P/T) of (P/T) between the one-phase and the two-phase regions along the coexistence curve as a function of . The asymptotic behavior of (1/) (P/T) versus near the critical point gives a power law with an exponent (+–1)^–1=1.39±0.02 for0.010.2 or–1×10 ^–2t–10 ^–6 , from which we deduce =1.14±0.01, using =0.361 determined from the shape of the coexistence curve. An analysis of the discontinuity (P/T) with a correction-to-scaling term gives =1.17±0.02. The quoted errors are fromstatistics alone. Furthermore, we combine our data with heat capacity results by Brown and Meyer to calculate (/T) _c as a function oft. In the two-phase region the slope (²/T ²)_c is different from that in the one-phase region. These findings are discussed in the light of the predictions from simple scaling and more refined theories and model calculations. For the isochores 0 we form a scaling plot to test whether the data follow simple scaling, which assumes antisymmetry of – ( _c ,t) as a function of on both sides of the critical isochore. We find that indeed this plot shows that the assumption of simple scaling holds reasonably well for our data over the ranget0.1. A fit of our data to the linear model approximation is obtained for0.10 andt0.02, giving a value of =1.16±0.02. Beyond this range, deviations between the fit and the data are greater than the experimental scatter. Finally we discuss the (P/T) data analysis for ⁴ He by Kierstead. A power law plot of (1/) P/T) versus belowT _c leads to =1.13±0.10. An analysis with a correction-to-scaling term gives =1.06±0.02. In contrast to ³ He, the slopes (²/T ²)_c above and belowT _c are only marginally different.Work supported by a grant from the National Science Foundation.     

The redistribution of alloying elements by rapid-heating solution treatment of an (α +β) titanium alloy

Thin-foil X-ray energy-dispersive chemical analysis of an (+) titanium alloy has been used to establish the compositional profiles which develop between the and phases as a result of heating into the field at a rate of 100 K sec^–1. The results show that phase transforms to via a diffusional mechanism as it is progressively enriched in-stabilizing solutes. Complete diffusional transformation of to occurs 160 K above the transus but the phase remains chemically inhomogeneous. On subsequent quenching at a rate of 400 K sec^–1, phase containing less than approximately 10wt% Mo equivalent of -stabilizing solutes transforms to martensite. The proposed transformation mechanisms are consistent with the results of resistivity measurements made during the heating and cooling cycles.