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.     

Fabrication of silicon nitride nanoceramics—Powder preparation and sintering: A review

Fine-grained silicon nitride ceramics were investigated mainly for their high-strain-rate plasticity. The preparation and densification of fine silicon nitride powder were reviewed. Commercial sub-micrometer powder was used as raw powder in the “as-received” state and then used after being ground and undergoing classification operation. Chemical vapor deposition and plasma processes were used for fabricating nanopowder because a further reduction in grain size caused by grinding had limitations. More recently, nanopowder has also been obtained by high-energy milling. This process in principle is the same as conventional planetary milling. For densification, primarily hot pressing was performed, although a similar process known as spark plasma sintering (SPS) has also recently been used. One of the advantages of SPS is its high heating rate. The high heating rate is advantageous because it reduces sintering time, achieving densification without grain growth. We prepared silicon nitride nanopowder by high-energy milling and then obtained nanoceramics by densifying the nanopowder by SPS.     

α-β phase transformation of silicon nitride — computer simulation

The simulation model of - silicon nitride phase transformation was developed for the case when the crystallization of the phase is the rate controlling step. The results gained on the base of the present model indicate that the temperature and total free surface area of silicon nitride phase present in the firing body limit the rate of transformation and total amount of transformed silicon nitride phase. These results are acceptable from the point of view of experimental experience and support the applicability of the presented model.     

Fabrication and mechanical properties of silicon carbide–silicon nitride nanocomposites

A powder mixture of ultrafine –SiC–35 wt% –Si₃N₄ containing 6 wt% Al₂O₃ and 4 wt% Y₂O₃ as sintering additives were liquid–phase sintered at 1800°C for 30 min by hot–pressing. The hot–pressed composites were subsequently annealed at 1920°C under nitrogen–gas–pressure to enhance grain growth. The average grain–size of the sintered bodies were ranged from 96 to 251 nm for SiC and from 202 to 407 nm for Si₃N₄, which were much finer than those of ordinary sintered SiC–Si₃N₄ composites. Both strength and fracture toughness of fine–grained SiC–Si₃N₄ composites increased with increasing grain size. Such results suggested that a small amount of grain growth in the fine–grained region (250 nm for SiC and 400 nm for Si₃N₄) was beneficial for mechanical properties of the composites. The room–temperature flexural strength and fracture toughness of the 8–h annealed composites were 698 MPa and 4.7 MPa · m^1/2, respectively.     

Gas-phase synthesis of amorphous silicon nitride — reaction paths and powder characteristics

The gas phase reaction between SiCl₄ and NH₃ is investigated in the temperature range between 525 and 800°C at atmospheric pressure and at conditions typical for powder synthesis. By means of mass spectrometric in-situ measurements it was possible to detect the gaseous compounds H₂NSiCl₃, H₂NSiCl₂NH₂, Cl₃SiNHSiCl₃, NH₂Cl₂SiNHSiCl₃, (SiCl₂NH)₃ and Si₃(NH)₃Cl₅NH₂. The reactions taken place in the gas phase are very fast and result in the formation of a fine, chlorine containing product. Powders sampled at a reaction temperature of 800°C have an average molar ratio Si : N : Cl of 1 : 1, 33 : 0.28. Based on the proved gaseous intermediates and the composition of the powders reaction paths resulting in the formation of powders are derived. -Si₃N₄ powders with a high sintering activity are obtained after thermal dechlorination of the synthesis products in ammonia atmosphere followed by a crystallization process between 1200 and 1500°C.     

Different strategies for the synthesis of silicon carbide–silicon nitride composites from preceramic polymers

Three strategies for the synthesis of silicon carbide–silicon nitride composites from organosilicon preceramic polymers were investigated. Firstly, polymeric precursors with reactive groups for silicon carbide and silicon nitride were synthesized, blended and pyrolyzed. Secondly, a polymeric precursor for silicon carbide was mixed with silicon powder which acts as a reactive filler and the resulting mixtures were pyrolyzed. Thirdly, a co-polycyclodisilazane–silane single polymeric precursor was synthesized and pyrolyzed. The precursors and the various stages of processing were studied using gel permeation chromatography, Fourier transform-infrared spectroscopy, thermo-mechanical analysis, thermogravimetry and X-ray diffraction. In each instance silicon carbide–silicon nitride composites were prepared successfully.     

Commercial refrigeration – An overview of current status

Commercial refrigeration comprises food freezing and conservation in retail stores and supermarkets, so, it is one of the most relevant energy consumption sectors, and its relevance is increasing. This paper reviews the most recent developments in commercial refrigeration available in literature and presents a good amount of results provided these systems, covering some advantages and disadvantages in systems and working fluids. Latest researches are focused on energy savings to reduce CO₂ indirect emissions due to the burning of fossil fuels. They are focused on system modifications (as dedicated subcooling or the implementation of ejectors), trigeneration technologies (electrical, heating and cooling demand) and better evaporation conditions control. Motivated by latest GWP regulations that are intended to reduce high GWP HFC emissions; R404A and R507 are going to phase out. Besides hydrocarbons and HFO, CO₂ appears as one of the most promising HFC replacements because its low contribution to global warming and high efficiencies when used in transcritical and low-stage of cascade systems.     

Can the use of pulsed direct current induce oscillation in the applied pressure during spark plasma sintering?

The spark plasma sintering (SPS) process is known for its rapid densification of metals and ceramics. The mechanism behind this rapid densification has been discussed during the last few decades and is yet uncertain. During our SPS experiments we noticed oscillations in the applied pressure, related to a change in electric current. In this study, we investigated the effect of pulsed electrical current on the applied mechanical pressure and related changes in temperature. We eliminated the effect of sample shrinkage in the SPS setup and used a transparent quartz die allowing direct observation of the sample. We found that the use of pulsed direct electric current in our apparatus induces pressure oscillations with the amplitude depending on the current density. While sintering Ti samples we observed temperature oscillations resulting from pressure oscillations, which we attribute to magnetic forces generated within the SPS apparatus. The described current–pressure–temperature relations might increase understanding of the SPS process.     

Can the use of pulsed direct current induce oscillation in the applied pressure during spark plasma sintering?

Abstract

The spark plasma sintering (SPS) process is known for its rapid densification of metals and ceramics. The mechanism behind this rapid densification has been discussed during the last few decades and is yet uncertain. During our SPS experiments we noticed oscillations in the applied pressure, related to a change in electric current. In this study, we investigated the effect of pulsed electrical current on the applied mechanical pressure and related changes in temperature. We eliminated the effect of sample shrinkage in the SPS setup and used a transparent quartz die allowing direct observation of the sample. We found that the use of pulsed direct electric current in our apparatus induces pressure oscillations with the amplitude depending on the current density. While sintering Ti samples we observed temperature oscillations resulting from pressure oscillations, which we attribute to magnetic forces generated within the SPS apparatus. The described current–pressure–temperature relations might increase understanding of the SPS process.     

Cell control research— current status and development trends

A critical literature review on cell controller research is presented in this paper. Different definitions of a flexible manufacturing cell and cell controller are analysed, and comprehensive cell and cell controller definitions are given. Based on the requirements for a cell control system suggested by practitioners, users and researchers, a new set of general requirements for the development of a cell control system is proposed. After many well-known cell control systems are reviewed, a general structure of a cell controller and the general architecture of the cell control system, which includes a cell controller and a sub-system for the generation and configuration of a cell controller, are suggested. The scheduling approaches used in cell control are also discussed. The tools employed for modelling the cell control logic are examined. The trends and potential research directions in cell controller development are addressed.     

The α/β silicon nitride phase transformation

The literature on the / silicon nitride transformation is reviewed briefly. Data are presented on the kinetics of the tranformation of 1600° C on low and high purity silicon nitride powders. The addition of magnesia increased the rate of transformation while the addition of yttria had no effect. Scanning electron photomicrographs show clearly the morphology changes that accompany the transformation. It is concluded that the transformation occurs via a solution-precipitation mechanism and that and are probably low and high temperature forms of silicon nitride.     

TEM observation of liquid-phase bonded aluminum–silicon/aluminum nitride hetero interface

Liquid-phase bonded aluminum–silicon/aluminum nitride interface structure was investigated using high-resolution transmission electron microscopy. A textured layer of aluminum formed a stable orientation relationship with aluminum nitride, which showed Al(111) to be tilted by about 4° with respect to the AlN(0001) interface plane. The unique orientation relationship between Al and AlN was predicted as one of the stable orientation relationships using coincidence of reciprocal lattice point method, which surveys the degree of geometrical coherency between two crystals in three-dimensional space. A stable orientation relationship was found to be (001)[1_boxclose \bar{1} 0]Al//(2[`2] \bar{2} 03)[11[`2] \bar{2} 0]AlN.     

Pulse electric current sintering of hydroxyapatite/β-tricalcium phosphate composites

Hydroxyapatite (HA)/β-tricalcium phosphate (β-TCP) composites attract attentions as bone implant materials. As one of the fabrication method of HA/β-TCP is mixing of HA and β-TCP powder in advance of sintering. This method enables to control the ratio of content of β-TCP easier. However, it is difficult to obtain dense composites. In this study, we focused on pulse electric current sintering (PECS) to obtain dense HA/β-TCP composites. The sinterability is evaluated with relative density and grain size measurements. Composition of sintered body was also characterized by X-ray diffraction. In comparison with pressureless sintering, PECS increased relative density of the composites without grain growth. In HA/β-TCP sintered by PECS, the phase transformation from β-TCP to α-TCP was promoted. This is due to higher thermal energy by spark discharge during PECS. On the other hand, sintering additives (MgO) inhibited phase transformation. It was suggested that sinterability of HA/β-TCP composites was improved by PECS.     

Gallium nitride heterostructures on 3D structured silicon

We investigated GaN-based heterostructures grown on three-dimensionally patterned Si(111) substrates by metal organic vapour phase epitaxy, with the goal of fabricating well controlled high quality, defect reduced GaN-based nanoLEDs. The high aspect ratios of such pillars minimize the influence of the lattice mismatched substrate and improve the material quality. In contrast to other approaches, we employed deep etched silicon substrates to achieve a controlled pillar growth. For that a special low temperature inductively coupled plasma etching process has been developed. InGaN/GaN multi-quantum-well structures have been incorporated into the pillars. We found a pronounced dependence of the morphology of the GaN structures on the size and pitch of the pillars. Spatially resolved optical properties of the structures are analysed by cathodoluminescence.     

Reverse cyclic fatigue of a hot isostatically pressed silicon nitride at 1370 °C

The uniaxial, reverse cyclic fatigue performance of a commercially available hot isostatically pressed silicon nitride was examined at 1370 °C in air and with a 1 Hz sinusoidal waveform using button-head tensile specimens. Specimens did not fail in less than 10⁶ cycles when the applied stress amplitude was less than 280 MPa. Slow crack growth occurred at stress amplitudes 280 MPa and failure always occurred during the tensile stroke of the waveform. Multi-grain junction cavities resulted (i.e., the accumulation of net tensile creep strain) as a consequence of the reverse cyclic loading even though the specimens endured half their life under tensile stresses and the other half under compressive stresses. The presence of multi-grain junction cavities was a consequence of the stress exponent of tensile creep strain being greater than the stress exponent of compressive creep strain. Lastly, it was observed that the static creep resistance of this material improved when it was first subjected to reverse cyclic loading at 1370°C for at least 10⁶ cycles at 1 Hz. Silicon nitride grain coarsening (which was a consequence of the completion of the to silicon nitride solution/reprecipitation process that occurred during the history of the reverse cyclic loading) lessened the capacity for grain boundary sliding resulting in an improved static creep resistance.     

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.     

The effects of residual α phase on the 1370°C creep performance of yttria-doped HIPed silicon nitride

The creep behaviour at 1370°C (2500°F) of yttria-doped, hot isostatically pressed silicon nitride was examined as a function of residual phase content. The pre-test silicon nitride materials had either 30% or 40% phase content. The creep resistance was found to increase as the residual phase content decreased. For equivalent times and stresses, the higher -containing silicon nitride accumulated more creep strain and exhibited faster creep rates. The residual phase decreased as a function of time at 1370°C and converted to phase; it was also found that the to phase transformation rate was enhanced by stress. In the absence of stress, the kinetics of the to phase transformation at 1370°C followed a first-order reaction. If a first-order reaction was assumed for the to phase transformation in the presence of stress at 1370°C, then the magnitude of the reaction rate constant for this transformation was twice as large for tensile stresses equal to or greater than 130 MPa than for the reaction rate constant describing the transformation with no applied stress. © 1998 Chapman & Hall     

Hot-pressing and the α-β phase transformation in silicon nitride

The kinetics of densification and the kinetics of the- phase transformation have been measured during the hot-pressing of silicon nitride ceramics using magnesia as additive. Two mechanisms of densification have been identified. The first is a very rapid particle rearrangement, liquid-enhanced above 1550° C, which operates up to relative densities of about 0.65. The kinetics of the much slower decelerating second stage obey the Coble hot-pressing equation and the rate of densification is found to be proportional to the amount of additive. The controlling mechanism is believed to be diffusion in a boundary second phase, and values for the diffusion coefficient,D _b, of the rate-controlling species in the boundary phase for temperatures above and below 1550° C are given. The kinetics of the to transformation, the greater part of which occurs after densification is complete, are described by a first order reaction; the dependence of rate on the quantity of additive and on temperature is similar to that found for densification, and a similar controlling mechanism is believed to be responsible for the two processes.