• Volume 24, Issue 2

April 2001,   pages  95-255

• Foreword

• Some numerical approaches of creep, thermal shock, damage and delayed failure of ceramics and refractories

Numerical simulation is now very often used to predict the behaviour of components in service conditions. This paper is interested in specific approaches concerning ceramic materials and refractories. Creep can be satisfactorily described by a kinematic hardening, and exhibits different creep rates in tension and compression. Concerning the thermal shock of materials, the numerical approach depends whether or not the material is able to develop a sprayed out damage, leading to micro- or macro-cracking. Finally, delayed failure at high temperature can be considered as a consequence of creep, but the random aspect of failure seriously complicates the numerical models. The lack of experimental data presently limits the calibration and the validation of the numerical models.

• Effect of zirconia addition on the fatigue behaviour of fine grained alumina

The fatigue behaviour of fine grained Al2O3 and ZrO2 toughened Al2O3 (ZTA) compositions with 15 vol% ZrO2 (3 mol% Y2O3 stabilized: 3Y-TZP) have been investigated by using three different techniques. Primarily 4-point bending load was employed to generate tension–tension fatigue data under both static and cyclic conditions. The results clearly showed that the materials were susceptible to both the static and cyclic fatigue and the time to failure under cyclic loading was considerably shorter than the equivalent static loads. The repeated indentations at the same spot with varying loads showed a typical fatigue behaviour. In addition, both the materials were subjected to the repeated impact cycles at varying subcritical loads simulating impact fatigue. In all the cases typical fatigue curves were obtained having a progressive endurance at subcritical loads having an endurance limit. The fatigue behaviour of Al2O3 was much improved by the addition of 15 vol% 3Y-TZP, having micro-plasticity contributing towards the cyclic fatigue phenomena of these materials.

• Indentation fatigue in silicon nitride, alumina and silicon carbide ceramics

Repeated indentation fatigue (RIF) experiments conducted on the same spot of different structural ceramics viz. a hot pressed silicon nitride (HPSN), sintered alumina of two different grain sizes viz. 1 𝜇m and 25 𝜇m, and a sintered silicon carbide (SSiC) are reported. The RIF experiments were conducted using a Vicker’s microhardness tester at various loads in the range 1–20 N. Subsequently, the gradual evolution of the damage was characterized using an optical microscope in conjunction with the image analysing technique. The materials were classified in the order of the decreasing resistance against repeated indentation fatigue at the highest applied load of 20 N. It was further shown that there was a strong influence of grain size on the development of resistance against repeated indentation fatigue on the same spot. Finally, the poor performance of the sintered silicon carbide was found out to be linked to its previous thermal history.

• Fracture resistance of 8 mol% yttria stabilized zirconia

An in situ technique for the assessment of fracture resistance employing double cantilever beam (DCB) specimens was developed in the present study. The side-grooved DCB specimens were loaded with pure bending moments in a specially designed and fabricated test fixture which went inside the specimen chamber of a scanning electron microscope. The study as conducted on a 8 mol% fully stabilized cubic phase yttria (Y2O3) stabilized zirconia (YSZ) ceramic. The powder processed sheets were sintered at 1600°C for 2 h in a zirconia tube furnace. The mode I applied energy release rate, 𝐺I was determined for both pure YSZ and treated YSZ. Two sets of experiments were conducted for the complete characterization of the ceramics. Three fracture toughness values were determined for the pure and treated ceramics, viz.

1. at the onset of the crack initiation, 𝐺ic,
2. at the arrest of a subcritical crack, 𝐺ia and
3. at the onset of the fast fracture, 𝐺if.

Two analyses of the experimental data were carried out, viz. method of extrapolation and statistical analysis. In case of the pure YSZ, a transgranular mode of the stable crack growth was identified to be predominant. The porous coating treatment appeared to have positive effects as the crack initiation resistance increased due to electrode layers. The stable crack growth behaviours of the ceramics were investigated by monitoring the crack growth velocity as a function of applied 𝐺 values. The results obtained were of direct significance in designing and fabrication of SOFC stacks.

• Fracture toughness and reliability in high-temperature structural ceramics and composites: Prospects and challenges for the 21st Century

The importance of high fracture toughness and reliability in Si3N4, and SiC-based structural ceramics and ceramic matrix composites is reviewed. The potential of these ceramics and ceramic matrix composites for high temperature applications in defence and aerospace applications such as gas turbine engines, radomes, and other energy conversion hardware have been well recognized. Numerous investigations were pursued to improve fracture toughness and reliability by incorporating various reinforcements such as particulate-, whisker-, and continuous fibre into Si3N4 and SiC matrices. All toughening mechanisms, e.g. crack deflection, crack branching, crack bridging, etc essentially redistribute stresses at the crack tip and increase the energy needed to propagate a crack through the composite material, thereby resulting in improved fracture toughness and reliability. Because of flaw insensitivity, continuous fibre reinforced ceramic composite (CFCC) was found to have the highest potential for higher operating temperature and longer service conditions. However, the ceramic fibres should display sufficient high temperature strength and creep resistance at service temperatures above 1000°C. The greatest challenge to date is the development of high quality ceramic fibres with associate coatings able to maintain their high strength in oxidizing environment at high temperature. In the area of processing, critical issues are preparation of optimum matrix precursors, precursor infiltration into fibre array, and matrix densification at a temperature, where grain crystallization and fibre degradation do not occur. A broad scope of effort is required for improved processing and properties with a better understanding of all candidate composite systems.

• Mechanical characteristics of microwave sintered silicon carbide

The present work deals with the sintering of SiC with a low melting additive by microwave technique. The mechanical characteristics of the products were compared with that of conventionally sintered products. The failure stress of the microwave sintered products, in biaxial flexure, was superior to that of the products made by conventional sintering route in ambient condition. In firing of products by conventionally sintered process, SiC grain gets oxidized producing SiO2 (∼ 32 wt%) and deteriorates the quality of the product substantially. Partially sintered silicon carbide by such a method is a useful material for a varieties of applications ranging from kiln furniture to membrane material.

• Mechanical characterization of microwave sintered zinc oxide

The mechanical characterization of microwave sintered zinc oxide disks is reported. The microwave sintering was done with a specially designed applicator placed in a domestic microwave oven operating at a frequency of 2.45 GHz to a maximum power output of 800 Watt. These samples with a wide variation of density and hence, of open pore volume percentage, were characterized in terms of its elastic modulus determination by ultrasonic time of flight measurement using a 15 MHz transducer. In addition, the load dependence of the microhardness was examined for the range of loads 0.1–20 N. Finally, the fracture toughness data (𝐾IC) was obtained using the indentation technique.

• Effect of alkali treated jute fibres on composite properties

Jute fibres were subjected to a 5% alkali (NaOH) solution treatment for 0, 2, 4, 6 and 8 h at 30°C. An improvement in the crystallinity in the jute fibres increased its modulus by 12%, 68% and 79% after 4, 6 and 8 h of treatment respectively. The tenacity of the fibres improved by 46% after 6 and 8 h treatment and the % breaking strain was reduced by 23% after 8 h treatment. For the 35% composites with 4 h treated fibres, the flexural strength improved from 199.1 MPa to 238.9 MPa by 20%, modulus improved from 11.89 GPa to 14.69 GPa by 23% and laminar shear strength increased from 0.238 MPa to 0.2834 MPa by 19%. On plotting the different values of slopes obtained from the rates of improvement of the flexural strength and modulus, against the NaOH treatment time, two different failure modes were apparent before and after 4 h of treatment. In the first region between 0 and 4 h, fibre pull out was predominant whereas in the second region between 6 and 8 h, transverse fracture occurred with a minimum fibre pull out. This observation was well supported by the SEM investigations of the fracture surfaces.

• Behaviour of 𝐸-glass fibre reinforced vinylester resin composites under impact fatigue

An impact fatigue study has been made for the first time on 63.5% glass fibre reinforced vinylester resin notched composites. The study was conducted in a pendulum type repeated impact apparatus especially designed and fabricated for determining single and repeated impact strengths. A well-defined impact fatigue (S–N) behaviour, having a progressive endurance below the threshold single cycle impact fracture stress with decreasing applied stress has been demonstrated. Fractographic analysis revealed fracture by primary debonding having fibre breakage and pullout at the tensile zone, but a shear fracture of fibre bundles at the compressive zone of the specimen. The residual strength, modulus and toughness showed retention of the properties at high impact stress levels up to 1000 impacts followed by a sharp drop. Cumulative residual stresses with each number of impacts not withstanding the static fatigue failure at long endurances have been ascribed for the composite failures under the repeated impact stresses.

• Failure analysis of multiple delaminated composite plates due to bending and impact

The present work aims at the first ply failure analysis of laminated composite plates with arbitrarily located multiple delaminations subjected to transverse static load as well as impact. The theoretical formulation is based on a simple multiple delamination model. Conventional first order shear deformation is assumed using eight-noded isoparametric quadratic elements to develop the finite element analysis procedure. Composite plates are assumed to contain both single and multiple delaminations. For the case of impact, Newmark time integration algorithm is employed for solving the time dependent multiple equations of the plate and the impactor. Tsai-Wu failure criterion is used to check for failure of the laminate for both the cases. To investigate the first ply failure, parametric studies are made for different cases by varying the size and number of delaminations as well as the stacking sequences and boundary conditions.

• Mechanical properties of very thin cover slip glass disk

The biaxial flexural strength, Young’s modulus, Vicker’s microhardness and fracture toughness data for very thin, commercial, soda-lime-silica cover slip glass (diameter, D-18 mm, thickness, T-0 3 mm; T/D ≈ 0.02) are reported here. The ball on ring biaxial flexure tests were conducted at room temperature as a function of the support ring diameter (≈10–20 mm) and cross head speed (0.1–10 mm min–1). In addition, the Weibull modulus data were also determined. The Young’s modulus data was measured using a linear variable differential transformer (LVDT) from biaxial flexure tests and was checked out to be comparable to the data obtained independently from the ultrasonic time of flight measurement using a 15 MHz transducer. The microhardness data was obtained for the applied load range of 0.1–20 N. The fracture toughness (𝐾IC) data was obtained by the indentation technique at an applied load of 20 N.

• Cracking phenomena in lithium-di-silicate glass ceramics

Lithium-di-silicate glass ceramic (Li2O, SiO2) with uniformly oriented crystals was placed on a Vickers indentation with extrusion axis horizontally parallel to the base axis. The material was rotated through 0°– 90° and at each angle a 20 N load was applied to ascertain the crack path. It was observed that the crack length decreases and the crack deviates from its original path with increasing angle. The deviation of the crack was correlated with the component of the crack driving force and the theoretical strength of the aligned crystals at different angles.

• Critical fatigue behaviour in brittle glasses

The dynamic fatigue fracture behaviour in different glasses under various sub-threshold loading conditions are analysed here employing an anomalous diffusion model. Critical dynamical behaviour in the time-to-fracture and the growth of the micro-crack sizes, similar to that observed in such materials in the case of quasi-static (instantaneous”) failures for above-threshold conditions, are predicted and compared with some of the experimental observations in different glasses.

• Stress relaxation and estimation of activation volume in a commercial hard PZT piezoelectric ceramic

The stress relaxation of ferroelectric/piezoelectric material was studied using compression testing. The deformation was produced by the switching of ferroelectric domains. The internal stresses were estimated by decremental stress relaxation during unloading. The results were interpreted in terms of reversible and irreversible switching of the domains.

• Effect of stress ratio and frequency on fatigue crack growth rate of 2618 aluminium alloy silicon carbide metal matrix composite

Effect of stress ratio and frequency on the fatigue crack propagation of 2618 aluminium alloy–silicon carbide composite were investigated at ambient temperature. With the first set of specimens, the fatigue crack growth rates were studied at three frequencies of 1 Hz, 5 Hz and 10 Hz at a stress ratio of 0.1 whereas the effects of stress ratios of 0.1, 0.25 and 0.50 were studied with the second set of specimens. The study showed that the fatigue crack propagation behaviour of this metal matrix composite was influenced to an appreciable extent by the stress ratio, but not by the fatigue frequencies used in this investigation.

• Particle fracture and plastic deformation in vanadium pentoxide powders induced by high energy vibrational ball-mill

An X-ray powder profile analysis in vanadium pentoxide powder milled in a high energy vibrational ball-mill for different lengths of time (0–250 h), is presented. The strain and size induced broadening of the Bragg reflection for two different crystallographic directions ([001] and [100]) was determined by Warren–Averbach analysis using a pattern-decomposition method assuming a Pseudo–Voigt function. The deformation process caused a decrease in the crystallite size and a saturation of crystallite size of ∼ 10 nm was reached after severe milling. The initial stages of milling indicated a propensity of size-broadening due to fracture of the powder particles caused by repeated ball-to-powder impact whereas with increasing milling time microstrain broadening was predominant. WA analysis indicated significant plastic strain along with spatial confinement of the internal strain fields in the crystallite interfaces. Significant strain anisotropy was noticed in the different crystallographic directions. A near-isotropy in the crystallite size value was noticed for materials milled for 200 h and beyond. The column-length distribution function obtained from the size Fourier coefficients progressively narrowed down with the milling time.

• Study of indentation induced cracks in MoSi2-reaction bonded SiC ceramics

MoSi2–RBSC composite samples were prepared by infiltration of Si–2 at.% Mo melt into a preform of commercial SiC and petroleum coke powder. The infiltrated sample had a density > 92% of the theoretical density (TD) and microstructurally contained SiC, MoSi2, residual Si and unreacted C. The material was tested for indentation fracture toughness at room temperature with a Vicker’s indenter and KIC was found to be 4.42 MPa√m which is around 39% higher than the conventional RBSC material. Enhancement in indentation fracture toughness is explained in terms of bowing of propagating cracks through MoSi2/SiC interface which is under high thermal stress arising from the thermal expansion mismatch between MoSi2 and SiC.

• Stereological characterization of crack path transitions in ceramic matrix composites

All ceramic composites involve a mismatch in physical properties the extent of which differs from one composite to another. Mismatch in thermal expansion (𝛥 𝛼) and elastic modulus (𝛥E) is known to produce stresses that influence the path of a propagating crack. Thus, the relative effect of thermal and elastic mismatch on the crack path is expected to change with change in stress intensity. We propose that the crack path in ceramic composites should undergo a transition with the crack being strongly influenced by the thermal mismatch stresses at low stress intensity and elastic mismatch stresses at high stress intensities. Thus, a material in use under different applications each with its own loading conditions is expected to exhibit different crack propagation tendencies which may be reflected in the 𝑣–𝐾 characteristics of the composite material. In the present work several model composites with different combinations of thermal and elastic mismatch have been considered. Cracks propagating at different sub-critical stress intensities (velocities) were generated by a novel indentation technique. Each indentation was performed at a constant displacement rate and a peak load. A range of displacement rates were used to produce cracks propagating at different velocities. The indentations were made using a Vickers indentor fitted in a universal mechanical testing machine. The crack paths in composites were quantified by stereological technique and the proposed theory was verified.

• Densification and mechanical properties of mullite–SiC nanocomposites synthesized through sol–gel coated precursors

Mullite–SiC nanocomposites are synthesized by introducing surface modified sol–gel mullite coated SiC particles in the matrix and densification and associated microstructural features of such precursor are reported. Nanosize SiC (average size 180 nm) surface was first provided with a mullite precursor coating which was characterized by the X-ray analysis and TEM. An average coating thickness of 120 nm was obtained on the SiC particles. The green compacts obtained by cold isostatic pressing were sintered in the range 1500–1700°C under pressureless sintering in the N2 atmosphere. The percentage of the theoretical sintered density decreases with increase in SiC content. A maximum sintered density of 97% was achieved for mullite–5 vol.% SiC. The fractograph of the sintered composite showed a highly dense, fine grained microstructure with the SiC particles uniformly distributed along the grains as well as at the grain boundaries inside the mullite. The Vicker’s microhardness of mullite–5 vol.% SiC composite was measured as 1320 kg/mm2 under an applied indentation load of 500 𝑔. This value gradually decreased with an increase in SiC content.

• Mechanical properties of glass polymer multilayer composite

The preliminary experimental studies on the comparative behaviour of the deformation processes involved in the failure of a commercial, 0.3 mm thick, 18 mm diameter soda–lime–silica glass disks (𝐺) and multilayered glass disk–epoxy (GE) as well as glass disk–epoxy–𝐸-glass fabric (GEF) composite structures are reported. The failure tests were conducted in a biaxial flexure at room temperature. The epoxy was a commercial resin and the 𝐸-glass fabric was also commercially obtained as a two-dimensional weave of 𝐸-glass fibres to an area density of about 242 g m–2. The multilayered structures were developed by alternate placement of the glass and reinforcing layers by a hand lay-up technique followed by lamination at an appropriate temperature and pressure. Depending on the number of layers the volume fraction of reinforcement could be varied from about 0.20 for the GE system to about 0.50 for the GEF system. It was observed that the specific failure load (load per unit thickness) was enhanced from a value of about 60 N/mm obtained for the glass to a maximum value of about 100 N/mm for the GE composites and to a maximum of about 70 N/mm for the GEF composite system. Similarly, the displacements at failure (𝛿) measured with a linear variable differential transformer (LVDT) were also found to be a strongly sensitive function of the type of reinforcement (GE or GEF) as well as the number of layers.

• Crack propagation studies and bond coat properties in thermal barrier coatings under bending

Ceramic based thermal barrier coatings (TBC) are currently considered as a candidate material for advanced stationary gas turbine components. Crack propagation studies under bending are described that were performed on plasma sprayed ZrO2, bonded by MCrAlY layer to Ni base superalloy. The crack propagation behaviour of the coatings at room temperature in as received and oxidized conditions revealed a linear growth of the cracks on the coating till the yield point of the super alloy was reached. High threshold load at the interface between the ceramic layer and the bond coat was required to propagate the crack further into the bond coat. Once the threshold load was surpassed the crack propagated into the brittle bond coat without an appreciable increase in the load. At temperatures of 800°C the crack propagated only in the TBC (ceramic layer), as the ductile bond coat offered an attractive sink for the stress relaxation. Effects of bond coat oxidation on crack propagation in the interface region have been examined and are discussed.

• Macroporous silica–alumina composites with mesoporous walls

Macroporous silica–alumina composites with mesopores have been prepared by employing polymethylmethacrylate beads as templates in the presence of the cationic surfactant, N-cetyl-N,N,N-trimethylammonium bromide. The Si/Al ratio in the composites has been varied between 4.5 and 48 and the occurrence of mesopores has been verified by X-ray diffraction. The surface areas of the samples vary between 676 and 1038 m2g–1, with the highest value in the sample with Si/Al = 48.

• High temperature flow behaviour of SiC reinforced lithium aluminosilicate composites

The compressive flow behaviour of lithium aluminosilicate (LAS) glass, with and without SiC particulate reinforcements, was studied. The LAS glass crystallized to 𝛽 spodumene during high-temperature testing. The flow behaviour of LAS glass changed from Newtonian to non-Newtonian due to the presence of crystalline phase. Further, with the addition of 40 vol.% SiC additions, the strain rate sensitivity of flow stress decreased. While the activation energy for flow in LAS was 300 kJ/mole, it increased to 995 kJ/mole with the addition of 40 vol.% SiC reinforcements.

• Effect of filler addition on the compressive and impact properties of glass fibre reinforced epoxy

Flyash is incorporated in glass fibre reinforced epoxies to study their response to the filler addition. Low cost of flyash can reduce the overall cost of the component. Only very low volume fractions of filler are investigated in the present study. To obtain further clarification of the observed phenomenon, another abundantly available low cost material, calcium carbonate is incorporated in one set of the specimens. Compressive strength of the material is found to decrease, whereas steep increase in impact strength is observed by introduction of very small quantity of fillers. Specimens containing calcium carbonate are tested for impact properties only. Effect of specimen aspect ratio on the compressive strength values is also studied by testing specimens of three different aspect ratios. Scanning electron microscopic observations are taken to develop a better understanding of the phenomena taking place in the material system at microscopic level.

• A detailed model for defect concentration and dopant activation in GaAs

Defects in semi-insulating (SI) GaAs are especially critical in determining the properties of devices in which dopants are introduced by ion-implantation. The defects in GaAs are native to the material and their concentrations are subsequently modified after ion-implantation and annealing. In this work, we have extended the existing models in the literature by incorporating a large set of defects and using the most recent values for formation energies of these defects. The model includes eight types of point defects, the vacancy of Ga and As, their antisites and interstitials of Ga and As on both sub-lattices, along with carbon related defects always present in SI–GaAs. We have also included Si and related defects when this element is implanted as an 𝑛-type dopant. All these defects are considered in several charge states allowed by their stability conditions. The model assumes thermodynamic equilibrium between the point defects at an anneal temperature. Then the GaAs wafer is quenched so that the number of defects remain the same as those at the anneal temperature, but redistribution of charges occurs in various charge states. We find that the defect concentrations are extremely sensitive to the crystal stoichiometry, and good agreement with experimental data is shown. However, when we calculate the dopant activation in implanted GaAs, the quantitative agreement with experiments is not adequate. This discrepancy is explained on the basis of available formation energies for the defects.

• Study of fatigue behaviour of 7475 aluminium alloy

Fatigue properties of a thermomechanically treated 7475 aluminium alloy have been studied in the present investigation. The alloy exhibited superior fatigue life compared to conventional structural aluminium alloys and comparable stage II crack growth rate. It was also noticed that the fatigue crack initiated from a surface grain and the crack extension was dominated by ductile striations. Analysis also revealed that this alloy possessed fracture toughness and tensile properties superior to that noticed with other structural aluminium alloys. Therefore the use of this alloy can safely reduce the overall weight of the aircraft.

• Catalytic activity of polymer-bound Ru(III)–EDTA complex

Chloromethylated styrene–divinylbenzene copolymer was chemically modified with ethylenediaminetetraacetic acid ligand. Catalytically active polymer containing Ru(III) moieties were synthesized from this polymeric ligand. They were characterized using FTIR, UV-vis, SEM, ESR and TGA. Other physico-chemical properties such as bulk density, surface area, moisture content and swelling behaviour in different solvents were also studied. The polymer bound complex was used to study hydrogenation of 1-hexene to 𝑛-hexane under mild conditions. Influence of [1-hexene], [catalyst], temperature and nature of the solvent on the rate of the reaction was investigated. A rate expression is proposed based on the observed initial rate data. Recycling efficiency of the catalyst has also been studied.

• Studies on compensating valency substituted BaTi(1-𝑥)Mn𝑥/2Nb𝑥/2O3 ceramics

The paper reports investigations of relative permittivity, 𝜀𝑟, electrical conductivity, 𝜎, saturation polarization, 𝑃𝑠, infrared absorption and structural properties of compensating valency substituted BaTiO3. The compositions investigated are BaTi(1-𝑥)Mn𝑥/2Nb𝑥/2O3 for 𝑥 = 0.00; 0.025; 0.05; 0.1; 0.2; 0.4. The compositions for 𝑥 < 0.1 are observed to be ferroelectric and the transition temperature and value of 𝜀𝑟 are observed to decrease as concentration of substitution is increased. The dielectric investigations are carried out on two sets of samples

1. as sintered and
2. annealed.

Annealing is observed to improve quality factor `𝑄' of the materials with a consequent reduction in the 𝜀𝑟. The observations on 𝜀𝑟 and saturation polarization suggest that additional material engineering efforts are required to improve the material properties.

• Thermal behaviour of strontium tartrate single crystals grown in gel

Thermal behaviour of strontium tartrate crystals grown with the aid of sodium metasilicate gel is investigated using thermogravimetry (TG) and differential thermal analysis (DTA). Effect of magnetic field and dopant (Pb)2+ on the crystal stability is also studied using thermal analysis. This study reveals that water molecules are locked up in the lattice with different strengths in the grown crystals.

• Analysis of corrosive environmental factors of seabed sediment

The corrosivity of seabed sediment at spots at different distances from seashore was studied based on in situ investigations in the northern sea area of the Yellow River mouth. The results show that there is close relation between distance from seashore and corrosivity of seabed sediment.

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