Elastic behaviour of zirconium titanate bulk material at room and high temperature

Zirconium titanate (ZrTiO₄) is a well known compound in the field of electroceramics, however, its potential for structural applications has never been analysed. Moreover, it is compatible with zirconia, thus, zirconium titanate–zirconia composites might have potential for structural applications in oxidizing atmospheres. Nevertheless, there are currently no data about elastic properties of zirconium titanate materials in the literature. In view of the importance of these properties for the structural integrity of components subjected to high temperature and mechanical strains, an attempt was done in this work to determine the elastic properties of ZrTiO₄, both at room and high temperature. Young's modulus (161 ± 4 GPa), shear modulus (61 ± 1 GPa) and Poisson's ratio (0.32 ± 0.01) values at room temperature have been estimated for a fully dense single phase ZrTiO₄ material from experimental data of sintered single phase ZrTiO₄ materials with different porosities (6–19%). Values for room temperature Young's modulus are in agreement with those obtained by nanoindentation. Young's modulus up to 1400 °C shows an unusual dependence on temperature with no significant variation up to 500 °C an extremely low decrease from 500 to 1000 °C (≈0.02–0.03% every 100 °C) followed by a larger decrease that can be attributed to grain boundary sliding up to 1400 °C.     

Thermal shock resistance of magnesia–chrome refractories—experimental and criterial evaluation

Eleven commercially available magnesia–chrome refractories have been tested. Their basic properties have been determined along with bending strengths at 20,950 and 1400 °C, linear thermal expansion coefficients at 950 °C and 1400 °C, Young's modulus by the static method and the work of fracture at 950 °C. Young's modulus was determined within the temperature range 20–1000 °C, in the process of heating and cooling. The values of thermal shock resistance R_st and R₄ were calculated and correlated to thermal shock resistance (TSR). It has been demonstrated that the R_st criterion is a useful tool to forecast TSR, no matter whether the value of the E modulus is determined by the static or dynamic method. The values of Young's modulus obtained by various methods at 20 °C and 950 °C have been compared. It has been proven that Young's modulus dependence on temperature is a specific feature of a given material.     

Mechanical properties of alumina-rich magnesium aluminate spinel/tungsten composites

The mechanical properties and microstructure of alumina-rich magnesium aluminate spinel/tungsten (14 and 22 vol.% W) composites obtained by hot press at 1650 °C under reducing conditions have been investigated. The R-curve for these composites was estimated by the indentation strength method and compared with that of the monolithic spinel obtained under similar conditions. Rising R-curve behavior was specially observed in the composites when tungsten content was higher. Other mechanical properties such as hardness, toughness, Young's modulus and bending strength, were also determined for both (composites and monolithic magnesium aluminate). Higher values of bending strength were found as the metal volume fraction increases in the composite. The metal content dependence of Young's modulus and Vickers hardness follow the rule of mixtures. Mechanical properties and specially toughness are influenced by the metal content and its grain size.     

Mechanical characterization of a polysiloxane-derived SiOC glass

Silicon oxycarbide glass with the composition Si_1.0O_1.6C_0.8 was synthesized from a commercial polysiloxane by polymer pyrolysis. Dense SiOC samples were obtained by cross linking of the polysiloxane followed by warm pressing to form cylindrical samples and subsequent pyrolysis of the shaped polymer at 1100 °C in Ar. Hardness (H), Young's modulus (E) and Poisson's ratio (ν) of the as-prepared SiOC glass were evaluated from indentation studies and from acoustic microscopy. Indentation studies showed that E depends on the applied load and amounts to 90 GPa for low load and to 180 GPa for high load. Average values of 6.4 and 101 GPa were obtained for H and E, respectively, by the Vickers indentation method. Acoustic microscopy analysis yielded values of 96 GPa and 0.11 for E and ν, respectively. Compared to vitreous silica, the Young's modulus of the SiOC glass is about 1.3–1.5 times higher. To the knowledge of the present authors, the measured Poisson's ratio (ν = 0.11) is the lowest reported so far for glasses and polycrystalline ceramics.     

Elastic properties of translucent polycrystalline cubic boron nitride as characterized by the dynamic resonance method

Cubic boron nitride (cBN) is second only to diamond in a number of extreme material properties, and its performance exceeds diamond in many applications involving contact with ferrous alloys and/or high temperatures. However, its properties are less well understood. We have sintered cBN powder (2–4 μm or 8–12 μm particle size) into pure, translucent, polycrystalline compacts by pressing at a pressure of 7.7 GPa and temperatures from 2100 to 2350°C without any sintering agent. We have determined the Young's modulus E, shear modulus G, and Poisson's ratio ν of a number of translucent polycrystalline cBN compacts, in the form of free-standing disks, using the dynamic resonance method. The measured values for E, G, and ν lay in the ranges of 665–895 GPa, 295–405 GPa, and 0.11–0.15, respectively, depending on the grain size of the cBN starting material and the sintering temperature. These values may be compared with the theoretical values of E, G, and ν for pure, equiaxed, cBN of 909 GPa, 405 GPa, and 0.12, respectively. Combining the Young's modulus with previous Vickers hardness measurements, the fracture toughness K_IC of well-sintered translucent PCBN is evaluated as 6.8 MPa m^1/2. The dependence of the elastic properties on the synthesis conditions is discussed in the context of the microstructure and of related material properties.     

An estimate of quartz content and particle size in porcelain tiles from young's modulus measurements

The influence of quartz particle size, weight content and firing temperature on the Young's modulus of porcelain tiles was studied. To simulate a porcelain tile microstructure, an albite glass matrix with added crystalline quartz particles was developed. Average particle size of quartz (3.4 and 31 µm) and volume content (18.5 and 37.6 vol%) were varied. An acoustic impulse excitation technique was used to measure the elastic modulus from room temperature up to 700 °C. Results showed that quartz has a major influence on the elastic modulus of porcelain tiles. At temperatures below 573 °C, a hysteresis area between the Young's modulus curves during heating and cooling was closely related to quartz particle size. Between 573 and 700 °C, the variation of the Young's modulus was related to the quartz volume fraction. By using those correlations, a prediction of quartz content and quartz particle size in commercial porcelain materials can be carried out from Young´s modulus data.     

Effects of densification and mullitization on the evolution of the elastic properties of a clay-based material during firing

The microstructural evolution of an illito-kaolinitic raw material has been characterized during firing at 10 °C/min up to 1200 °C. The strong evolution of porosity and amount of mullite formed from the viscous flux (from 1000 °C) has been quantified using dilatometric measurement, image analysis and X-ray diffraction. In situ ultrasonic echography has been used in order to determine the Young's modulus (E) evolution associated to the microstructural changes. This technique is highly sensitive to porosity elimination and mullite development even though an abundant viscous flux is present. For low amount of mullite (<24.7 vol.%), the E evolution observed can be easily related to porosity and mullite volume proportion changes by applying the Hashin & Shtrikman approach (lower bound). For higher mullite content, the strong experimental E increase observed between 25.9 and 51.2 GPa has been related to the transition from isolated rigid inclusions (mullite and quartz) in soft matrix (viscous flux) toward a percolating network.     

Mechanical properties of ZrB2–SiC(ZrSi2) ceramics

Mechanical properties of ZrB₂–SiC and ZrB₂–ZrSi₂–SiC ceramics in the temperature range from 20 to 1400 °C were studied. It was found that the introduction of zirconium silicide resulted in pore-free ceramics having bending strengths of 400–500 MPa over a wide range of boride–carbide compositions. Zirconium silicide additive did not lead to significant strength and hardness changes at low temperature, but essentially increased Weibull modulus, and, therefore, the reliability of the ceramics. However, zirconium silicide additions resulted in noticeably reduced bending strength in ZrB₂–SiC based composites at 1400 °C.     

Nanoindentation study of nickel manganite ceramics obtained by a complex polymerization method

The chemical synthesis of nickel manganite powder was performed by a complex polymerization method (CPM). The obtained fine nanoscaled powders were uniaxially pressed and sintered at different temperatures: 1000–1200 °C for 2 h, and different atmospheres: air and oxygen. The highest density was obtained for the sample sintered at 1200 °C in oxygen atmosphere. The energy for direct band gap transition (Eg) calculated from the Tauc plot decreases from 1.51 to 1.40 eV with the increase of the sintering temperature. Indentation experiments were carried out using a three-sided pyramidal (Berkovich) diamond tip, and Young's modulus of elasticity and hardness of NTC (negative temperature coefficient) ceramics at various indentation depths were calculated. The highest hardness (0.754 GPa) and elastic modulus (16.888 GPa) are exhibited by the ceramics sintered at highest temperature in oxygen atmosphere.     

Columnar and DVC-structured thermal barrier coatings deposited by suspension plasma spray: high-temperature stability and their corrosion resistance to the molten salt

High-temperature stability of SPS YSZ coatings with the columnar and deep vertically cracked (DVC) structures and their corrosion resistance to 56 wt% V₂O₅+44 wt% Na₂SO₄ molten salt mixture were investigated. Both the columnar and DVC-structured YSZ coatings were sintered at 1000 °C, but a significant increase in porosity in combination with significant reductions in Vickers’ hardness and Young's modulus were observed at the temperatures from 1200 °C to 1400 °C. The DVC-structured YSZ coating exhibited superior corrosion resistance against the molten salt mixture attack to the columnar-structured one due to its higher density behaving as a sealing protective top layer at 950 °C.     

Mullite–zirconia–zircon composites: Properties and thermal shock resistance

In the refractory field mullite and zirconia are the basis of materials used in the glass industry or when high chemical stability and corrosion resistance are necessary. In this work various mullite–zirconia/zircon compositions were investigated to improve the thermal shock (TS) resistance of dense composites produced by slip casting and sintering at 1600 °C. Zircon (SiZrO₄) acts as bonding phase and its thermal decomposition adds zirconia and silica to the material. Resultant composites were characterized by density and dilatometric measurements, XRD and SEM techniques. TS behavior was tested by quenching in water with quenching temperature differentials ΔT from 400 to 1200 °C. The degree of damage after the TS was experimentally evaluated through the variation of the elastic modulus E which is measured by the excitation technique. The severity of the TS test and the effect of the number of thermal cycles on E for each ΔT employed were determined.The tested materials retained their original mechanical properties for temperatures below a critical temperature ΔT_c near 600 °C. Materials quenched from ΔT of 1000 °C showed as much as 30% reduction in E indicating the important microstructure damage. The TS resistance improved with increasing zircon addition to 35 wt% in agreement with the behavior predicted from R parameter for crack initiation.     

Mechanical behaviour of MgO–C refractory bricks evaluated by stress–strain curves

In this work, the mechanical behaviour of a set of resin- and pitch-bonded MgO–C refractories containing metallic additives was evaluated in laboratory tests at high temperature in a non-oxidant atmosphere. Commercial bricks were used for this evaluation, and a comprehensive characterization of the as-received materials was performed using several techniques (mineralogical analysis by X-ray diffraction, density and porosity measurements, differential thermal and thermogravimetric analyses and microstructural analysis by reflected light microscopy coupled with cathodoluminiscence accessory and scanning electron microscopy). Stress–strain curves in compression were obtained at room temperature, 600, 1000 and 1400 °C under flowing N₂ gas. An Instron 8501 servo-hydraulic machine was used with a capacitive extensometer suitable for axial strain measurements at high temperatures. A constant displacement of 0.1 mm/min was applied until specimen failure. Several parameters were calculated from the stress–strain curves: failure stress, failure strain, yield stress and secant Young's modulus. Moreover, a comprehensive characterization of the tested specimens was carried out. The analysis of the mechanical behaviour has been based on previous research and the results have been interpreted in terms of the thermal evolution of the brick's microstructure. The resin-based refractory exhibited the higher values of mechanical strength and Young's modulus in the entire range of testing temperatures. Up to 1000 °C, the mechanical behaviour was controlled by the type of binder and the changes in porosity whereas at 1400 °C, the main differences between the responses of resin- and pitch-based refractories were mainly caused by the metallic additive reactions.     

Mechanical and functional properties of Al2O3–ZrO2–MWCNTs nanocomposites

Multi-walled carbon nanotubes (MWCNTs) are often reported as additives improving mechanical and functional properties of ceramic composites. However, despite tremendous efforts in the field in the past 20 years, the results are still inconclusive. This paper studies room temperature properties of the composites with polycrystalline alumina matrix reinforced with 0.5–2 vol.% MWCNTs (composites AC) and zirconia toughened alumina with 5 vol.% of yttria partially stabilised zirconia (3Y-PSZ) containing 0.5–2 vol.% of MWCNTs (composites AZC). Dense composites were prepared through wet mixing of the respective powders with functionalised MWCNTs, followed by freeze granulation, and hot-pressing of granulated powders. Room temperature bending strength, Young's modulus, indentation fracture toughness, thermal and electrical conductivity of the composites were studied, and related to their composition and microstructure. Slight increase of Young's modulus, indentation fracture toughness, bending strength, and thermal conductivity was observed at the MWCNTs contents ≤1 vol.%. At higher MWCNTs contents the properties were impaired by agglomeration of the MWCNTs. The DC electrical conductivity increased with increasing volume fraction of the MWCNTs.     

Thermal shock behavior of nano-sized ZrN particulate reinforced AlON composites

Aluminum oxynitride (AlON) has been considered as a potential ceramic material for high-performance structural and advanced refractory applications owing to its excellent stability and mechanical properties such as high rigidity and good chemical stability. Thermal shock resistance is a major concern and an important performance index of refractories and high-temperature ceramics. While zirconium nitride (ZrN) particles have been proven to improve mechanical properties of AlON ceramic, the thermal shock behavior has not been evaluated yet. The aim of this investigation was to identify the thermal shock resistance and underlying mechanisms of hot-pressed 2.7% ZrN–AlON composites by a water-quenching technique over a temperature range between 225 °C and 275 °C. The residual strength and Young's modulus after thermal shock decreased with increasing temperature range and thermal shock times due to large temperature gradients and thermal stresses caused by abrupt water-quenching. The presence of nano-sized ZrN particles exhibited a positive effect on the improvement of both residual strength and critical temperature difference of AlON ceramic due to the toughening effects, the higher thermal conductivity of ZrN, the refined grain size and the reduction of porosity. Different toughening mechanisms including crack deflection, crack bridging and crack branching were observed during thermal shock experiments, thus effectively enhancing the crack initiation and propagation resistance and leading to a considerable improvement in thermal shock resistance in the ZrN–AlON composites.     

Isothermal and adiabatic Young's moduli of alumina and zirconia ceramics at elevated temperatures

The elastic moduli (Young's moduli) of alumina and zirconia ceramics with porosities ranging from almost dense (2–3%) to highly porous (46–52%), the latter prepared with starch as a pore-forming agent, have been measured via impulse excitation and four-point bending tests from room temperature up to more than 1200 °C. It is shown that, independent of the temperature and the material, the porosity dependence of the Young's modulus is well predicted by our exponential relation and that, irrespective of porosity, the temperature dependence follows a master curve that is characteristic of the material (for alumina exhibiting a decrease with a gradually growing tangent slope and for zirconia exhibiting a steep decrease with an inflection point at moderately elevated temperatures below 400 °C). Differences between isothermal (static) and adiabatic (dynamic) values are negligible as long as the materials are purely elastic (i.e. at temperatures below approximately 1000 °C).     

Mechanical properties of NiO/Ni–YSZ composites depending on temperature,porosity and redox cycling

The Impulse Excitation Technique (IET) was used to determine the elastic modulus and specific damping of different Ni/NiO–YSZ composites suitable for use in solid oxide fuel cells (SOFC). The porosity of the as-sintered samples varied from 9 to 38% and that of the reduced ones from 31 to 52%. For all samples a linear relation between Young's modulus and porosity was found. The temperature dependency of the mechanical properties of both as-sintered and reduced composites was investigated by IET up to 1200 °C. In the as-sintered state, first an increase and peak of stiffness coinciding with the Néel temperature, 250 °C, of NiO was observed. Above this temperature, a linear decrease occurred. Specific damping showed a peak at 170–180 °C and increased above ca. 1000 °C in NiO–YSZ. In the reduced state the elastic modulus decreased linearly with temperature; specific damping increased above ca. 600 °C and was found to be very dependent on microstructure. Damage caused by redox cycling degraded the elastic properties of the composites. Degradation started linearly from 0.5 to 0.6% redox strain leading to macroscopic sample failures at about 2.5% dL/L_o. A simple continuum elastic damage model was fitted to the degradation data.     

The impact of heat treatment on the microstructure of a clay ceramic and its thermal and mechanical properties

This paper presents the results of an experimental study on the microstructure, the thermal and the mechanical properties of a clay-based ceramic used in building applications. The X-ray tomography analysis showed a layered microstructure of clay with 200 µm sheets of porosity after the extrusion process. The gas release from the dehydration, dehydroxylation and decarbonation induced a 7 vol% formation of porosity during the heat treatment of the clay-based ceramic up to 850 °C. The porosity increase and the development of metakaolin led to a 38% decrease in the thermal conductivity. On the other hand, the Young's modulus of the clay-based ceramic was conserved due to the formation of smaller pores than the 200 µm sheets of porosity. The densification and the crystallization of amorphous phases also led to a 110% increase of the Young's modulus from 850 °C to 1050 °C. The Young's modulus of the clay-based ceramic was only decreased by the β→α quartz inversion of the cooling due to sand addition. Hence, this study provided a useful insight into how the microstructure of fired clay bricks can be specifically transformed by the porosity during the heat treatment to control the thermal and mechanical properties.     

Fabrication and characterization of PIP based C/SiC composites having improved mechanical properties using high modulus M40J carbon fiber as reinforcement

PIP based C/SiC composites are fabricated using high modulus M40J carbon fiber. High ceramic yield polycarbosilane (PCS) was also synthesized in the laboratory and the same was used to infiltrate the fibrous preforms. The infiltrated preforms were pyrolyzed at three different temperatures viz. 1400, 1500 and 1600 °C and termed as set-1, set-2 and set-3. Flexural strength was determined using 3-point bend fixture and the data obtained are analyzed using Weibull distribution. Average flexural strengths were found to be 691±23 MPa, 654.6±24 MPa, and 504±31 MPa for the sets 1, 2 and 3 respectively and the corresponding Weibull moduli were found to be 27.9, 25.5 and 15.6. The composites pyrolyzed at 1400 and 1500 °C, have been found to exhibit extensive fiber pull-out and thus demonstrated pseudo-ductile fracture behavior. A relatively brittle fracture was observed for the composites pyrolyzed at 1600 °C. Area under the flexural stress and displacement curve is found to be in the ratio 1.0:0.92:0.8 for the for the sets 1, 2 and 3 respectively. The effect of the pyrolysis temperature on the mechanical properties is discussed in the light of the microstructure of the composites.     

Young's modulus,thermal expansion coefficient and fracture behavior of selected Si–B–C based carbides in the 20–1200 °C temperature range as derived from the behavior of carbon fiber reinforced microcomposites

The Young's modulus, thermal expansion coefficient and fracture behavior of different ceramic phases in the Si–B–C system have been determined from room temperature up to 1200 °C using results of tests performed on matrix-dominated carbon fiber reinforced microcomposites by means of a specific high temperature testing apparatus. Results have shown that the boron-rich materials had higher stresses to failure and thermal expansion coefficients than silicon-rich materials whereas all the boron containing materials exhibited a viscoplastic time-dependant mechanical behavior over 1000 °C. The thermoelastic values of the Si–B–C based carbides thus obtained have been used to compute thermal residual stresses in model composite systems, in view of understanding some results reported in the literature regarding the implantation of layered matrices in ceramic matrix composites.