Early stage cavitation erosion within ceramics—An experimental investigation

Six ceramic material types were considered within an experimental investigation to identify the erosion damage mechanisms resulting from cavitation exposure. These materials were a Y-TZP-type zirconia, different commercially available silicon nitrides, a high-purity alumina and a hardened high-nitrogen stainless steel as reference. An ultrasonic transducer was utilised to produce cavitation conditions and the configuration was “static specimen method” using a 5-mm diameter probe, 20-kHz and 50-μm amplitude. The exposure times were periods from 15 s to 3 h.Experimental methods employed to characterise wear mechanisms were light microscopy, scanning light interferometry and scanning electron microscopy.It was found that the zirconia and silicon nitrides demonstrated evidence of local pseudo-plastic deformation or depression prior to more pronounced erosion damage by fracture. Zirconia showed evidence of delayed surface changes when the sample is at rest stored in air, possibly by spontaneous phase transformation after the completion of the erosion tests. Alumina showed evidence of brittle surface fracture and negligible or no pseudo-plastic deformation. All wear mechanisms are discussed, and the materials are ranked in terms of cavitation resistance performance.     

Investigation of the effect of ZrO2 and ZrO2/Al2O3 additions on the hot-pressing and properties of equimolecular mixtures of α- and β-Si3N4

In this work, hot-pressing of equimolecular mixtures of α- and β-Si₃N₄ was performed with addition of different amounts of sintering additives selected in the ZrO₂–Al₂O₃ system. Phase composition and microstructure of the hot-pressed samples was investigated. Densification behavior, mechanical and thermal properties were studied and explained based on the microstructure and phase composition. The optimum mixture from the ZrO₂–Al₂O₃ system for hot-pressing of silicon nitride to give high density materials was determined. Near fully dense silicon nitride materials were obtained only with the additions of zirconia and alumina. The liquid phase formed in the zirconia and alumina mixtures is important for effective hot-pressing. Based on these results, we conclude that pure zirconia is not an effective sintering additive. Selected mechanical and thermal properties of these materials are also presented. Hot-pressed Si₃N₄ ceramics, using mixtures from of ZrO₂/Al₂O₃ as additives, gave fracture toughness, K_IC, in the range of 3.7–6.2 MPa m^1/2 and Vicker hardness values in the range of 6–12 GPa. These properties compare well with currently available high performance silicon nitride ceramics. We also report on interesting thermal expansion behavior of these materials including negative thermal expansion coefficients for a few compositions.     

Synthesis and mechanical and tribological characterization of alumina–yttria stabilized zirconia (YSZ) nanocomposites with YSZ synthesized by means of an aqueous solution–gel method or a hydrothermal route

In the present study, yttria stabilized zirconia (YSZ) nanoparticles, prepared by means of an aqueous solution–gel method or a hydrothermal route, are incorporated in a matrix of submicron alumina particles by wet mechanical milling. The microstructural characteristics and the mechanical and tribological properties of the obtained alumina–YSZ nanocomposites are evaluated as a function of different processing conditions like milling time, YSZ amount, sintering procedure and synthesis method of YSZ.     

Influence of corrosion and mechanical loads on advanced ceramic components

Advanced oxide ceramics are prospective materials for severe application conditions, including corrosion, particularly, in oxygen-rich environments, combined with the action of mechanical loads. The corrosion behavior and mechanical strength decrease of oxide ceramics, such as high alumina, alumina–mullite and zirconia-based ceramics, were studied in water steam supercritical conditions (elevated temperatures and pressures). The strength decrease under the action of the studied aggressive environment is mostly dealt with the glassy phase dissolution and intergranular corrosion for alumina–mullite and high alumina ceramics, while degradation of zirconia-based ceramics is also dealt with the phase transformation. The influence of structure defects related to processing of the ceramics on corrosion is considered.     

Phase stability and hot corrosion behavior of ZrO2–Ta2O5 compound in Na2SO4–V2O5 mixtures at elevated temperatures

For thermal barrier coating (TBC) applications, yttria stabilized zirconia (YSZ) is susceptible to hot corrosion. This paper examines the hot corrosion performance of ZrO₂/Ta₂O₅ compounds. Different compositions of ZrO₂–Ta₂O₅ samples in the presence of molten mixture of Na₂SO₄+V₂O₅ at 1100 °C were tested. The compositions were selected to form tetragonal and orthorhombic phases of zirconium-tantalum oxides. Results show that orthorhombic zirconium-tantalum oxide is more stable, both thermally and chemically in Na₂SO₄+V₂O₅ media at 1100 °C, and shows a better hot corrosion resistance than the tetragonal phase.     

Investigation on mechanochemical synthesis of Al2O3/BN nanocomposite by aluminothermic reaction

Alpha-alumina–boron nitride (α-Al₂O₃–BN) nanocomposite was synthesized using mixtures of aluminum nitride, boron oxide and pure aluminum as raw materials via mechanochemical process under a low pressure of nitrogen gas (0.5 MPa). The phase transformation and structural evaluation during mechanochemical process were investigated by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and differential thermal analysis (DTA) techniques. The results indicated that high exothermic reaction of Al–B₂O₃ systems under the nitrogen pressure produced alumina, aluminum nitride (AlN), and aluminum oxynitride (Al₅O₆N) depending on the Al value and milling time, but no trace of boron nitride (BN) phases could be identified. On the other hand, AlN addition as a solid nitrogen source was effective in fabricating in-situ BN phase after 4 h milling process. In Al–B₂O₃–AlN system, the aluminothermic reaction provided sufficient heat for activating reaction between B₂O₃ and AlN to form BN compound. DTA analysis results showed that by increasing the activation time to 3 h, the temperature of both thermite and synthesis reactions significantly decreased and occurred as a one-step reaction. SEM and TEM observations confirmed that the range of particle size was within 100 nm.     

Crystallization behaviour and hardness of glass ceramics rich in nanocrystals of ZrO2

This research is mainly directed toward the development of hardness of glass ceramic by adding different amounts of ZrO₂ to the glass and by applying different heat-treatments. Differential thermal analysis (DTA), X-ray diffraction (XRD) and Scanning electron microscope (SEM) were used to study the crystallization behaviour of the glass samples. The only observed crystalline phases were tetragonal and monoclinic zirconia. Hardness was found to increase by increasing time and temperature of heat-treatment due to the formation of monoclinic phase as a result of the martensitic reaction. This transformation opposes crack opening.     

Studies on ionic conductivity of stabilized zirconia ceramics (8YSZ) densified through conventional and non-conventional sintering methodologies

Densification studies of 8 mol% yttria stabilized zirconia ceramics were carried out by employing the sintering techniques of conventional ramp and hold (CRH), spark plasma sintering (SPS), microwave sintering (MWS) and two-stage sintering (TSS). Sintering parameters were optimized for the above techniques to achieve a sintered density of >99% TD. Microstructure evaluation and grain size analysis indicated substantial variation in grain sizes, ranging from 4.67 μm to 1.16 μm, based on the sintering methodologies employed. Further, sample was also sintered by SPS technique at 1425 °C and grains were intentionally grown to 8.8 μm in order to elucidate the effect of grain size on the ionic conductivity. Impedance spectroscopy was used to determine the grain and grain boundary conductivities of the above specimens in the temperature range of RT to 800 °C. Highest conductivity of 0.134 S/cm was exhibited by SPS sample having an average grain size of 1.16 μm and a decrease in conductivity to 0.104 S/cm was observed for SPS sample with a grain size of 8.8 μm. Ionic conductivity of all other samples sintered vide the techniques of TSS, CRH and MWS samples was found to be ∼0.09 S/cm. Highest conductivity irrespective of the grain size of SPS sintered samples, can be attributed to the low densification temperature of 1325 °C as compared to other sintering techniques which necessitated high temperatures of ∼1500 °C. The exposure to high temperatures while sintering with TSS, CRH and MWS resulted into yttria segregation leading to the depletion of yttria content in fully stabilized zirconia stoichiometry as evidenced by Energy Dispersive Spectroscopy (EDS) studies.     

Fabrication and characteristic of non-oxide fiber tow reinforced silicon nitride matrix composites by low temperature CVI process

Non-oxide fiber tow reinforced silicon nitride matrix composite was fabricated by low temperature CVI process with PyC as interphase. The tensile strength of the C and SiC fiber tow composites were 547 MPa and 740 MPa, respectively. The difference in tensile strength was analyzed based on the length, amount of pull-out fiber and also interface bonding. The infiltration uniformity of CVI silicon nitride (SiN) matrix within SiC fiber tow was comparable with that of CVI SiC matrix. These results suggested that the low temperature CVI process is suitable for the fabrication of fiber reinforced SiN matrix composites with proper interface bonding and high strength.     

Microstructure, mechanical properties and thermal shock resistance of plasma sprayed nanostructured zirconia coatings

Nanostructured yttria stabilized zirconia (YSZ) coatings were deposited by Atmospheric Plasma Spraying (APS). X-ray diffraction (XRD) was used to investigate their phase composition, while scanning electron microscopy (SEM) was employed to examine their microstructure. The coatings showed a unique and complex microstructure composed of well-melted splats with columnar crystal structure, partially melted areas, which resembled the morphology of the powder feedstock, and equiaxed grains. Vickers microhardness of nanostructured zirconia coatings was similar to that of the conventional ones and strongly depended on the indentation load. Otherwise, a higher thermal shock resistance was found. This effect was addressed to the retention of nanostructured areas in coating microstructure and to the corresponding high porosity.     

Thermal cyclic behavior of glass–ceramic bonded thermal barrier coating on nimonic alloy substrate

Thermal barrier coating system comprised of 8 wt.% yttria stabilized zirconia (YSZ) top coat, glass–ceramic bond coat and nimonic alloy (AE 435) substrate was subjected to thermal shock test from 1000 °C to room temperature for 100 cycles. Two types of thermal shock testing were performed. In one test, specimens held at 1000 °C for 5 min were forced air quenched while in the other test specimens were water quenched from the same conditions. Microstructural changes were investigated by scanning electron microscopy (SEM) and phase analysis was conducted by XRD and energy dispersive X-ray (EDX) analysis. In the case of forced air quenched specimens, no deterioration was observed in the top coats after 100 cycles while the top coats were damaged in the water quenched ones. In both forced air quenched and water quenched specimens, interfacial crack was not observed at the top coat–bond coat and bond coat–substrate interfaces after thermal cycling experiments and the top coat maintained its phase stability.     

Compressive creep behavior of spark plasma sintered La2O3–YSZ composite

The present paper describes compressive creep behavior of cubic 8 mol% yttria stabilized zirconia+10 mol% La₂O₃ (fabricated by Spark Plasma Sintering) in the temperature range of 1300–1330 °C at a stress level of 45–78 MPa in vacuum. The pre- and post-creep microstructures, relative magnitudes of the stress exponent (n=1.7–2.1) and the activation energy (540–580 kJ/mol) suggest that grain boundary sliding aided by inter-diffusion of La and Zr leading to the formation of pyrochlore La_1.6Y_0.4Zr₂O₇ phase at the grain boundaries during creep is the active creep mechanism in this composite.     

Preparation and characterization of ZTA bioceramics with and without gradient in composition

Properties and proof of suitability of homogeneously and graded ZTA bioceramics with various Y₂O₃ stabilized zirconia contents were investigated. Therefore porous alumina was infiltrated with different amounts of Y₂O₃ doped ZrO₂ precursors. At homogeneously infiltrated samples biaxial flexural strength and wear behavior were investigated (ISO 6474). Subsequently, at hip joint heads the static fracture strength was determined (ISO 7206-10). Materials ranging from approx. 4 to 20 wt% Y₂O₃ stabilized zirconia were characterized relative to the sinter density, the microstructure, the phase composition and the dispersion of the stabilized zirconia phase. Bioceramics showed high sinter density, fine microstructures, excellent wear property and significantly increased biaxial flexural strength. A 41% increase in strength through the formation of Y₂O₃ stabilized zirconia gradient in the conical bore of the heads was reached. Low compressive stresses in cone of this heads were found.ZTA bioceramics are potentially suitable for use as hip replacement components.     

Determination of structural and mechanical properties of multilayer graphene added silicon nitride-based composites

Silicon nitride based nanocomposites have been prepared with different amount (1 and 3 wt%) of multilayer graphene (MLG) as well as exfoliated graphite nanoplatelets (xGnP) and nano graphene platelets (Angstron) in comparison. The microstructure and mechanical properties of the graphene reinforced silicon nitride based composite materials have been investigated. Homogeneous distribution of the MLG additives have been observed on the fracture surface of the sintered material. The scanning electron microscopy examinations showed that graphene platelets are inducing porosity in matrix. The bending strength and elastic modulus of MLG/Si₃N₄ composites showed enhanced values compared to the other graphene added silicon nitride ceramic composites. These observations may be explained by the different type and quality of the starting materials and by the dispersion grade of graphene platelets having direct impact to the resulting density of the sintered samples.     

Ceramic/metal nanocomposites by lyophilization: Spark plasma sintering and hardness

The present study is focused on the procedure of spray-drying and lyophilization techniques for the preparation of ceramic/metal nanocomposites. The results of the study at all stages are compared with those corresponding to powders conventionally dried by heating in furnace. Starting from aqueous solutions of metal salts and ceramic powders, the procedure follows with spray-drying, lyophilization, calcination of the resulting powders and subsequent Spark Plasma Sintering (SPS). X-ray diffraction analysis of the powders at different stages of the processing routes was used for phase indexing; further characterization was performed by Transmission Electron Microscopy and Energy Dispersive X-Ray Spectroscopy, revealing that the sizes of the metal particles obtained are in the nanometer range and appear homogeneously and well dispersed on the zirconia surface. The mechanical performance of the SPSed compacts was studied by means of the Vickers hardness, showing excellent results: an increase of 30% with respect to pure zirconia.     

Effect of TiO2 addition on thermal and mechanical properties of Y-Si-Al-O-N glasses

Y-Si-Al-O-N glasses are intergranular phases in silicon nitride based ceramics in which the composition and volume fraction of oxynitride glass phases determine the sintering/shrinkage behaviour. Several investigations on oxynitride glass formation and properties have shown that addition of nitrogen increases glass transition and softening temperatures, viscosity, elastic modulus and hardness. In the present study, effect of TiO₂ addition on thermal and mechanical properties of Y-Si-Al-O-N glasses is investigated since the most typical Si₃N₄ ceramics for bearing applications are fabricated using a Si₃N₄-Y₂O₃-Al₂O₃-TiO₂-AlN system. Addition of TiO₂ is effective in preparing Y-Si-Al-O-N glasses with lower glass transition temperatures and with higher hardness.     

Glass–ceramics as oxidation resistant bond coat in thermal barrier coating system

Thermal barrier coating (TBC) system consisting of yttria stabilized zirconia (YSZ) top coat, glass–ceramic bond coat and nickel base superalloy substrate was subjected to static oxidation test at 1200 °C for 500 h in air. Oxidation resistance of this TBC system was compared with the conventional TBC system under identical heat treatment condition. Both the TBC systems were characterized by SEM as well as EDX analysis. No TGO layer was found between the bond coat and the top coat in the case of glass–ceramic bonded TBC system while the conventional TBC system exhibited a TGO layer of about 16 μm thickness at the bond coat-top coat interface region.     

Cavitation and rolling wear in silicon nitride

Rolling contact and cavitation testing were integrated in a testing methodology to study their combined effect on silicon nitride rolling elements. This testing methodology is well suited to perform controlled cavitation and rolling contact experiments. Acoustic cavitation method and a rotary tribometer were utilized to achieve this objective. Silicon nitride degradation initiated with the formation of blisters in rolling contact. This blisters underwent cracking in the subsequent testing, thereby allowing the lubricant to squeeze in due to rolling contact. Erosion pits formed and their density increased along with their growth by detaching grains and bridging into adjacent pits. As the erosion severity in the rolling contact increased the material eventually failed in a short period of time with respect to the testing conditions. The effect of cavitation and rolling contact parameters on material damage is detailed in this paper thereby allowing an evaluation of material systems for cavitation-rolling contact fatigue (RCF) conditions.     

In situ preparation of SiC/Si3N4-NW composite powders by combustion synthesis

Large-scale composite powders containing silicon carbide (SiC) particles and silicon nitride nanowires (Si₃N₄-NWs) were synthesized in situ by combustion synthesis (CS). In this process, a mixture of silicon, carbon black, polytetrafluoroethylene (PTFE) and a small amount of iron powders was used as the precursor. The products were characterized by XRD, SEM, EDS and TEM. The particles are equiaxed with diameters in the micron range, and the in situ formed nanowires are straight with uniform diameters of 20-350 nm and lengths of tens of microns. The Si₃N₄-NWs are characterized to be α-phase single crystals grown along the [1 0 1] or [1 0 0] direction. VLS and SLGS processes are proposed as the growth mechanisms of the nanowires. The as-synthesized powders have great potential for use in the preparation of high-performance SiC/Si₃N₄-NW composites.     

The effect of silica content on microstructure and mechanical properties of calcia-stabilized tetragonal zirconia polycrystalline ceramic

The present study was aimed at investigating the effect of silica impurities on structure and mechanical properties of zirconia ceramics, stabilized in tetragonal phase by addition of 6.5?mol% calcia. The effect of silica was studied in 0–5?mol% silica concentration range. It was shown that notable increase in fracture toughness (from 7.5?MPa?m^0.5 to 12.5?MPa?m^0.5) as well as limited rise in hardness (from 12?GPa to 13?GPa) can be achieved by addition of ~ 2.5?mol% of SiO2. It was shown that further increase in SiO₂ concentration above 3.75?mol% results in destabilization of tetragonal phase and degradation of mechanical properties. It is suggested that silica reacts with calcia resulting in formation of amorphous calcium silicate, decreasing calcia content in zirconia matrix, and facilitates sintering and grain growth, resulting in lower stability of tetragonal phase.