Mechanical Properties and Failure Analysis of Alumina-Glass Dental Composites

Strength measurements and fractography were used to investigate the failure of alumina-glass dental composites containing 75 vol% alumina and 25 vol% glass. Alumina compacts were prepared by slip casting and sintering at 1100°C for 2 h. Dense composites were made by infiltrating partially sintered alumina with glass at 1150°C for 8 h. Young's modulus and the hardness of the composites were 270 GPa and 12 GPa, respectively. The mean strength (460 MPa) and fracture toughness (4.0 MPa·m^1/2) of the composites were insensitive to the glass thermal expansion coefficient (α_glass= 5.9 × 10⁻⁶ to 7.8 × 10⁻⁶°C⁻¹). Typical flaws were pores and cracklike voids formed by poor particle packing and differential sintering near agglomerates of alumina in the composite. Crack deflection and crack bridging were observed in indentation cracks. Fracture toughness was single-valued because the alumina particle size was small (∼3 μm). Alumina-glass composites are promising new ceramics for dental crown and bridge applications, because their strength and fracture toughness are ∼2 times greater than those of current dental ceramics.     

Flexure Strength, Fracture Toughness, and Slow Crack Growth of YSZ/Alumina Composites at High Temperatures

Flexure strength and fracture toughness of zirconia–alumina composites, fabricated by hot pressing 10 mol% yttria-stabilized zirconia (10-YSZ) reinforced with 0–30 mol% alumina particulates or platelets, were determined as a function of alumina content at 1000°C in air. Both strength and fracture toughness of the two composite systems increased with increasing alumina content. For a given alumina content, flexure strength of the particulate composites was greater than that of the platelet composites at higher alumina contents (≥20 mol%); whereas, fracture toughness of the platelet composites was greater than that of the particulate counterparts, regardless of the alumina content. The susceptibility to slow crack growth (SCG), determined at 1000°C via constant stress-rate testing, was greatest for 30 mol% particulate composite with SCG parameter n =5–8 and was least for 30 mol% platelet composite with n =33. Elastic modulus of both composite systems decreased below 400°C and then remained almost unchanged up to 1000°C, forming a unique transition around 400°C, irrespective of alumina content.     

Cardanol as a dispersant plasticizer for an alumina/toluene tape casting slip

Cardanol, a naturally occurring C₁₅ alkyl chain substituted phenol obtained from cashew nut shell liquid (CNSL), is used as a dispersant and plasticizer for PMMA binder based alumina tape casting slips in toluene medium. The best dispersion of an alumina powder with BET surface area of 10.4 m²/g occurs at a cardanol concentration 2 wt.% of the powder at which the cardanol molecules form a monolayer on the particles with an end-on-adsorbed configuration through phenolic hydroxyl anchored on the surface. Cardanol added in excess of the dispersing agent acts as a plasticizer for PMMA, as revealed by significant decrease in the T_g of the polymer, reduction in the slurry viscosity and increase in the tape flexibility. Green tapes with good flexibility (failure strain, 10–20%) and strength (5.7–7 MPa) were obtained using a binder content 12 wt.% of alumina and employing a plasticizer to binder ratio in the range 0.66–0.82 by weight. The green tapes were thermally debinded with or without extraction of the plasticizer with methanol. The solvent extraction of the plasticizer prior to thermal debinding, however, did not show any effect on the density (97% TD) of the tapes sintered at 1500°C.     

Mechanical Properties and Fracture Toughness of α-Al2O3-Platelet-Reinforced Y-PSZ Composites at Room and High Temperatures

YPSZ/Al₂O₃-platelet composites were fabricated by conventional and tape-casting techniques followed by sintering and HIPing. The room-temperature fracture toughness increased, from 4.9 MPa·m^1/2 for YPSZ, to 7.9 MPa·m^1/2 (by the ISB method) for 25 mol% Al₂O₃ platelets with aspect ratio = 12. The room-temperature fiexural strength decreased 21% and 30% (from 935 MPa for YPSZ) for platelet contents of 25 vol% and 40 vol%, respectively. Al₂O₃ platelets improved the high-temperature strength (by 110% over YPSZ with 25 vol% platelets at 800°C and by 40% with 40 vol% platelets at 1300°C) and fracture toughness (by 90% at 800°C and 61% at 1300°C with 40 vol% platelets). An amorphous phase at the Al₂O₃-platelet/YPSZ interface limited mechanical property improvement at 1300°C. The influence of platelet alignment was examined by tape casting and laminating the composites. Platelet alignment improved the sintered density by >1% d _th , high-temperature strength by 11% at 800°C and 16% at 1300°C, and fracture toughness by 33% at 1300°C, over random platelet orientation.     

Shrinkage of Tape Cast Products During Binder Burnout

During sintering of tape cast products, anisotropic shrinkage occurs, which can be attributed to an anisotropic green tape structure concerning particle and pore orientation. Little is known about the shrinkage during binder burnout (BBO) and its relation to the microstructure of green tapes including the binder–plasticizer phase. Therefore, the article determines the shrinkage behavior of green tapes derived from alumina powders with different particle shape during binder burnout and prefiring in all spatial directions. The shrinkage after prefiring relative to the green and the debindered states is also discussed. The interrelation between shrinkage behavior and microstructure is investigated in dependence on different process parameters and specifically on the thermal behavior of the binder–plasticizer phase in the green tapes. It is shown that the subtraction of the BBO shrinkage from the total shrinkage results in completely different data for the sintering shrinkage anisotropy in z direction.     

Postsintering Hot Isostatic Pressing of Ceria-Doped Tetragonal Zirconia/Alumina Composites in an Argon–Oxygen Gas Atmosphere

Ceria-doped tetragonal zirconia (Ce-TZP)/alumina (Al₂O₃) composites were fabricated by sintering at 1450° to 1600°C in air, followed by hot isostatic pressing (postsintering hot isostatic pressing) at 1450°C and 100 MPa in an 80 vol% Ar–20 vol% O₂ gas atmosphere. Dispersion of Al₂O₃ particles into Ce-TZP was useful in increasing the relative density and suppressing the grain growth of Ce-TZP before hot isostatic pressing, but improvement of the fracture strength and fracture toughness was limited. Postsintering hot isostatic pressing was useful to densify Ce-TZP/Al₂O₃ composites without grain growth and to improve the fracture strength and thermal shock resistance.     

Mechanical Properties and Microstructure of Alumina-Glass Composites

Alumina blanks were prepared via isostatic pressing and sintering at 1400°C for 2 h, whereas alumina-glass composites were prepared by infiltrating the molten glass into the partially sintered alumina compacts. The samples had a high bending strength (340 MPa) and high fracture toughness (3.91 MPa·m^1/2) and were free of shrinkage. Concurrently, zirconia (5 wt%) was used as an additive to alumina to improve the mechanical properties of both partially sintered alumina and alumina-glass composites. Results show that zirconia notably improves the mechanical properties of the partially sintered alumina but increases that of the composites by no more than 10%.     

Tape Casting of Lanthanum Chromite

The effects of process additives, ball milling, and solids loading were evaluated for tape casting suspensions of glycinenitrate-synthesized La_0.7Ca_0.31CrO₃ powder. An optimized formulation was obtained based on rheological characterization, electrokinetic sonic amplitude measurements, qualitative examination of green tapes, and the sintered microstructure. The tape casting formulation incorporated 66:34 methyl ethyl ketone/ethyl alcohol solvent, an aliphatic phosphate ester dispersant, and 80 wt% (35 vol%) solids. The best binder/plasticizer system was 12 wt% (15 vol%) poly(isobutyl methacrylate) and 5 wt% (6.3 vol%) benzyl butyl phthalate plasticizer (binder:plasticizer = 2.3). Cast tapes were sintered at 1300°C for 2 h, producing a bulk density of 96.2% theoretical, with linear shrinkage of 22% and an approximate grain size of 1.3 μm.     

Melt-Infiltration Processing and Fracture Toughness of Alumina-Glass Dental Composites

Alumina-glass composites were prepared by a melt-infiltration process that is similar to a fabrication method for dental crowns and bridges. Cylindrical alumina samples with green densities ranging from 62% to 72% of theoretical were formed by slip casting followed by sintering at 1100°C for 2 h. A borosilicate glass was infiltrated at 1200°C, resulting in a composite microstructure consisting of fused alumina particles and glass-filled pores. Fracture toughness of the composites, measured by a chevron-notch method with a short rod sample, was ∼3.8 MPa·m^1/2 and was relatively insensitive to the volume fraction of alumina in the range of 0.62 to 0.72.     

Mechanical Properties of Gd‐CeO2 Electrolyte for SOFC Prepared by Aqueous Tape Casting

Mechanical properties of gadolinium‐doped ceria (Ce_0.9Gd_0.1O_1.95, 10GDC) green tape prepared by aqueous‐based tape casting process were characterized by tensile test and shear punch test (SPT). SPT was found to be a useful method for characterizing mechanical properties of green tapes. Microstructures and mechanical properties such as flexural modulus, bending strength, and microhardness of tapes sintered at 1,300–1,500 °C have been evaluated. Indentation fracture toughness was also determined by the method of Palmqvist cracks at different applied loads for tapes sintered at 1,500 °C. Grain size measurements showed that excessive grain growth occurred during sintering despite using 10GDC nanopowders as the starting material. However, mechanical properties of sintered tapes improved by increasing sintering temperature and the results are comparable with those reported for 10GDC in literature.     

Spark Plasma Sintering of Magnesia-Doped Alumina with High Hardness and Fracture Toughness

The effect of grain size of magnesia and its content as well as spark plasma sintering conditions on the density, grain size, strength, hardness, and toughness of alumina was investigated. Spark plasma sintering conditions were optimized at 1150°C/5 min/175°C/min. Addition of 100 nm magnesia gave higher density levels (99.5%), while better strength (600 MPa), hardness (25 GPa), and fracture toughness (4.5 MPa·m^1/2) were obtained with 15 nm magnesia. The good strength and hardness is attributed to the submicrometer grain size of the matrix, and the improved toughness to the presence of Mg-rich nanoparticles and nanopores at grain boundaries.     

Pulse Electric Current Sintering of Al2O3/3 vol% ZrO2 with Constrained Grains and High Strength

The pulse electric current sintering technique (PECS) was demonstrated to be effective in rapid densification of fine-grained Al₂O₃/3Y-ZrO₂ using available commercial powders. The composites attained full densification (>99% of TD) at 1450°C in less than 5 min. The composites sintered at a high heating rate had a fine microstructure. The incorporation of 3 vol% 3Y-ZrO₂ substantially increased the average fracture strength and the toughness of alumina to as high as 827 MPa and 6.1 MPa·m^1/2, respectively. A variation in the heating rate during the PECS process influenced grain size, microstructure, and strength, though there was little or no variation in the fracture toughness.     

Reinforcement of Hydroxyapatite Bioceramic by Addition of Ti3SiC2

Ti₃SiC₂/HAp composites with different Ti₃SiC₂ volume fractions were fabricated by spark plasma sintering (SPS) at 1200°C. The effects of Ti₃SiC₂ addition on the mechanical properties and microstructures of the composites were investigated. The bending strength and fracture toughness of the composites increased with increasing of Ti₃SiC₂ content, whereas the Vickers hardness decreased. The bending strength and fracture toughness reached 252±10 MPa and 3.9±0.1 MPa·m^1/2, respectively, with the addition of 50 vol% Ti₃SiC₂. The increases in the mechanical properties were attributed to the matrix strengthening and interactions between cracks and the Ti₃SiC₂ platelets.     

Influence of chemical composition on sintering ability of ZTA ceramics consolidated from freeze dried granules

Dense zirconia-toughened alumina (ZTA) ceramic composites with ZrO₂ = 0, 5, 10, 15, 20, 30, 60 and 100 wt.% have been prepared by sintering green compacts obtained by dry powder pressing of freeze dried granules consisting of α-alumina and a yttria partially stabilized zirconia (YPSZ) at various temperatures ranging from 1450 to 1650 °C for 1-2 h. The characteristics of sintered products were determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), Archimedes principle, Vickers indentation method and by 3-point bend test. Characterization results revealed that adding YPSZ increased the 3-point bend (flexural) strength, fracture toughness and homogeneity of the microstructure, but slightly decreased the hardness and the sintering ability of alumina. A 20 wt.% YPSZ was sufficient to increase the fracture toughness and flexural strength of specimens sintered for 2 h at 1600 °C from 2.5 to 4.6 MPa m^1/2 and 150 to 400 MPa, respectively. The XRD results revealed that there is no solid-solution formation between zirconia and alumina constituents of ZTA ceramic composites upon sintering.     

Mechanical and tribological properties of TiB2-SiC and TiB2-SiC-GNPs ceramic composites

TiB₂-SiC and TiB₂-SiC-graphene nanoplatelets (GNPs) composites were prepared using field-assisted sintering technology at 2100 °C in argon atmosphere, and the influence of the SiC and different GNPs addition on microstructure development, mechanical and tribological properties has been investigated. Instrumented hardness, bending strength, chevron-notched fracture toughness and ball-on-flat tribological tests were used for the testing and characterization of the composites. The addition of SiC significantly improved the bending strength and elastic modulus with values of 601 MPa and 474 GPa, respectively, but decreased the fracture toughness with a value of 4.8 MPa.m^1/2. The addition of GNPs has a positive effect on fracture toughness and flexural strength but a negative one on the hardness. The increasing amount of both GNPs has a positive influence on wear characteristics of the composites thanks to the described wear mechanisms.     

Aqueous tape casting of silicon nitride

Slurries consisting of a low cost silicon nitride powder, sintering aids yttria and alumina, dispersants, binders, defoamers and water as a solvent were optimised for tape casting by electroacoustic and viscosity measurements and by casting experiments. The slurries exhibit shear-thinning behaviour due to the highly shear-thinning binder emulsion. Crack free tapes with a maximum thickness of approx. 250 μm and a binder content of 13–15 wt.% could be obtained. The green tapes with a high flexibility and green strength could be laminated easily by compression at room temperature. After sintering a dense microstructure developed. A significant shrinkage anisotropy parallel and perpendicular to the cast direction was observed.     

Effect of the volume ratio of zirconia and alumina on the mechanical properties of fibrous zirconia/alumina bi-phase composites prepared by co-extrusion

Fibrous zirconia/alumina composites with different composition were fabricated by piston co-extrusion. After a 3rd extrusion step and sintering at 1600 °C, crack-free composites with a fibre width of 50 μm were obtained for all compositions. The effect of the volume ratio of secondary phase on the mechanical properties was investigated. The Young's modulus of the composites decreased linearly with increasing the zirconia content. The fracture toughness of the composites was improved by introducing fine second phase filaments into the matrix. The maximum fracture toughness of 6.2 MPa m^1/2 was attained in the 3rd co-extruded 47/53 vol% zirconia/alumina composite. The improvement in toughness was attributed to both “stress-induced” transformation of zirconia and a crack deflection mechanism due to thermal expansion mismatch between the two phases. Bending strength of the composites was almost the same as that of the monolithic alumina regardless of the composition.     

Organic Distributions in Dried Alumina Green Tape

Distributions of organic binder (poly(vinyl butyral) (PVB)) and plasticizer (dibutyl phthalate (DBP)) in alumina green tape dried at different temperatures are studied. More PVB and DBP are observed on the bottom (Mylar side) than on the top surface (air side) of the green tape. Inside the green tape, however, PVB distribution, which remains relatively unchanged with drying temperature in the range of 30°–80°C, increases with distance from the bottom to the top. In contrast, the DBP concentration remains relatively unchanged with the depth of green tape when the drying temperature is <50°C. At 80°C, however, a significant drop in DBP concentration near the top surface of green tape is found. Mathematical analysis using the finite difference method is completed to describe the PVB distribution in alumina green tape, and the results show reasonable agreement with experimental observations.     

Fabrication and Properties of Tape-Cast Laminated and Functionally Gradient Alumina–Titanium Carbide Materials

A tape-casting process was used to prepare various Al₂O₃–TiC green tapes, from which laminated and functionally gradient Al₂O₃–TiC materials (FGM Al₂O₃–TiC) were produced by cutting, stacking, and laminating the material, removing the binder, and hot-pressing the green bodies. The bending strength of the FGM Al₂O₃–TiC composites was not much less than that of the laminated Al₂O₃–TiC composites. However, the fracture toughness was >50% higher; the fracture toughness of the FGM composite sintered at 1700°C was 9.43 MPa·m^1/2. This increased toughness was attributed to the stress distribution that was caused by variations in the composition of the FGM composite layers. The present results demonstrate that the FGM design is a useful method for modifying the mechanical properties of ceramic composites.     

Preparation of Titanium Nitride/Alumina Laminate Composites

A preparation route for TiN/Al₂O₃ laminate composites has been described. A water-based process using Al₂O₃ and TiN slurries with solids contents of 40 and 35 vol%, respectively, was used to make TiN and Al₂O₃ tapes. The removal of the binder was monitored by weight-loss measurements in a thermogravimetry unit. Bodies composed of Al₂O₃ and TiN tapes were densified at temperatures of 1400° and 1500°C using the Spark Plasma Sintering^® (SPS) technique. Densities of >98% of the theoretical densities were approached. Crack-free and almost fully densified TiN/Al₂O₃ compacts were prepared by heating the burned-out green bodies to the final sintering temperature (1500°C) at a rate of 100°C/min, and with a holding time of 5–10 min, under a pressure of 75 MPa. The microstructures of the obtained compacts were studied using scanning electron microscopy. Grain sizes in the sintered Al₂O₃ and TiN compacts were similar to those of the precursor powders. Hardness and indentation fracture toughness were measured at room temperature, and the monolithic compacts as well as the laminate composites exhibited anisotropic mechanical behavior; i.e., the cracks propagated much more easily in a direction parallel to the laminas than perpendicular to them.