Zirconia/Alumina Functionally Gradiented Composites by Electrophoretic Deposition Techniques

An electrophoretic deposition and sintering route was used to prepare YSZ/Al₂O₃ composites with a compositional gradient. The YSZ content was continuously decreased from the YSZ-rich surface to the Al₂O₃-rich surface, Microstructural and Vickers hardness (16–24 GPa) evidence tracked the compositional development, and the indentation fracture toughness was found to vary across the section (10–3 MPa·m^1/2).     

Microstructure and Properties of Spark Plasma-Sintered ZrO2–ZrB2 Nanoceramic Composites

In a recent work, ¹ we have reported the optimization of the spark plasma sintering (SPS) parameters to obtain dense nanostructured 3Y-TZP ceramics. Following this, the present work attempts to answer some specific issues: (a) whether ZrO₂-based composites with ZrB₂ reinforcements can be densified under the optimal SPS conditions for TZP matrix densification (b) whether improved hardness can be obtained in the composites, when 30 vol% ZrB₂ is incorporated and (c) whether the toughness can be tailored by varying the ZrO₂–matrix stabilization as well as retaining finer ZrO₂ grains. In the present contribution, the SPS experiments are carried out at 1200°C for 5 min under vacuum at a heating rate of 600 K/min. The SPS processing route enables retaining of the finer t -ZrO₂ grains (100–300 nm) and the ZrO₂–ZrB₂ composite developed exhibits optimum hardness up to 14 GPa. Careful analysis of the indentation data provides a range of toughness values in the composites (up to 11 MPa·m^1/2), based on Y₂O₃ stabilization in the ZrO₂ matrix. The influence of varying yttria content, t -ZrO₂ transformability, and microstructure on the properties obtained is discussed. In addition to active contribution from the transformation-toughening mechanism, crack deflection by hard second phase brings about appreciable increment in the toughness of the nanocomposites.     

Synthesis, Physical, and Mechanical Properties of Bulk Zr3Al3C5 Ceramic

An in situ reactive hot-pressing process using zirconium (zirconium hydride), aluminum, and graphite as staring materials and Si and Y₂O₃ as additives was used to synthesize bulk Zr₃Al₃C₅ ceramics. This method demonstrates the advantages of easy synthesis, lower sintering temperature, high purity and density, and improved mechanical properties of synthesized Zr₃Al₃C₅. Its electrical and thermal properties were measured. Compared with ZrC, Zr₃Al₃C₅ has a relatively low hardness (Vickers hardness of 12.5 GPa), comparable stiffness (Young's modulus of 374 GPa), but superior strength (flexural strength of 488 GPa) and toughness (fracture toughness of 4.68 MPa·m^1/2). In addition, the stiffness decreases slowly with increasing temperature and at 1600°C remains 78% of that at ambient temperature, indicating that Zr₃Al₃C₅ is a potential high-temperature structural ceramic.     

Preparation, Hardness, and Fracture Toughness of Tantalum Oxynitride Ceramics

Tantalum oxynitride powder with a baddeleyite crystal structure was synthesized and densified by hot pressing in Ar and under high pressure using a belt-type high-pressure apparatus. The tantalum oxynitride powder could not be densified completely under hot-pressing conditions at 1400°C. The use of high pressure resulted in dense materials. The samples showed a hardness of 16–17 GPa and a fracture toughness of 3–4 MPa·m^1/2. The hardness is higher compared with that of ZrO₂ and HfO₂ ceramics. The fracture toughness corresponds to the value of fully stabilized ZrO₂ due to the absence of any transformation toughening mechanism.     

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.     

Microstructure and Mechanical Properties of Hot-Pressed α-Al2O3-Seeded γ-Alumina Ceramics

High-quality alumina ceramics were fabricated by a hot pressing with MgO and SiO₂ as additives using α-Al₂O₃-seeded nanocrystalline γ-Al₂O₃ powders as the raw material. Densification behavior, microstructure evolution, and mechanical properties of alumina were investigated from 1250°C to 1450°C. The seeded γ-Al₂O₃ sintered to 98% relative density at 1300°C. Obvious grain growth was observed at 1400°C and plate-like grains formed at 1450°C. For the 1350°C hot-pressed alumina ceramics, the grain boundary regions were generally clean. Spinel and mullite formed in the triple-grain junction regions. The bending strength and fracture toughness were 565 MPa and 4.5 MPa·m^1/2, respectively. For the 1300°C sintered alumina ceramics, the corresponding values were 492 MPa and 4.9 MPa·m^1/2.     

Field-Assisted Densification of Superhard B6O Materials with Y2O3/Al2O3 Addition

B₆O is a possible candidate of superhard materials with a hardness of 45 GPa measured on single crystals. Up to now, densification of these materials was only possible at high pressure. However, recently it was found that Al₂O₃ can be utilized as an effective sintering additive, similar to the addition of Y₂O₃/Al₂O₃ that was used in this work. The densification behavior of the material as a function of applied pressure, its microstructure evolution, and the resulting mechanical properties were investigated. A strong dependence of the densification with increasing pressure was found. The material revealed characteristic triple junctions filled with amorphous residue composed of B₂O₃, Al₂O₃, and Y₂O₃, while no amorphous grain-boundary films were observed along internal interfaces. Mechanical testing revealed on average a hardness of 33 GPa, a fracture toughness of 4 MPa·m^1/2, and a strength value of 520 MPa.     

Spark Plasma Sintering of Alumina

A systematic study of various spark plasma sintering (SPS) parameters, namely temperature, holding time, heating rate, pressure, and pulse sequence, was conducted to investigate their effect on the densification, grain-growth kinetics, hardness, and fracture toughness of a commercially available submicrometer-sized Al₂O₃ powder. The obtained experimental data clearly show that the SPS process enhances both densification and grain growth. Thus, Al₂O₃ could be fully densified at a much lower temperature (1150°C), within a much shorter time (minutes), than in more conventional sintering processes. It is suggested that the densification is enhanced in the initial part of the sintering cycle by a local spark-discharge process in the vicinity of contacting particles, and that both grain-boundary diffusion and grain-boundary migration are enhanced by the electrical field originating from the pulsed direct current used for heating the sample. Both the diffusion and the migration that promote the grain growth were found to be strongly dependent on temperature, implying that it is possible to retain the original fine-grained structure in fully densified bodies by avoiding a too high sintering temperature. Hardness values in the range 21–22 GPa and fracture toughness values of 3.5 ± 0.5 MPa·m^1/2 were found for the compacts containing submicrometer-sized Al₂O₃ grains.     

Subcritical Crack Growth in Y-TZP and Al2O3-Toughened Y-TZP

Crack velocity curves for Y-TZP and Al₂O₃-toughened Y-TZP were determined for long cracks in compact tension specimens with an in situ fracture device on the stage of an optical microscope. Indications for a crack velocity threshold were found for both materials. Above this threshold, at 2.6 MPa·m^1/2 for Y-TZP and 3.6 MPa·m^1/2 for Al₂O₃-toughened Y-TZP, chemically assisted subcritical crack growth occurs over an extended regime of applied stress intensity factors of width 2.1–2.8 MPa·m^1/2. It is recognized that the dependence of the shielding term on the crack-tip stress field renders transformation-toughened materials particularly susceptible to stress-corrosion cracking. This interrelation leads to the definition of a steady-state velocity at constant applied stress intensity factor. This velocity is obtained in the situation where the shielding term is fully defined by the present crack-tip stress field, not depending on prior loading history.     

Influence of Planetary High-Energy Ball Milling on Microstructure and Mechanical Properties of Silicon Nitride Ceramics

The influence of ball-milling methods on microstructure and mechanical properties of silicon nitride (Si₃N₄) ceramics produced by pressureless sintering for a sintering additive from MgO–Al₂O₃–SiO₂ system was investigated. For planetary high-energy ball milling, the mechanical properties of Si₃N₄ ceramics were evidently improved and a homogeneous microstructure developed. In contrast, some exaggerated elongated grains were developed due to the local enrichment of sintering additives in the specimen prepared by general ball milling. For Si₃N₄ ceramics produced by planetary ball milling, flexure strength of 1.06 GPa, Vickers hardness of 14.2 GPa, and fracture toughness of 6.6 MPa·m^0.5 were achieved. The differences in the mechanical properties of Si₃N₄ ceramics produced by different processing seem to arise mainly from the changes in microstructural homogenization and sinterability. The planetary high-energy ball-milling process provides a good route to mix starting powders for developing ceramics with uniform microstructure and promising mechanical properties.     

Fabrication, Mechanical Properties, and Electrical Conductivity of Co3O4 Ceramics

Well-densified Co₃O₄ ceramics (98.3% of theoretical) have been fabricated by the combined use of hot pressing (800°C/I h/30 MPa) and hot isostatic pressing (880°C/2 h/196 MPa). Their Vickers hardness and fracture toughness are 10.3 GPa and 4.2 MPa·m^1/2, respectively. They exhibit a high electrical conductivity of 3.35 × 10' S·cm⁻¹ at 800°C.     

Fabrication of Hard and Strong α/β-Si3N4 Composites With MgSiN2 as Addivitives

α/β-Si₃N₄ composites with various α/β phase ratios were prepared by hot pressing at 1600°–1650°C with MgSiN₂ as sintering additives. An excellent combination of mechanical properties (Vickers indentation hardness of 23.1 GPa, fracture strength of about 1000MPa, and toughness of 6.3 MPa·m^1/2) could be obtained. Compared with conventional Si₃N₄-based ceramics, this new material has obvious advantages. It is as hard as typical in-situ-reinforced α-Sialon, but much stronger than the latter (700 MPa). It has comparable fracture strength and toughness, but is much harder than β-Si₃N₄ ceramics (16 GPa). The microstructures and mechanical properties can be tailored by choosing the additive and controlling the heating schedule.     

Fabrication of Elongated α-SiAlON via a Reaction-Bonding Process

A reaction-bonding process, which offers low sintering shrinkage and is a low-cost process, was applied to fabricate Y–α-SiAlON ceramics. The green compacts composed of Si, Y₂O₃, Al₂O₃, and AlN were nitrided and subsequently postsintered. Dense single-phase Y–α-SiAlON with elongated grain morphology could be achieved in the specimen postsintered at 1900°C. The material exhibited high hardness (1850 HV10) and high fracture toughness (5.1 MPa·m^1/2).     

Mechanical Properties of Alumina–Zirconia–Silver Composites

Either ceramic inclusions or metallic inclusions can be used to enhance the mechanical properties of ceramics. In the present study, both silver inclusions and zirconia agglomerates have been added to alumina. The presence of the inclusions inhibits the grain growth of the alumina matrix. The strength of AI₂O₃-ZrO₂-Ag composites is increased by microstructural refinement. Together with the plastic deformation of silver inclusions and the phase transformation of tetragonal zirconia agglomerates, the toughness of the composites is enhanced. Because silver inclusions and zirconia agglomerates are attached after sintering, the toughness increase for the Al₂O₃-ZrO₂-Ag composites is less than the sum of the toughness increments for Al₂O₃-Ag and Al₂O₃-ZrO₂ composites.     

Pressureless Sintering of Si3N4 Ceramic Using AlN and Rare-Earth Oxides

Using intermediate, liquid-forming compositions in the (Y,La)₂O₃-AlN system as additives, fully dense Si₃N₄ ceramics with high strength at high temperature have been obtained by pressureless sintering. The ceramics contain rod-shaped β-Si₃N₄ with M' or K' solid solutions as grain-boundary phases. The strength of these ceramics is 1150 MPa at 1200°C, and the room-temperature toughness is maintained at }7 MPa·m^1/2. Phase relations that are pertinent to the new additive compositions are delineated to rationalize their beneficial effects on sinterability and mechanical properties.     

Fabrication of an Al2O3/YAG/ZrO2 Ternary Eutectic by Combustion Synthesis Melt Casting Under Ultra-High Gravity

This work presents a novel method for preparing an Al₂O₃/YAG/ZrO₂ ternary eutectic whereby combustion synthesis melt casting has been combined with the ultra-high gravity (UHG) technique. The fabricated product had a relative density of 99.3% of the theoretical one. Phase composition and microstructure analyses indicated that the application of UHG resulted in a metal-free ceramic microstructure with no porosity or microcracks. The microstructure comprises ZrO₂ rods dispersed in Al₂O₃. The product had 17.82 GPa Vickers hardness and 5.51 MPa·m^1/2 fracture toughness.     

Sol–Gel Processed Y-PSZ Ceramics with 5 wt% Al2O3

Y-PSZ ceramics with 5 wt% Al₂O₃ were synthesized by a sol–gel route. Experimental results show that powders of metastable tetragonal zirconia with 2.7 mol% Y₂O₃ and 5 wt% Al₂O₃ can be fabricated by decomposing the dry gel powder at 500°C. Materials sintered in an air atmosphere at 1500°C for 3 have high density (5.685 g/cm³), high content of metastable tetragonal zirconia (>96%), and high fracture toughness (8.67 MPa.m^1/2). Compared with the Y-PSZ ceramics, significant toughening was achieved by adding 5 wt% Al₂O₃.     

High-Density Pressureless-Sintered HfC-Based Composites

Hafnium carbide (HfC)-(5, 10, and 20 vol%) MoSi₂ ceramics were pressureless sintered at 1950°C in an argon flux. The materials had nearly full density (96%–98%), with mean grain sizes in the range of 3–4 μm. Depending on the MoSi₂ amount (5–20 vol%), the mechanical properties were in the following ranges: hardness 16–15 GPa, Young's modulus 434–385 GPa, fracture toughness 3.6–3.4 MPa·m^1/2, and room-temperature 4-point flexural strength 465–383 MPa.     

Development and Characterization of Y2O3-Stabilized ZrO2 (Y-TZP) Composites with TiB2, TiN, TiC, and TiC0.5N0.5

Up to 50 vol% of TiB₂, TiC_0.5N_0.5, TiN, or TiC was added to Y₂O₃-stabilized tetragonal ZrO₂ polycrystals (Y-TZP) and hot pressed under vacuum. The influence of the type of secondary phase on the microstructure and mechanical properties was studied, as a function of the hot-pressing temperature. The influence of the secondary-phase content on the mechanical properties was studied by varying the TiB₂ content up to 50 vol%. Fully dense Y-TZP-based composites with very high toughness (up to 10 MPa·m^1/2), excellent bending strength (up to 1237 MPa), and increased hardness, with respect to ZrO₂ (Vickers hardness up to 1450 kg/mm²), were obtained.     

Processing and Properties of TiB2 with MoSi2 Sinter-additive: A First Report

The densification of non-oxide ceramics like titanium boride (TiB₂) has always been a major challenge. The use of metallic binders to obtain a high density in liquid phase-sintered borides is investigated and reported. However, a non-metallic sintering additive needs to be used to obtain dense borides for high-temperature applications. This contribution, for the first time, reports the sintering, microstructure, and properties of TiB₂ materials densified using a MoSi₂ sinter-additive. The densification experiments were carried out using a hot-pressing and pressureless sintering route. The binderless densification of monolithic TiB₂ to 98% theoretical density with 2–5 μm grain size was achieved by hot pressing at 1800°C for 1 h in vacuum. The addition of 10–20 wt% MoSi₂ enables us to achieve 97%–99%ρ_th in the composites at 1700°C under similar hot-pressing conditions. The densification mechanism is dominated by liquid-phase sintering in the presence of TiSi₂. In the pressureless sintering route, a maximum of 90%ρ_th is achieved after sintering at 1900°C for 2 h in an (Ar+H₂) atmosphere. The hot-pressed TiB₂–10 wt% MoSi₂ composites exhibit high Vickers hardness (∼26–27 GPa) and modest indentation toughness (∼4–5 MPa·m^1/2).