Toughening mechanisms of ZTA ceramics at cryogenic temperature (77 K)

ZTA ceramics containing 20 wt% ZrO₂ were fabricated at different sintering temperatures (1450, 1500 and 1550 °C) by SPS and HP processes, respectively. The influence of sintering process on the mechanical properties of ZTA ceramics at 298 K and 77 K was investigated. It can be seen that the bending strength and fracture toughness of samples prepared by the two processes both improved at cryogenic temperature. The stress-induced martensitic transformation toughening mechanism was confirmed by the in-situ Raman technique. The tetragonal ZrO₂ would be even more easy to transform because of the residual stress generated when temperature decreased from 298 K to 77 K. Therefore, the transformation toughening effect would become stronger, result in the increase of mechanical properties.     

High temperature mechanical properties of Al2O3/TiC micro–nano-composite ceramic tool materials

A type of Al₂O₃-based composite ceramic tool material simultaneously reinforced with micro-scale and nano-scale TiC particles was fabricated by the hot-pressing technology with different contents of cobalt additive. The effects of cobalt on the ambient temperature mechanical properties and high temperature flexural strength were investigated. The flexural strength and fracture toughness of the composite with 3 vol% cobalt as a function of temperature were investigated. Cobalt greatly enhanced the ambient temperature flexural strength and fracture toughness, while further increasing the content of cobalt led to a dramatic strength degradation, especially at high temperature. The flexural strength of the composite containing 3 vol% cobalt decreased as the temperature increased from 20 to 1200 °C, and the fracture toughness decreased as a function of the temperature up to 1000 °C but increased at 1200 °C. The degradation of high temperature flexural strength was ascribed to the change of the fracture mode, the grain and grain boundary oxidation, the decrease of elastic modulus and the grain boundary sliding.     

Microwave sintering of CeO2 and Y2O3 co-stabilised ZrO2 from stabiliser-coated nanopowders

Tetragonal ZrO₂ polycrystalline (TZP) composites with 2 wt.% Al₂O₃ and co-stabilised with 1 mol% Y₂O₃ and (4, 6 or 8) mol% CeO₂ were sintered at 1450 °C for 20 min in a single mode 2.45 GHz microwave furnace. For comparison, conventional sintering was performed in air at 1450 °C for 20 min. The starting powder mixture was obtained by a suspension coating technique using yttrium nitrate, cerium nitrate and pure m-ZrO₂ nanopowder. Fully dense material grades were obtained by both sintering methods. The influence of the composition and the sintering methods on the final phase composition and microstructure were investigated by X-ray diffraction and scanning electron microscopy. Finer and more uniform microstructures were observed in the microwave sintered ceramics when compared to the conventionally sintered samples. The fracture toughness increases with decreasing stabiliser content, whereas a reverse relation was found for the Vickers hardness. Comparable toughness and hardness values were obtained for the microwave and conventionally sintered samples.     

Improving the surface hardness of zirconia toughened alumina (ZTA) composites by surface treatment with a boehmite sol

This paper reports a novel way of enhancing the hardness of a zirconia-toughened alumina (ZTA) composite with a zirconia content of 20 vol% by surface treatments with a boehmite sol. More specifically, a ZTA composite was first prepared by heat-treating a mixture of alumina and zirconia powders containing Cr₂O₃ and SrAl₁₁CrO₁₉, as a reinforcement at 1400 °C for 1 h, and then infiltrating them with the boehmite sol, followed by heat-treatment at 1650 °C for 1 h to densify them. This treatment led to a significant increase in the surface hardness of the ZTA composite, which was attributed mainly to an increase in the volume fraction of an alumina phase with greater hardness, whereas the flexural strength and fracture toughness decreased slightly. The Vickers hardness, flexural strength and fracture toughness were 17.1 ± 2.5 GPa, 738 ± 88 MPa and 4.2 ± 0.11 MPa m^1/2, respectively.     

Spark plasma sintering of TiC ceramic with tungsten carbide as a sintering additive

By adding a small amount of tungsten carbide (WC) as sintering aids, nearly fully dense TiC ceramics were obtained by spark plasma sintering at 1450–1600 °C. The results show that the densification temperature of TiC ceramic was significantly decreased with the addition of 3.5 wt% WC. Compared with the monolithic TiC, the densification temperature of TiC–3.5 wt% WC is lower by ～150 °C and no deterioration of mechanical properties is observed. The TiC composite sintered at 1600 °C exhibits full density, a Vickers hardness of 28.2 ± 1.2 MPa, a flexural strength of 599.5 ± 34.7 MPa and a fracture toughness of 6.3 ± 1.4 MPa m^1/2.     

Microporous alumina substrate with porosity >70% by gelcasting

Microporous alumina membrane substrate in tubular and planar configurations have been prepared by gelcasting of alumina powder slurry using high amount of urea–formaldehyde as gelling agent followed by humidity controlled drying, binder removal and sintering of the gelled bodies. Porosity of the substrate samples sintered at 1350 °C was more than 70% as measured by mercury porosimeter. More than 51% porosity could be retained even after sintering of the samples at 1450 °C. Average pores size of the membrane substrate samples sintered at temperature in the range from 1250 to 1550 °C varied between 0.42 and 0.56 with a maximum at 1350 °C. More uniform pores were observed in sample sintered at 1450 °C. Urea-formaldehyde polymer present in the gelcast body acts as template for micropores.     

Pressureless sintering of titanium carbide doped with boron or boron carbide

Titanium carbide ceramics with different contents of boron or B₄C were pressureless sintered at temperatures from 2100 °C to 2300 °C. Due to the removal of oxide impurities, the onset temperature for TiC grain growth was lowered to 2100 °C and near fully dense (>98%) TiC ceramics were obtained at 2200 °C. TiB₂ platelets and graphite flakes were formed during sintering process. They retard TiC grains from fast growth and reduced the entrapped pores in TiC grains. Therefore, TiC doped with boron or B₄C could achieve higher relative density (>99.5%) than pure TiC (96.67%) at 2300 °C. Mechanical properties including Vickers’ hardness, fracture toughness and flexural strength were investigated. Highest fracture toughness (4.79 ± 0.50 MPa m^1/2) and flexural strength (552.6 ± 23.1 MPa) have been obtained when TiC mixed with B₄C by the mass ratio of 100:5.11. The main toughening mechanisms include crack deflection and pull-out of TiB₂ platelets.     

Mechanical behaviour of a low-clay translucent whiteware

A novel low-clay translucent whiteware body, using mostly non-plastic prefired materials and only a small amount of clay, was fabricated by slip casting and the effect of slip's solid content and sintering temperature on the mechanical behaviour was investigated. The degree of densification in the sintered specimens was determined by measuring the bulk density. The mechanical behaviour was determined by measuring the flexural strength and fracture toughness. Young's modulus and hardness were also measured. X-ray diffraction (XRD) and scanning electron microscopy (SEM) studies were carried out to analyse the microstructure.The flexural strength and fracture toughness increase with both increasing the slip's solid content and the sintering temperature up to a certain level, but further increase in solid content and sintering temperature had an adverse effect on the properties. The maximum flexural strength (∼135 MPa) and fracture toughness (∼1.85 MPa m^1/2) values were attained with specimens produced from a slip having 45 vol.% solid content at a sintering temperature of 1350 °C. It was found that the amount and distribution of closed pores, their size and possible link with each other control the flexural strength and fracture toughness of the low-clay translucent whiteware.     

Environment-dependent indentation recovery of select soda-lime silicate glasses

Indentations made on silicate glasses can easily be affected by the environment. In the present work, indentations were made on select commercial float glasses as well as on experimental soda-lime silicate glasses using a 1 mm diameter spherical tungsten carbide ball-mounted Brinell indenter. Recovery of indentations made on the glass samples was measured in different environments, namely, 100 °C, room temperature/room humidity and 100% relative humidity, as a function of time by using a Zygo laser non-contact profiliometer. Elastic (Young's modulus, bulk modulus, shear modulus and Poisson's ratio) and indentation (Vickers hardness, fracture toughness, brittleness and fracture surface energy) properties of the glasses were also determined by a pulse-echo and Vickers indentation methods, respectively, to correlate with the recovery of indentations. The elastic properties and Vickers hardness are directly proportional to the packing ions present in the glass structure and the strength of an individual bond, whereas the brittleness and fracture toughness more likely depend on molar volume of the glasses. According to the applied environment, a recovery rate of indentations follows the order: room temperature/room humidity <100% relative humidity <100 °C, regardless of glass composition. The reason for higher recovery rate of indentations is attributed to the structural relaxation, which is promoted by a thermodynamic driving force at 100 °C, and stored strain energy in deformation zone, allowing the indentations to regain their original configurations at certain points.     

Glass infiltration of gelcast zirconia-toughened alumina ceramics for dental restoration

This study investigated the effects of process parameters and material characteristics in glass infiltration of gelcast zirconia-toughened alumina (ZTA) ceramics for dental applications. Nine types of lanthanum-based silicate glasses with different concentrations of La₂O₃, B₂O₃, and Li₂O were prepared and characterized on the basis of their melting temperature, crystal structure, and thermal characteristics. These glasses were infiltrated into a ZTA matrix that was semi-sintered at 1200 °C to obtain a ceramic material with low shrinkage and high strength. The performance of the glass-infiltrated ceramic samples obtained with various glasses for various infiltration durations and temperatures was evaluated on the basis of the linear shrinkage rate, three-point bending strength, fracture morphology, and elemental composition. From the results, the infiltration temperature was identified as 1150 °C, and the optimum glass composition was 30%La₂O₃–15%Al₂O₃–15%B₂O₃–15%SiO₂–5%Li₂O by mass. The glass-infiltrated gelcast ZTA ceramic has a strength of 291.24 ± 27.94 MPa with a shrinkage of 1.8548 ± 0.2663%. These findings could provide a basis for further development of gelcast dental ceramics, which will make all-ceramic oral restoration less reliant on special equipment and materials.     

Hard and tough carbon nanotube-reinforced zirconia-toughened alumina composites prepared by spark plasma sintering

It is demonstrated that 0.1 wt% of multi-walled carbon nanotubes (MWCNTs) or single-walled carbon nanotubes (SWCNTs) added to zirconia toughened alumina (ZTA) composites is enough to obtain high hardness and fracture toughness at indentation loads of 1, 5, and 10 kg. ZTA composites with 0.01 and 0.1 wt% of MWCNTs or SWCNTs were densified by spark plasma sintering (SPS) at 1520 °C resulting in a higher hardness and comparable fracture toughness to the ZTA matrix material. The observed toughening mechanisms include crack deflection, pullout of CNTs as well as bridged cracks leading to improved fracture toughness without evidence of transformation toughening of the ZrO₂ phase. Scanning electron microscopy showed that MWCNTs rupture by a sword-in-sheath mechanism in the tensile direction contributing to an additional increase in fracture toughness.     

Preparation of ZTA ceramic by aqueous gelcasting with a low-toxic monomer DMAA

The present work reports the development of aqueous gelcasting of ZTA ceramic with a low-toxicity monomer DMAA. The rheological properties and the gelation behaviors of the slurries for gelcasting were investigated. It was proved that the time available for casting the slurry (idle time) can be controlled by the amounts of initiator. The ZTA green bodies exhibited a mechanical strength as high as 21 MPa. After sintered at 1600 °C for 2 h, the highest bending strength and fracture toughness of the sintered ZTA samples were as high as 643.3 ± 75 MPa and 6.3 ± 0.3 MPa m^1/2, respectively. SEM photographs revealed that the green bodies and sintered part had a uniform microstructure. The volume fraction of tetragonal phase zirconia was as high as 90%. Dense ZTA green bodies and ceramic parts with complex shaped were produced through the new gelcasting system.     

Sodalite zeolite as an alternative all-ceramic infiltrating material for alumina and zirconia toughened alumina frameworks

The purpose of this study was to determine the effects of synthesized sodalite zeolite infiltration achieved by a direct in-situ hydrothermal reaction followed by sintering process on the flexural strength and hardness of alumina and zirconia-toughened alumina (ZTA) frameworks. Ceramic core materials were prepared as disk-shaped specimens with 16 mm diameter and 1.2±0.2 mm thickness. The case-study group was synthesized sodalite zeolite-infiltrated alumina (IA-SOD) and synthesized sodalite zeolite-infiltrated ZTA (IZ-SOD); and the control group was glass-infiltrated alumina (IA-glass) and glass-infiltrated ZTA (IZ-glass). The biaxial flexural strength (piston-on-three-balls test) and Vickers microhardness were compared among groups (n=10 specimens in each group). Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) were used to investigate the structural characteristics of specimens at the fracture and cross-sectional surfaces. For both IA-SOD and IZ-SOD, the biaxial flexural strength exceeded the required value of 100–150 MPa as specified by ISO 6872(2015), indicating their potential as all-ceramic core materials. The flexural strengths and Vickers microhardness of IZ-SOD were respectively 324.7 MPa and 1162 VHN, while these values were measured 233.6 MPa and 1013 VHN for IA-SOD. The mechanical properties and microstructure of core materials have been advocated as crucial to the clinical performance of all-ceramic dental restorations. This investigation provides data regarding the flexural strength, hardness and microstructure of partially sintered alumina and ZTA frameworks with synthesized sodalite zeolite infiltration.     

Fabrication of toughened B4C composites with high electrical conductivity using MAX phase as a novel sintering aid

MAX phase Ti₃AlC₂ was chosen as a novel sintering aid to prepare electrically conductive B₄C composites with high strength and toughness. Dense B₄C composites can be obtained at a hot-pressing temperature as low as 1850 °C with 15 vol% Ti₃AlC₂. The enhanced sinterability was mainly ascribed to the in situ reactions between B₄C and Ti₃AlC₂ as well as the liquid phase decomposed from Ti₃AlC₂. Both the Vickers hardness and fracture toughness increase with increasing Ti₃AlC₂ amount, and high hardness and toughness values of 28.5 GPa and 7.02 MPa m^−1/2 respectively were achieved for B₄C composites sintered with 20 vol% Ti₃AlC₂ at 1900 °C. Crack deflection by homogenously distributed TiB₂ particles was identified as the main toughening mechanism. Besides, B₄C composites sintered with Ti₃AlC₂ show significantly improved electrical conductivity due to the percolation of highly conductive TiB₂ phase, which could enhance the machinability of B₄C composites largely by allowing electrical discharge machining.     

Hot pressing of bimodal alumina powders with magnesium aluminosilicate (MAS) addition

High quality alumina ceramics were fabricated by hot-pressed sintering using bimodal alumina with superfine component as raw material and magnesium aluminosilicate (MAS) glass as sintering aid. Densification behavior, microstructure evolution and mechanical properties of alumina were investigated from 1300 °C to 1450 °C. The bimodal alumina powders were sintered to 99.8% of the theoretical value at 1400 °C and a comparative dense microstructure with a few plate-like abnormal grains was observed. With increase of sintering temperature up to 1450 °C, many fine matrix grains were consumed and quite a few abnormal grains impinged upon each other. For the alumina ceramics hot-pressed from bimodal alumina with 30 wt.% superfine component, optimal mechanical properties were obtained at 1400 °C. The bending strength and fracture toughness were 522 MPa and 5.0 MPa m^1/2, respectively.     

Microstructural evolution,mechanical and thermal properties of LaB6 embedded in Si-B-C-N prepared by spark plasma sintering

Si-B-C-N monoliths with 5 wt% LaB₆ additives were prepared by spark plasma sintering at 1250–2000 °C and 50 MPa using a mechanically alloyed mixture of graphite, c-Si, h-BN and LaB₆ powders as the starting materials. Microstructural evolution, mechanical and thermal properties of the as-prepared La/Si-B-C-N monoliths were investigated. The densification of the ceramics starts at 1160° and ends at 1800 °C with the formation of La-containing compounds coupled with SiC and BN(C) phases. La-containing BN(C) grains develop into a lamellar structure at 1900 °C offering improved fracture toughness and decreased Vickers hardness, flexural strength and elastic modulus. The formation of lamellar BN(C) is also responsible for a high thermal expansion coefficient of 4.2×10⁻⁶ /°C.     

Mechanical and physical behaviors of short pitch-based carbon fiber-reinforced HfB2–SiC matrix composites

Short Pitch-based carbon fiber-reinforced HfB₂ matrix composites containing 20 vol% SiC, with fiber volume fractions in the range of 20–50%, were manufactured by hot-press process. Highly dense composite compacts were obtained at 2100 °C and 20 MPa for 60 min. The flexural strength of the composites was measured at room temperature and 1600 °C. The fracture toughness, thermal and electrical conductivities of the composites were evaluated at room temperature. The effects of fiber volume fractions on these properties were assessed. The flexural strength of the composites depended on the fiber volume fraction. In addition, the flexural strength was significantly greater at 1600 °C than at room temperature. The fracture toughness was improved due to the incorporation of fibers. The thermal and electrical conductivities decreased with the increase of fiber volume fraction, however.     

Preparation and properties of in-situ mullite whiskers reinforced aluminum chromium phosphate wave-transparent ceramics

In-situ mullite whisker reinforced aluminum chromium phosphate wave-transparent ceramics were designed and prepared. The phase transformation, microstructure, mechanical and electrical properties of the ceramics were investigated, and the mechanisms of in-situ growth and toughening were discussed. Results indicated that the in-situ growth of mullite whisker significantly improved the mechanical properties of the matrix, especially the high temperature flexural strength. The room temperature flexural strength, 1000 °C flexural strength and fracture toughness of the ceramics were 135.60 MPa, 121.71 MPa and 4.52 MPa m^1/2. After sintering at 1500 °C, the optimum properties of ε^'_r, tanδ and microwave transmittance at region 8–12 GHz were <3.6, <0.03 and>80%, respectively. The sinterability of ACP matrix was improved by the in-situ process of high mullization above 1450 °C. Using ACP binder as the raw material can avoid the phase transformation from B-AlPO₄ to T-AlPO₄. The synthesized mullite whiskers played a role in toughening by whiskers fracture, crack deflection and whisker pulling out.     

Microstructure and mechanical properties of ZTA composites fabricated by oscillatory pressure sintering

The influence of sintering temperature on the microstructure and mechanical properties of Al₂O₃?20 wt% ZrO₂ composites fabricated by oscillatory pressure sintering (OPS) was investigated by means of X-ray diffraction, scanning electron microscopy, three-point bending test and Vickers indentation. Results were compared to specimens obtained by conventional hot pressing (HP) under a similar sintering schedule. The optimum oscillatory pressure sintering temperature was found to be 1600 °C; almost fully dense materials (99.94% of theoretical density) with homogeneous microstructure could be achieved. The highest flexural strength, fracture toughness and hardness of such composites reached 1145 MPa, 5.74 MPa m^1/2 and 19.08 GPa when sintered at 1600 °C, respectively. Furthermore, the oscillatory pressure sintering temperature could be decreased by more than 50 °C as compared with the HP method, OPS favouring enhanced grain boundary sliding, plastic deformation and diffusion in the sintering process.     

Spark plasma sintering of silicon nitride/barium aluminum silicate composite

Si₃N₄ based composites were successfully sintered by spark plasma sintering using low cost BaCO₃, SiO₂ and Al₂O₃ as additives. Powder mixtures were sintered at 1600–1800 °C for 5 and 10 min. Displacement-temperature-time (DTT) diagrams were used to evaluate the sintering behavior. Shrinkage curve revealed that densification was performed between 1100 and 1700 °C. The specimen sintered at 1700 °C showed the maximum relative density (99.8±0.1%), flexural strength (352±16 MPa), Vickers harness (11±0.1 GPa) and toughness (5.6±0.05 MPa m^1/2).