Effect of printing parameters on mechanical properties of extrusion-based additively manufactured ceramic parts

The purpose of this study is to investigate the effect of printing parameters on the physical and mechanical properties of additively manufactured ceramics (alumina and zirconia). Sample parts were obtained by extrusion-based additive manufacturing of a ceramic-binder mixture and subsequent post-processing (debinding and sintering). Their mechanical properties (microhardness, flexural strength, toughness) were measured and correlated with the printing parameters. Part orientation is the most significant factor for microhardness and flexural strength in both ceramic materials. Parts with vertical orientation show higher hardness while horizontal samples show higher flexural strength compared to their respective counterparts. Extrusion velocity was found to be insignificant for hardness and flexural strength. However, a marginal increase in fracture toughness with the increase in the extrusion velocity was observed. The fracture toughness of additively manufactured ceramics shows an increasing trend with elastic modulus and flexural strength and a decreasing trend with hardness and sintered density.     

Impact of sandblasting on the mechanical properties and aging resistance of alumina and zirconia based ceramics

Bioinert zirconia and alumina ceramic devices are widely used, both in orthopaedics and in dentistry. In order to improve their bonding with bone tissues or dental resin cements, their surfaces are often roughened at different scales. In this work, we have investigated the effects of the same sandblasting treatment on alumina, zirconia and a zirconia-toughened alumina, focusing on their mechanical performance and the interplay between surface defects and residual stresses. Additionally, we explored the impact of the treatment on the hydrothermal aging of the two zirconia-containing materials. Residual stresses generated during sandblasting were always predominant over surface defects but their effect varied with the material: while they had a weakening effect on alumina, they reinforced both zirconia-containing materials. Finally, we found that the monoclinic grains at the surface of sandblasted zirconia recrystallized into tetragonal nanograins after annealing and this led to an increased resistance to aging.     

Microstructure and flexural properties of multilayered fiber-reinforced oxide composites fabricated by a novel lamination route

All-oxide ceramic matrix composites produced by a novel route based on the lamination of thermoplastic prepregs are investigated. This route allows for the production of composites with very homogeneous microstructures and a reduced amount of matrix cracks. Nextel^TM 610 alumina woven fabric is used here to reinforce a porous oxide matrix composed of 80 vol% Al₂O₃ and 20 vol% ZrO₂. The mechanical behavior of composites submitted to different heat treatments is investigated under 4-point bending and short beam shear. Results show that composites with low interlaminar shear strength present a graceful failure under 4-point bending, characterized by a stepwise stress reduction upon straining beyond the peak stress. The fracture of such composites is accompanied by a series of interfacial delamination events, which enhance energy dissipation during failure. An increase of the interlaminar shear strength due to matrix densification causes a loss of the stepped stress–strain behavior. Nevertheless, fiber-related toughening mechanisms such as crack deflection and bridging still ensure inelastic deformation up to failure of these composites.     

Processing of yttria stabilized zirconia reinforced with multi-walled carbon nanotubes with attractive mechanical properties

The improvement of the mechanical properties of carbon nanotube reinforced polycrystalline yttria-stabilized zirconia (CNT-YSZ) was questionable in earlier investigations due to several difficulties for processing of these composites. In the present article, the authors are proposing a successful technique for mixing pre-dispersed CNTs within YSZ particles followed by a fast spark plasma sintering at relatively low temperature, resulting in near full-dense structure with well-distributed CNTs. Composites with CNT quantities ranging within 0.5-5 wt% have been analyzed and a significant improvement in mechanical properties, i.e. Young's modulus, indentation hardness and fracture toughness with respect to monolithic YSZ could be observed. To support these interesting mechanical properties, high-resolution electron microscopy and Raman spectroscopy measurements have been carried out. The analysis of densification shows that the lower densification rate of CNT reinforced composites with respect to the pure YSZ could be attributed to a slower grain boundary sliding or migration during sintering.     

Fracture behavior of Ce-TZP/alumina/aluminate composites with different amounts of transformation toughening. Influence of the testing methods

The fracture behavior of four Ce-TZP zirconia composites containing 8 vol% alumina and 8 vol% strontium hexa-aluminate was investigated. The composites exhibited different degrees of transformation toughening obtained by varying the amount of the CeO₂ stabilizer and the sintering temperature. The strength was measured by 4-point bending (4PB) and piston-on-three balls (POB) methods Toughness and crack growth resistance (R-curve) were determined from Single Edge V-Notched Beam (SEVNB) and double torsion (DT) samples, and slow crack growth (SCG) curves were determined by DT method.Increasing the transformability of the composites enhanced their crack growth resistance and consequently, increased their resistance to SCG, which was completely inhibited for the most transformable composites. Simultaneously, flaw tolerance was also improved although a decrease in strength was observed. Under all configurations, the composites exhibited a plastic behavior and it was shown that their properties are correlated to the crack shielding due to autocatalytic phase transformation that not only depend on the material transformability, but is also strongly influenced by the testing method.     

Mechanical and thermal properties of spark plasma sintered Al2O3-graphene-SiC hybrid composites

Monolithic Al₂O₃ and Al₂O₃-graphene-SiC hybrid composites were prepared by spark plasma sintering (SPS) under vacuum atmosphere. The results show that the hybrid composites were almost completely dense (>97%). SiC content has a significant effect on the microstructure of the composites. With the increase of SiC content, the average grain size of alumina decreased gradually. The addition of SiC to alumina changed fracture mode from inter-granular fracture to mixed fracture mode of inter-granular fracture and trans-granular fracture. The Al₂O₃-0.4 wt%graphene-5 wt% SiC hybrid composite has the highest bending strength and hardness, which were 57% and 19.22% higher than those of the monolithic alumina, respectively. The room temperature (RT) thermal conductivity of the monolithic Al₂O₃ (25.5 W/m·K) was the highest. The thermal conductivity and thermal diffusivity coefficient of the composites decreased with the increase in temperature, while the specific heat of monolithic alumina and composites increased with the increase in temperature and additives. These properties were related to the microstructure of materials and the possible transport mechanisms were discussed.     

Characterization of thermochemical properties of Al nanoparticle and NiO nanowire composites

Thermochemical properties and microstructures of the composite of Al nanoparticles and NiO nanowires were characterized. The nanowires were synthesized using a hydrothermal method and were mixed with these nanoparticles by sonication. Electron microscopic images of these composites showed dispersed NiO nanowires decorated with Al nanoparticles. Thermal analysis suggests the influence of NiO mass ratio was insignificant with regard to the onset temperature of the observed thermite reaction, although energy release values changed dramatically with varying NiO ratios. Reaction products from the fuel-rich composites were found to include elemental Al and Ni, Al₂O₃, and AlNi. The production of the AlNi phase, confirmed by an ab initio molecular dynamics simulation, was associated with the formation of some metallic liquid spheres from the thermite reaction.     

On the fracture toughness of calcium aluminate cement-phenol resin composites

Macro-defect-free (MDF) cement with high flexure strength has been an active research area over several decades. To study the tensile properties of these materials, it is essential to understand the mode I crack propagation. In this article, cleavage cracking in calcium aluminate cement (CAC)-phenol resin composites is analyzed based on an energy method. The crack-trapping effect of the cement particles is found to be significant. The fracture toughness rises with the particle size and is independent of the spacing between the particles. When the cement volume fraction is higher than a critical value the effective work of separation of the phenol resin decreases with the particle content with a coefficient of −1.88.     

Role of cement content on the properties of self-flowing Al2O3 refractory castables

In this work, Al₂O₃ self-flowing castables (SFCs) were produced based on various cement contents. The SFCs were sintered at 1273 K, 1573 K and 1773 K and the exhibited properties were experimentally determined. Among the properties determined in this work are bulk density (BD), apparent porosity (AP), water absorption (WA), cold crushing strength (CCS), modulus of rupture (MOR) and fracture toughness (K_IC). It is found that additions of 5% cement lead to SFCs with maximum MOR and K_IC values after firing at 1773 K. Firing at 1573 K leads to a reduction in both, MOR and K_IC. In SFC containing 3% cement, maximum K_IC values of 3.53 MPa m^1/2 were achieved after firing at 1573 K. In the low cement SFCs (1 wt%) after firing at 1773 K the exhibited K_IC values were below those obtained in either the SFC-3 or SFC-5, but they were significantly high (3.43 MPa m^1/2).     

Mechanical properties of graphene oxide reinforced alumina matrix composites

Graphene oxide (GO) reinforced alumina matrix composites have been fabricated by using graphene oxide synthesized by a modified Hummer's method. Samples were prepared by powder metallurgy and consolidated by Spark Plasma Sintering (SPS). The influence of GO addition on the microstructure and mechanical properties of the composites was investigated. Results show a significant increase (almost 35%) of the fracture toughness for composites containing 0.5 wt% graphene oxide compared to sintered pure alumina. In order to find reasons for this improvement Scanning/Transmission Electron Microscopy (SEM/TEM) observations were carried out. They reveal a good interface between the reinforcement and the matrix as well as such mechanisms like branching, deflection and bridging of crack propagation.     

莫来石纤维增强铝硅酸盐陶瓷的强度及断裂韧性

通过对莫来石纤维、铝硅酸盐陶瓷基体及复合材料力学参数的测定,以及通过扫描电镜、电子探针等观察,对复合材料的强度及断裂韧性进行了分析,认为这两种材料的复合是匹配的。本课题所试制的铝硅酸盐陶瓷基体的强度和断裂韧性有较大的提高。     

Determining the fracture toughness of ceramic filter materials using the miniaturized chevron-notched beam method at high temperature

The aim of the application of open cell ceramic foam filters during casting of metals is the reduction of non-metallic inclusions and turbulences in the melt flow. Hence, an improvement of the quality of the cast products is achieved. The integrity of the filter at mechanical loading under elevated temperatures requires a mechanical characterization of the bulk material of the filter. In particular, fracture toughnesses have to be determined for a new generation of filter materials. The presented work describes an experimental method to measure fracture toughnesses of the filter materials.The mechanical testing is performed with the help of 4-point-bending tests using miniaturized chevron-notched specimens at different temperatures. Additionally, the geometry function of the test set-up is calculated and compared with an empirical formula by Munz [1]. At the end, the fracture toughness is determined at room temperature and $800°\mathrm{C}$. Further results characterize the influence of different geometrical parameters of the test set-ups on the maximum tensile stresses in the specimen and the load-displacement curves.     

The formation and properties of Sialon-ZrN composites produced by reaction bonding combined with post gas-pressure sintering

Sialon-ZrN composites have been fabricated by a combination of reaction bonding and post-gas-pressure sintering. Composites with different amount of ZrN were post sintered at 1600, 1700 and 1800?°C under a nitrogen pressure of 0.7?MPa for 6?h. The results showed that mass loss due to decomposition increased with increasing sintering temperature. The mass loss at 1600 and 1700?°C was comparable, and below 3% even for the highest ZrN content of 50?wt%, but ranged between 6% and 9% for samples post sintered at 1800?°C with 10–50?wt% ZrN. Composites sintered at 1700?°C had the highest relative density (> 97%) and lowest open porosity (< 2%), and this was independent of ZrN content. The incorporation of the ZrN particles was observed to have an effect on the mechanical properties of the composites. The highest hardness (16.05?±?0.17?GPa) was observed for the composite sintered at 1700?°C with 20?wt% ZrN but decreased with higher ZrN contents, due to a weak bonding between the ZrN particles and the Sialon matrix. The fracture toughness showed a continuous increase with increasing ZrN content, due to the effect of the weak bonding on toughening mechanisms such as crack branching, crack deflection and crack bridging. The highest fracture toughness (5.35?±?0.18?MPa?m^1/2) was observed for the composited sintered at 1700?°C with 50?wt% ZrN.     

Al2O3/diopside ceramic composites and their behaviour in simulated body fluid

Al₂O₃/diopside ceramic composites with good mechanical properties were prepared by uniaxial hot-pressing and their biological activity in simulated body fluid was studied by SEM, XRD, FT-IR and EPMA. SEM micrographs showed a lath-like apatite layer to form on the soaked composite surface, whose good biological activity may be of some promise for biomedical application.     

Interface controlled micro- and macro- mechanical properties of aluminosilicate fiber reinforced SiC matrix composites

Novel Nextel™ 440 aluminosilicate fiber reinforced SiC matrix composites, with/without chemical vapor deposited carbon interphase were fabricated by polymer derived ceramic process, and they were studied by a combination of micro- and macro- mechanical techniques such as nanoindentation, micropillar splitting, fiber push-in, digital image correction and high temperature three point bend tests. Specifically, micropillar splitting test was firstly employed to measure in-situ the localized fracture toughness. The results revealed that the carbon interphase can effectively hinder the interfacial reactions between Nextel™ 440 fiber and SiC matrix, thus remarkably weakening the composite interfacial shear strength from ∼293 MPa to ∼42 MPa, and enhance the composite fracture toughness from ∼1.8 MPa√m to ∼6.3 MPa√m, respectively. This is mainly a consequence of weak interface that triggers crack deflection at the fiber/interphase interface. Finally, this novel composite showed stable mechanical properties in vacuum at temperature range from 25 °C to 1000 °C.     

塑性相结合刚玉复合材料的力学性能

在刚玉－碳化硅耐火材料中添加硅粉,利用硅粉所具有的金属塑性特征,使得制品具有了塑性成型的性质,而且提高了制品的致密化程度和断裂韧性,并达到了坯体增韧的效果。     

Microcracking of high zirconia refractories after t → m phase transition during cooling: An EBSD study

High zirconia refractories are composed of a zirconia skeleton surrounded by an intergranular glassy phase. In these materials, zirconia undergoes up to two successive phase transitions during the manufacturing process, c → t then t → m. This leads, after complete cooling, to the formation of microcracks.Preliminary observations have enabled to identify the mechanism mostly responsible for the observed microcracking. In particular, SEM imaging emphasizes the link between the positions of cracks and the presence of distinct crystallographic domains.Thus, our work focuses on the arrangement of the monoclinic and tetragonal domains in zirconia dendrites. The assessment by XRD of the thermal expansion coefficients of zirconia at the lattice scale and the analysis of EBSD maps show that cracking is produced by the thermal expansion mismatch between groups of crystallographic variants. The further reconstruction of both cubic and tetragonal - in the case of a presence of monoclinic zirconia at room temperature - parent grains enables to determine the impact of each transition on the final microstructure and the generated microcracking.     

Anisotropic mechanical and tribological properties of SiAlON matrix composites containing different types of GNPs

SiAlONs can have new application areas by increasing their lifetime and durability if their mechanical and tribological properties are improved. Even though the properties of the matrix improve with GNPs addition, the differences in GNPs properties lead to different property values. In this study, four different GNPs having different surface area, lateral dimension, thickness, and aspect ratio were added to SiAlON and composites were sintered by using SPS. The effects of these different properties on fracture toughness and friction coefficient of SiAlONs were investigated. GNPs, which have the high surface area, lateral dimension, aspect ratio and low thickness, provided the highest fracture toughness and best friction coefficient performance to SiAlON. The fracture toughness of composites were generally higher in the in-plane direction compared to through-plane direction due to GNPs orientation. Conversely, the friction coefficient and hardness values measured higher in the through-plane direction than in the in-plane direction.     

Hydration properties of vermiculite in phenolic resin friction composites

The dehydration and rehydration properties of the Mg-vermiculite are strongly affected by their crystal structure. Changes in the structure of Mg-vermiculite after dehydration and rehydration were used for evaluation of dehydration properties of composite materials containing vermiculite and phenol formaldehyde resin during friction process and for estimation of temperature on the surface of composite. From XRD patterns follows that d-spacing of the first basal diffraction varies as a function of applied annealing temperature and Mg-vermiculite alone rehydrates if the heating temperature does not exceed 700 °C. If embedded in a phenolic resin matrix, rehydration ability of vermiculite is limited and depends on vermiculite/resin content ratio. The maximum detected temperature on the friction surface of investigated composite samples after friction test was 900 °C.