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.     

Multiscale modelling of the thermoelastic properties of alumina-zirconia ceramics for 3D printing

Additive manufacturing appears to facilitate the accurate manufacturing of alumina-zirconia technical ceramics. Nevertheless, the fine tuning of the manufacturing of these components by 3D printing requires an analysis of the parameters that influence their final thermoelastic properties. In this context, this work presents the application of (finite element-based) numerical procedures that aim at the prediction of the effective thermoelastic properties of 3D-printed alumina-zirconia ceramics. The numerical modelling considers three different scales: micro-, meso- and macroscale. The microscale corresponds to the microstructural level of, sintered at 1500 °$\mathrm{C}$, slip-casted samples with different compositions of alumina-zirconia. On the other hand, the macroscale corresponds to the macrostructural level of porous lattice of 3D-printed ceramics, being defined at the mesoscale level by a periodic unit cell. Thus, an initial microstructural analysis (at microscale level) provides the influence of the alumina/zirconia ratio on the (macroscopically homogeneous and isotropic) material thermoelastic properties, which together with the definition of the geometry of a periodic unit cell (at mesoscale level), provides, by a second analysis (at both the meso- and macroscale levels), the coupled influence of material and geometry of the macrostructural lattice on the structural (macroscopically heterogeneous and anisotropic) thermoelastic properties. Moreover, experimental thermoelastic properties of the sintered slip-casted specimens were obtained for several alumina/zirconia ratios and analysed together with microstructure patterns. Prediction of the microstructural effective thermoelastic properties was also made using micromechanics and composite theory (analytical) models. All the numerical, experimental and analytical results for the microstructural level are presented and compared. Numerical results for the meso- and macrostructural levels are also presented.     

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.     

Processing and mechanical properties of new hierarchical metal-graphene flakes reinforced ceramic matrix composites

Hierarchical tantalum-graphene flakes reinforced zirconia (3Y-TZP) ceramic matrix composites were fabricated by wet processing route and freeze drying followed by spark plasma sintering (SPS). The microstructures and mechanical properties were investigated. The results show that graphene and Ta particles are homogeneously dispersed in the ceramic matrix and the optimum sintering temperature for complete densification of composites and thermal reduction of the graphene oxide is 1500 °C. The addition of dual reinforcements of tantalum microflakes and graphene nanoflakes results in significant improvement in the mechanical properties of the ZrO₂ matrix. Approximately a 30% increase in flexural strength vs the zirconia-Ta composite and a 175% increase in fracture toughness vs the monolithic zirconia have been achieved by introducing 0.5 vol% GO and 20 vol% Ta particles.     

Surface modification of graphene oxide nanoplatelets and its influence on mechanical properties of alumina matrix composites

This paper discusses the effect of modified graphene oxide nanoplatelets (RGO-Al₂O₃) and unmodified graphene oxide nanoplatelets (GO) addition on the microstructure and mechanical properties of alumina matrix composites. The sinters were prepared by powder metallurgy processing using Spark Plasma Sintering to consolidate the powder mixtures. Moreover, the influence of applied reinforcing phase on the fracture mechanism was also investigated. Significant improvement of the fracture toughness (60%) for the composites with 0.5 wt.% RGO-Al₂O₃ compared to the reference sample was observed. Moreover, 20% higher K_IC was noticed for RGO-Al₂O₃ reinforced composites than for Al₂O₃-GO.     

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.     

Effect of graphite nanoplatelets on the mechanical properties of alumina-based composites

Al₂O₃-based composites using exfoliated graphite nanoplatelets (xGnPs) have been developed by powder metallurgy (PM) route using both conventional as well as spark plasma sintering (SPS) processes. Al₂O₃-0.2, 0.5, 0.8, 3 and 5 vol% xGnP composites have been developed, and the effect of the addition of xGnP on the density, hardness, fracture toughness and wear behaviour of the various Al₂O₃-xGnP composites have been analyzed. Conventional sintering was done at a temperature of 1650 °C for 2, 3 and 4 h in inert atmosphere, whereas SPS was carried out at 1450 °C under 50 MPa pressure for 5 min. A uniform dispersion of the xGnP in the Al₂O₃ matrix was observed in the composites upto the addition of 3 vol% xGnP. Results indicate that a significant improvement in hardness, wear resistance and fracture toughness of the composites could be achieved by using xGnP as nanofiller. The hardness and fracture toughness of the composites developed by both conventional sintering and SPS show an increase upto the addition of 3 and 0.8 vol% xGnP respectively. The wear resistance of the composites also shows significant improvement upto the addition of 3 vol% xGnP. The composites developed by SPS have been found to possess superior mechanical properties as compared to the composites developed by conventional sintering. The improvement in the mechanical properties can be attributed to the strong interaction between the xGnP and the Al₂O₃ matrix at the interfaces and to the toughening mechanisms such as crack bridging and crack deflection.     

Effect of zirconia addition amount in glaze on mechanical properties of porcelain slabs

Applying toughened glaze layer on porcelain slabs can improve the fracture toughness of slabs and greatly reduce the production cost. In this study, porcelain slabs glaze with high toughness was fabricated by the processes of impregnation glazing and single firing method, using opaque frits, kaolin clay as the main raw materials, zirconia as an additive, and the effect of the addition amount of zirconia in glaze on fracture toughness of porcelain slabs was investigated. The results showed that the type and content of crystal phase of the glaze were greatly influenced by the addition amount of zirconia. Meanwhile, compared with the base glaze, the hardness and fracture toughness of the sample with zirconia glaze were significantly improved. Porcelain slabs with 10 wt% zirconia in glaze, sintering at 1200 °C, exhibited higher quality glaze and outstanding properties, including a water absorption of 1.95%, a Vickers hardness of 6.36 GPa, and a fracture toughness of 2.71 MPa m^1/2. The toughening mechanism of the glaze layer was as follows: a large number of zirconium silicate grains with high hardness were generated by the reaction of added zirconia with silica in the glass phase, which increased the content of crystal phase and then prevented the propagation of cracks; moreover during the martensitic transformation of the tetragonal zirconia grains, the volume and shear strain were generated to offset the stress field generated by the crack tip, thus toughening the material.     

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.     

Synthesis and characterization of zirconia toughened alumina ceramics prepared by co-precipitation method

Undoped and 3 mol% yttrium doped ZrO₂–Al₂O₃ composite powders with partially stabilized ZrO₂ (PSZ) content varying from 0 to 30 wt% were prepared by a co-precipitation route using inorganic precursors Al(NO₃)₃, ZrOCl₂ and Y(NO₃)₃. The precipitates were characterized by DTA and subsequently calcined at 1200 °C for 4 h to achieve fine grained composite powders. The calcined powders were characterized by FTIR and XRD. In order to enhance the sinterability, the calcined powders were wet milled in a high energy ball mill. Powders were uniaxially pressed to form pellets and sintered at 1600 °C for 5 h to achieve greater than 96% relative density. Microstructural analysis of the sintered compacts revealed the uniform distribution of the zirconia particles among the alumina matrix. It was also observed that the faceted intergranular zirconia grains were present at the grain boundaries and junctions in the alumina matrix. Vickers indentation was carried out at 1 kgf load for hardness and 2 kgf load for estimating the critical stress concentration factor (K_c). Microscopic studies of the indented samples showed that cracks were propagating around the grain boundaries. Highest K_c ∼8.40 ± 0.4 MPa√m and hardness ∼16.31 ± 0.58 GPa was obtained for the 30 wt% PSZ-Al₂O₃ composite. The sintered density and critical stress intensity factor (K_c) achieved were compararble to that achieved earlier by hot press and SPS.     

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.     

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.     

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).     

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.     

Microstructure and mechanical properties of hot-pressed SiC nanofiber reinforced SiC composites

This study reports on the preparation and mechanical properties of a novel SiC_nf/SiC composite. The single crystal SiC nanofiber(SiC_nf) reinforced SiC ceramic matrix composites (CMC) were successfully fabricated by hot pressing the mixture of β-SiC powders, SiC_nf and Al–B–C powder. The effects of SiC_nf mass fraction as well as the hot-pressing temperature on the microstructure and mechanical properties of SiC_nf/SiC CMC were systematically investigated. The results demonstrated that the 15 wt% SiC_nf/SiC CMC obtained by hot pressing (HP) at 1850 °C with 30 MPa for 60 min possessed the maximum flexural strength and fracture toughness of 678.2 MPa and 8.33 MPa m^1/2, respectively. The nanofibers pull out, nanofibers bridging and cracks deflection were found by scanning electron microscopy, which are believed can strengthen and toughen the SiC_nf/SiC CMC via consuming plenty of the fracture energy. Besides, although the relative density of the prepared SiC_nf/SiC CMC further increased with the sintering temperature rose to 1900 °C, the further coarsend composites grains results in the deterioration of the mechanical properties for the obtained composites compared to 1850 °C.     

Processing and characterization of fiber-reinforced and layered alumina - graphene composites

The aim of the present contribution is the processing and characterization of fiber-reinforced and layered alumina - graphene composites, prepared by the combination of electrospinning, calcination, chemical vapor deposition (CVD) and spark plasma sintering (SPS). The fiber-reinforced composite contains homogenously distributed graphene-coated polycrystalline alumina microfibers in the Al₂O₃ matrix. The layered composites contain Al₂O₃ layers and layers of graphene-coated alumina microfibers or layers of graphene-coated alumina grains of submicron size. The systems with high density, 99.5–99.9 %, show different grain sizes of Al₂O₃ in their constituents, changing from 0.08 to 1.9 μm in comparison to the monolithic alumina with the average grain size of 2.6 μm. The composites and their layers show increased electrical conductivity, hardness, and fracture toughness by approximately five orders of magnitude, 31 %, and 8%, respectively, in comparison to the monolithic alumina due to the presence of graphene layers, small grain-sized alumina, and microfibers in the composites.