Hydroxyapatite/bioactive glass functionally graded materials (FGM) for bone tissue engineering

In this work, HA/bioactive glass Functionally Graded Materials (FGMs) are obtained for the first time by means of Spark Plasma Sintering (SPS). Two series of highly dense 5 layered products, namely FGMS1 and FGMS2, are prepared under optimized SPS conditions, i.e. 1000 °C/2 min/16 MPa and 800 °C/2 min/50 MPa, respectively, using a die with varying cross section.Results arising from XRD, SEM, mechanical and biological characterization in SBF, evidence that lower temperature and higher-pressure levels used for FGMS2 samples provide better materials in terms of microstructure, compactness, hardness, elastic modulus and in vitro bioactivity. Indeed, a fully sintered and crack-free microstructure with no crystallisation at the top layer (100% bioactive glass) is correspondingly produced.The obtainment of such FGMs is quite promising, since it permits to vary the relative volume fractions of the two constituents and, consequently, tailor the biological response for specific clinical applications.     

Zirconia ultrafiltration membranes on silicon carbide substrate: microstructure and water flux

This study reported the preparation of ZrO₂/SiC ceramic membrane with silicon carbide as the substrate and intermediate layers and zirconia as the selective layer. The substrate and intermediate layers were sintered by evaporation-condensation process at 2200 and 1900 ℃, respectively. After sintering, the intermediate layer presented layer thickness of 50 μm, pore size of 0.87 μm and pure water permeability of 2140 L/(m²·h). The selective lay was deposited on the silicon carbide substrate by dip-coating method and then sintered in the temperature range from 800 to 1000 ℃. For the membrane coated by one dip-coating cycle and sintered at 800 ℃, it presented average pores of 82 nm and water flux of 850 L/(m²·h). Due to the exclusion of low-melting oxides during sintering, the ZrO₂/SiC ceramic membrane can satisfy the separation and purification of chemical corrosion and high temperature wastewater.     

Effect of the sintering temperature on microstructure and properties of Al2O3–Cu–Ni hybrid composites obtained by PPS

In the present research, the influence of sintering temperature on the microstructure and properties of Al₂O₃–Cu–Ni hybrid composites prepared by the Pulse Plasma Sintering (PPS) technique were described. In this research, three temperatures have been selected: 1250°C, 1300°C, and 1350°C. SEM observations were carried out to determine the distribution of the metallic phase in the composite depending on the sintering temperature. The conducted experiments and microscopic observations enabled a better understanding of the phenomena occurring between the ceramic matrix and metallic phase in the obtained materials. The mechanical properties like a hardness and fracture toughness were measured. The technology applied allowed us to obtain ceramic-metal composites with a homogeneous microstructure. It was found that the sintering temperature influences the selected physical and mechanical properties of the composites produced. It was found that samples produced at 1300°C are characterized by the highest relative density and the mechanical properties.     

Role of MgO on densification and mechanical properties in spark plasma sintered Os0.9Re0.1B2 ceramic

To promote the densification and therefore the mechanical properties of boride-based ceramics, MgO was added as sintering aid into Os_0.9Re_0.1B₂ powders for densification by using spark plasma sintering (SPS). The Os_0.9Re_0.1B₂ powders were synthesized by mechanochemical method from powder mixture of Os, Re and amorphous B. The role of MgO on densification, phase composition, microstructure and mechanical properties (hardness, fracture toughness and wear behavior) were studied by using X-ray diffraction (XRD), scanning electron microscope (SEM) with energy-dispersive spectroscopy (EDS), micro indentation and ball-on-disk tribometer. The results show that, with the introduction of MgO as sintering aid, the relative density of the Os_0.9Re_0.1B₂ ceramic samples increased. When the MgO content reached 9 wt%, the as-sintered sample is almost fully dense. No obvious regularity was found from the samples with the addition of different content of MgO. Vickers hardness values of the samples with 0, 3 wt% and 9 wt% MgO are found to be very close with each other within the experimental error (~30 GPa), while the sample with the addition of 6 wt% MgO exhibits the highest hardness of ~35 GPa. The fracture toughness of the samples is decreased slightly with the addition of MgO. The friction coefficient and wear rate of the sample with the addition of 6 wt% MgO was also found to be the lowest among all samples, which indicate best wear resistance. As a whole, with the addition content of 6 wt% MgO, the Os_0.9Re_0.1B₂ ceramic sample performs relatively excellent mechanical properties among four groups of samples.     

Preparation of biphasic hydroxyapatite/ β-tricalcium phosphate foam using the replication technique

Biphasic hydroxyapatite/β-tricalcium phosphate foams were prepared using the replication technique starting from a precipitated hydroxyapatite (Ca₁₀(PO₄)₆(OH)₂: HAP) powder, and sodium glycerophosphate (GP). The effect of the grinding time, solid loading, dispersant amount, and etching, replication, and sintering processes were investigated. The SEM, OEM and FTIR analyses proved that the surface of the polyurethane template must be treated with NaOH solution to make it more hydrophilic prior to the coating process. With a solid loading of 40 wt-%, the slurries prepared from the precipitated hydroxyapatite presented a shear thinning behavior, which was useful for the coating process. The SEM analysis of the foams showed that the optimum number of coating layers to obtain foam with an identical structure with the template was limited to three. The use of GP and the optimized preparation parameters helped to decrease the consolidation temperature of the ceramic foams to 1000 °C. The XRD and FTIR analyses of the prepared foams showed that the thermal treatment of the GP and the HAP mixture led to a partial decomposition of the HAP to tricalcium phosphate. The fitting of the XRD patterns and the obtained lattice parameters proved that the decomposition was accompanied by the insertion of sodium from GP toward the lattice of tricalcium phosphate and the formation of Na-β-tricalcium. The results of the SEM analysis, the pore size distribution and the mechanical strength showed that the presence of the Na-β-tricalcium reduced the pore size distribution from 500-2700 to 100–1700 μm, decreased slightly the total porosity from 80 vol-% to 70 vol-%; and improved the mechanical strength of the obtained foam from 1.56 MPa to 2.60 MPa.     

Influence of processing conditions on the ionic conductivity of holmium zirconate (Ho2Zr2O7)

Nanopowders of holmium zirconate (Ho₂Zr₂O₇) synthesised through carbon neutral sol-gel method were pressed into pellets and individually sintered for 2 h in a single step sintering (SSS) process from 1100 °C to 1500 °C at 100 °C interval and in a two step sintering (TSS) process at (I) −1500 °C for 5 min followed by (II) - 1300 °C for 96 h. Relative density of each of the sintered pellet was determined using the Archimedes’ technique and the theoretical density was calculated from crystal structure data. Grain size was obtained from SEM micrographs using ImageJ. Pellets processed by TSS have been found to be denser (98 %) with less grain growth (1.29 μm) as compared to the pellets processed using SSS process. Ionic conductivity of Ho₂Zr₂O₇ pellets sintered by two different processes was measured using ac impedance spectroscopy technique over the temperature range of 350 °C–750 °C in the frequency range of 100 mHz–100 MHz for both heating and cooling cycles. The temperature dependence of bulk (2.67⨯10⁻³ Scm⁻¹) and grain boundary (2.50⨯10⁻³ Scm⁻¹) conductivities of Ho₂Zr₂O₇ prepared by TSS process are greater than those processed by SSS process suggesting the strong influence of processing conditions and grain size. Results of this study, indicates that the TSS is the preferable route for processing the holmium zirconate as it can be sintered to exceptionally high densities at lower temperature, exhibits less grain growth and enhanced ionic conductivity compared with the samples processed by SSS process. Hence, holmium zirconate can be considered as a promising new oxide ion conducting solid electrolyte for intermediate temperature SOFC applications between 350 °C and 750 °C temperature range.     

High performance lead-free Na0.5K0.5NbO3 piezoelectric ceramics obtained via oscillatory hot-pressing

Lead-free Na_0.5K_0.5NbO₃ (KNN) piezoelectric ceramics is regarded as a potential candidate for PZT material, while high performance is difficult to be obtained due to its poor sinterability and non-stoichiometric component. In this work, oscillatory pressure-assisted hot pressing (OPAHP) is utilized to fabricate KNN ceramics with high density. The KNN ceramics sintered at 860 °C exhibits superior performance with piezoelectric parameter (d₃₃) of 142 pC/N, electromechanical coupling factors (k_p) of 0.41, and relative permittivity (ε^T₃₃/ε₀) of 472–620. Additionally, hardness and flexural strength are measured as 3.55 GPa and 99.13 MPa, respectively. This work indicates that OPAHP technique is effective for fabricating KNN piezoelectric ceramics with high performance.     

Fabrication of Ti3SiC2-based composites via three-dimensional printing: Influence of processing on the final properties

In this work the influence of the processing routes on the microstructure and properties of Ti₃SiC₂-based composites was investigated. The three main processing steps are (i) three-dimensional printing of Ti₃SiC₂ powder blended with dextrin, (ii) pressing of printed samples (uniaxial or cold isostatic pressing), and (iii) sintering of pressed samples at 1600 °C for 2 h. The Ti₃SiC₂-based composites were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDS). Young's Modulus and flexural strength were measured to examine the mechanical properties. Porosity, density, shrinkage, and mass change were measured at each processing step. Those samples uniaxially pressed at 726 MPa presented the highest density, shrinkage, and mass change. However, microstructural morphologies were crack-free and homogeneous for cold isostatic pressed Ti₃SiC₂-based composites as compared to uniaxially pressed samples. The highest values for Young's Modulus (~300 GPa) and flexural strength (~3 GPa) were observed with uniaxially pressed Ti₃SiC₂-based composites.     

Liquid-phase flash sintering 8YSZ with alkali halide sintering aids

The properties of ZrO₂: 8 mol% Y₂O₃ (8YSZ) ceramics with LiF and KCl sintering aids for liquid phase formation during electric field-assisted sintering were studied. Sintering experiments were carried out at 650 °C under 200 V cm⁻¹ AC electric field by varying current density, current application time, as well as LiF and KCl contents. Pellets sintered with KCl addition had cavities, cracks and fractures. Pellets sintered with 15 wt.% LiF, on the other hand, were homogeneous after thermal removal of LiF upon Joule heating. Low electric current densities coupled with longer application times produced homogeneous specimens. Three different stages were identified during sintering experiments: (i) LiF melting with the electric field applied at furnace temperatures lower than its melting point, (ii) shrinkage due to liquid phase formation and LiF removal, (iii) final densification due to grain growth and pore elimination. The electrical behavior and an estimate of the porosity were carried out by electrochemical impedance spectroscopy measurements.     

Effect of Nb2O5 content and sintering temperature on the microstructure and bending strength of porous Ni-YSZ cermets

Porous Ni-YSZ cermets are prepared by reducing NiO-YSZ composites upon exposure to (Ar+6% H₂) gas. The porous cermets are prepared by the addition of carbon black (0.123 mol) to mixed NiO-YSZ powders and the conversion of NiO to Ni in the NiO-YSZ composites. The microstructure and bending strength of porous Ni-YSZ cermets as functions of sintering temperature and Nb₂O₅ content are discussed. The Ni-YSZ cermets consist of uniformly distributed Ni and YSZ grains as well as pores. Both higher sintering temperature and higher Nb₂O₅ content yield lower porosity, thus increasing the bending strength. The bending strength of 0.00470 mol% Nb₂O₅–containing Ni-YSZ cermets sintered at 1400 °C (111 MPa) is about two times higher than that of Nb₂O₅–free Ni-YSZ cermets sintered at 1400 °C (59 MPa).