Two-step sinter-crystallization of K2O–CaO–P2O5–SiO2 (45S5-K) bioactive glass

Bioactive glasses and glass-ceramics (GCs) effectively regenerate bone tissue, however most GCs show improved mechanical properties. In this work, we developed and tested a rarely studied bioactive glass composition (24.4K₂O-26.9CaO-46.1SiO₂-2.6P₂O₅ mol%, identified as 45S5-K) with different particle sizes and heating rates to obtain a sintered GC that combines good fracture strength, low elastic modulus, and bioactivity. We analyzed the influence of the sintering processing conditions in the elastic modulus, Vickers microhardness, density, and crystal phase formation in the GC. The best GC shows improved properties compared with its parent glass. This glass achieves a good densification degree with a two-step viscous flow sintering approach and the resulting GC shows as high bioactivity as that of the standard 45S5 Bioglass®. Furthermore, the GC elastic modulus (56 GPa) is relatively low, minimizing stress shielding. Therefore, we unveiled the glass sintering behavior with concurrent crystallization of this complex bioactive glass composition and developed a potential GC for bone regeneration.     

Effects of (Li0.5Sm0.5)/W co-substitution and sintering temperature on the structure and electrical properties of ultrahigh Curie temperature piezoceramics,Ca0.92(Li0.5Sm0.5)0.08Bi2Nb2-xWxO9

With co-substitution of (Li_0.5Sm_0.5) at A site and W at B site, the electrical properties of modified Ca_0.92(Li_0.5Sm_0.5)_0.08Bi₂Nb_2-xW_xO₉ [(CLS)BN-xW, x = 0, 0.015 and 0.03] piezoceramics with ultrahigh Curie temperature (T_C) of > 930 °C were enhanced dramatically. The increased resistivity induced by the co-substitution ensure them to be polarized under an enough high field. Combined with the increase of spontaneous ferroelectric polarization (P_S), the significant enhancements in the piezoelectric, dielectric and ferroelectric properties can be obtained in the composition x = 0.015. Furthermore, the piezoelectric activity (d₃₃) and bulk resistivity (ρ_b) of (CLS)BN-0.015 W can be further enhanced at an appropriate sintering temperature. This optimum composition sintered at 1170 °C shows ultrahigh T_C of ～948 °C, d₃₃ of ～17.3 pC/N and ρ_b of ～6.9 MΩ cm at 600 °C, which are comparable to those of the reported high-temperature Aurivillius piezoceramics with T_C > 850 °C.     

Synthesis and slurry spray coating of barium strontium alumino silicate on SiC substrate

Barium strontium alumino silicate (BSAS); (Ba_0.6Sr_0.4Al₂Si₂O₈) was synthesized through solid state reaction between BaCO₃, SrCO₃, Al₂O₃ and SiO₂ subjected to wet milling in isopropanol for about 24 h. The sequence of the solid state reaction was studied by subjecting to DG/DTG from room temperature to 1550 °C. The crystallographic phase evolution was confirmed by X-ray diffraction of the powders calcined in the range 1000 to 1300 °C for 2 h. The monoclinic celsian phase obtained at 1300 °C, pelletized through uniaxial pressing was sinterable to 67 to 78% density in the temperature range of 1300 to 1500 °C. The density improved to 75 to 94% after ball milling for 76 h, while ZrO₂ addition further improved the density by 2%. The celcian phase of BSAS was dispersed in isopropyl alcohol, milled for about 24 h and spray coated on to plain SiC and mullite precoated SiC substrates. Sintering of coated samples and characterization for weight gain/loss, microstructure, scratch test prove that mullite + BSAS coating is more effective than single layer coating of BSAS on SiC substrates.     

Transient liquid phase sintering of high-purity mullite for high-temperature structural ceramics

High-purity mullite ceramics, promising engineering ceramics for high-temperature applications, were fabricated using transient liquid phase sintering to improve their high-temperature mechanical properties. Small amounts of ultrafine alumina or silica powders were uniformly mixed with the mullite precursor depending on the silica-alumina ratio of the resulting ceramics to allow for the formation of a transient liquid phase during sintering, thus, enhancing densification at the early stage of sintering and mullite formation by the reaction between additional alumina and the residual glassy phase (mullitization) at the final stage of sintering. The addition of alumina powder to the silica-rich mullite precursor resulted in a reaction between the glassy silica and alumina phases during sintering, thereby forming a mullite phase without inhibiting densification. The addition of fine silica powder to the mullite single-phase precursor led to densification with an abnormal grain growth of mullite, whereas some of the added silica remained as a glassy phase after sintering. The resulting mullite ceramics prepared using different powder compositions showed different sintering behaviors, depending on the amount of alumina added. Upon selecting an optimum process and the amount of alumina to be added, the pure mullite ceramics obtained via transient liquid phase sintering exhibited high density (approximately 99%) and excellent high-temperature flexural strength (approximately 320 MPa) at 1500 °C in air. These results clearly demonstrate that pure mullite ceramics fabricated via transient liquid phase sintering with compositions close to those of stoichiometric mullite could be a promising process for the fabrication of high-temperature structural ceramics used in an ambient atmosphere. The transient liquid phase sintering process proposed in this study could be a powerful processing tool that allows for the preparation of superior high-temperature structural ceramics used in the ambient processing atmosphere.     

Electric field-assisted synthesis/sintering cerium oxide: 5 wt.% gadolinium oxide

Gadolinium oxide ceramic powders were mixed to cerium oxide ceramic powders, pressed to pellets, and sintered either at 1450 °C or applying 200 V cm⁻¹ electric field at 800 °C, 900 °C and 1000 °C. The structural phases and the microstructure of the sintered pellets were analyzed by X-ray diffraction and scanning electron microscopy, respectively. The formation of substitutional solid solution was followed by monitoring the increase of the electrical conductivity by impedance spectroscopy and X-ray diffraction. The main results show that Joule heating due to the flow through the pellets of the electric current, which was produced by the application of the electric field, allows for promoting partial solid solution as well as partial sintering the ceria-gadolinia pellets. Moreover, grain growth that occurred in the high temperature sintered pellets was inhibited in the electric field-assisted synthesized/sintered pellets, being an alternative technique for producing cerium oxide-gadolinium oxide solid solutions.     

CO2 laser post-treatment of sol-gel-derived Y3Al5O12:Ce phosphor ceramic powders

Cerium-doped yttrium aluminum garnet (Y₃Al₅O₁₂:Ce, YAG:Ce) was prepared using a sol-gel method and then fired for CO₂ laser post-treatments. Phase transformations and formation of impurities were not observed in YAG:Ce after CO₂ laser sintering. The shift of the diffraction peak and the appearance of another Raman peak indicate a more homogeneous distribution of Ce activators and enhanced crystallinity in laser-sintered YAG hosts. Larger spheres (100–200 μm) with tiny crystallites (<10 μm) were observed on the smoother surface in the laser-sintered YAG:Ce, unlike the irregular, porous, and layered powders in the sol-gel-derived YAG:Ce (1–100 μm). Photoluminescence (PL) measurements revealed an emission increase of 180% and a red shift of the emission peak for the laser-sintered YAG:Ce powders compared with the sol-gel-derived powders. Both have comparable thermal PL quenching behavior; however, the YAG:Ce powders with CO₂ laser treatment exhibited a PL efficiency improvement of approximately 4%.     

Development and evaluation of TiB2–AlN ceramic composites sintered by spark plasma

Titanium diboride (TiB₂) is a ceramic material with high mechanical resistance, chemical stability, and hardness at high temperatures. Sintering this material requires high temperatures and long sintering times. Non-conventional sintering techniques such as spark plasma sintering (SPS) can densify materials considered difficult to sinter. In this study, TiB₂–AIN (aluminum nitride) composites were sintered by using the SPS technique at different sintering temperatures (1500 °C, 1600 °C, 1700 °C, 1800 °C, and 1900 °C). x-ray diffraction was used to identify the phases in the composites. mechanical properties such as hardness and indentation fracture toughness was obtained using a vickers indenter. Different toughening mechanisms were identified, and good densification results were obtained using shorter times and lower temperatures than those previously reported.     

Facile size-controlled synthesis of well-dispersed spherical amorphous alumina nanoparticles via homogeneous precipitation

Well-dispersed spherical amorphous alumina nanoparticles with a narrow size distribution were obtained by facile homogeneous precipitation and subsequent calcination. In the synthesis, formamide was used as the precipitant, and mixtures of aluminum sulfate and aluminum nitrate with different molar ratios were used as the aluminum sources. The average size of the amorphous alumina nanoparticles was successfully controlled by adjusting the amount of formamide and the sulfate/nitrate molar ratio. The particle size decreased with increasing amount of formamide and decreasing sulfate/nitrate molar ratio. Dispersed spherical amorphous alumina nanoparticles with average sizes of 23, 34, 45, and 57 nm were prepared using 100 mL formamide at sulfate/nitrate molar ratios of 1:9, 2:8, 3:7, and 4:6, respectively.     

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.     

Reaction coupling preparation of high sintering activity boron carbide nano-powders

Large scale B₄C nano-powders were synthesized via a novel ball milling assisted reaction coupling self-propagating high temperature synthesis method using Mg, B₂O₃ and CH₂H₃Cl as the starting materials. The XRD, FTIR, Raman, EDX, FSEM, TEM, HRTEM and SAED were used to characterize the B₄C samples. The optimum endothermic rate was 35%, when the samples presented fine and uniform regular morphology with an average particle diameter of about 100 nm. In addition, the reaction coupling principle, possible chemical reaction mechanism and the effects of the endothermic reaction rate were also discussed. Moreover, the commercial B₄C (C-B₄C) and homemade B₄C (H-B₄C) ceramics were prepared by spark-plasma sintering method at 1700 °C under 30 Mpa. Compared with the C-B₄C ceramic, the values of relative density, vickers hardness and fracture toughness of the H-B₄C ceramic were increased by 2.1%, 9.2% and 20.1%, respectively, demonstrating high sintering activity of the homemade B₄C nano-powders.