Effect of an abrupt change in pulling rate on microstructures of directionally solidified Al2O3-Er3Al5O12 eutectic and off-eutectic composite ceramics

Directionally solidified microstructures of Al₂O₃-Er₃Al₅O₁₂ eutectic and off-eutectic in situ composite ceramics were explored under abrupt-change pulling rate conditions. Corresponding temperature distributions and interface locations were studied. In eutectic composition, fluctuation of eutectic spacing occurred when the pulling rate increased abruptly. A gradually increase or abrupt increase in eutectic spacing was observed when the pulling rate decreased abruptly. In hypoeutectic and hypereutectic compositions, formation of the primary phases were suppressed when the pulling rate increased abruptly from 10?µm/s to 100?µm/s, while primary phases precipitated when the pulling rate decreased abruptly from 100?µm/s to 10?µm/s. The interface altitude decreased after the pulling rate increased abruptly, but increased after the pulling rate decreased abruptly. The liquid composition restriction (around the eutectic composition) at the eutectic interface plays an important role in the suppression of the primary dendrite and coupled eutectic oxides can be obtained in off-eutectic compositions even under higher solidification rate conditions.     

Development and monitoring of an integrated bioprocess for production of a potential malaria vaccine with Pichia pastoris

An engineered variant of the yeast Pichia pastoris was used to produce the potential malaria vaccine D1M1. This paper describes the implementation of an expanded bed adsorption chromatography step into a sequential cultivation process of the yeast in order to link protein expression, cell release, and product capture of the secreted protein in a fully automated plant. The process is operated with a semi-continuous strategy for an integrated production. Process improvements have been achieved using design of experiments. Resulting purities of product achieved up to 87% with recoveries of 51% in a single downstream operation. Furthermore, a multivariate analysis of historical batch data was used to develop a golden batch model for process monitoring.     

Hierarchical micro-nanostructured albite-based glass-ceramic for high dielectric strength insulators

A novel glass-ceramic material based on albite type Na-rich feldspar has been synthesized by conventional ceramic process. High crystallinity, >94%?Vol.% is obtained by fast sintering which allows energy saving processing. Albite is the main crystalline phase and tetragonal SiO₂ is a secondary phase. Electrical properties were examined by complex impedance, DC measurements, and dielectric breakdown test. Dielectric characterization shows a non-Debye type dielectric behavior with low dielectric constant, 4.6 at 1?MHz, low dielectric losses, (～10^?3 at 1?MHz, and a large dielectric strength, ～60?kV/mm), that it is the largest value reported in ceramic insulators. Those dielectric properties are attained by the low glassy phase content in the samples and their unique micro-nanostructure. All these properties make this novel material a very promising candidate in the market of ceramic electrical insulator, highlighting for high-voltage applications.     

Effects of SiC content on the densification,microstructure, and mechanical properties of HfB2–SiC composites

To investigate the effects of SiC on microstructure, hardness, and fracture toughness, 0, 10, 20, and 30 vol% SiC were added to HfB₂ and sintered by SPS. Upon adding SiC to 30 vol%, relative density increased about 4%; but HfB₂ grain growth had a minimum at 20 vol% SiC. This may be due to grain boundary silicate glass, responsible for surface oxide wash out, enriched in SiO₂ with higher fraction of SiC. By SiO₂ enrichment, the glass viscosity increased and higher HfO₂ remained unsolved which subsequently lead to higher grain growth. Hardness has increased from about 13 to 15 GPa by SiC introduction with no sensible variation with SiC increase. Residual stress measurements by Rietveld method indicated high levels of tensile residual stresses in the HfB₂ Matrix. Despite the peak residual stress value at 20 vol% SiC, fracture toughness of this sample was the highest (6.43 MPa m^0.5) which implied that fracture toughness is mainly a grain size function. Tracking crack trajectory showed a mainly trans-granular fracture, but grain boundaries imposed a partial deflection on the crack pathway. SiC had a higher percentage in fracture surface images than the cross-section which implied a weak crack deflection.     

Effects of hydrolysis of precursor on the structures and properties of polymer-derived SiBN ceramic fibers

In this paper, polyborosilazane precursor was synthesied from HMDZ, HSiCl₃, BCl₃ and CH₃NH₂ using a multistep method. By controlling the storage conditions, parts of the polyborosilazane fibers were hydrolyzed. FT-IR, NMR, XRD, TEM and monofilament tensile strength test were employed to study the effects of hydrolysis of precursor on the structures and properties of polymer-derived SiBN ceramic fibers. FT-IR and NMR results indicate that Si-N group in PBSZ reacts with H₂O to form Si-O-Si group. After pyrolysis reaction at 1400℃, Si-O-Si group will finally transformed into highly ordered cristobalite and β-quartz, resulting in formation of the wrinkled surface of the obtained SiBN ceramic fiber. The strip-like defects on fiber surface, according to monofilament tensile strength test, had a significant effect on mechanical property of the obtained SiBN ceramic fiber and caused no increase in fiber tensile strength of hydrolytic polyborosilazane fiber before and after pyrolytic process.     

Microwave dielectric properties of ultra-low loss Li2MgTi0.7(Mg1/3Nb2/3)0.3O4 ceramics sintered at low temperature by LiF addition

In this work, ultra-low loss Li₂MgTi_0.7(Mg_1/3Nb_2/3)_0.3O₄ ceramics were successfully prepared via the conventional solid-state method. X-ray photoelectron spectroscopy (XPS), thermally stimulated depolarization current (TSDC) and bond energy were used to determine the distinction between intrinsic and extrinsic dielectric loss in (Mg_1/3Nb_2/3)⁴⁺ ions substituted ceramics. The addition of (Mg_1/3Nb_2/3)⁴⁺ ions enhances the bond energy in unit cell without changing the crystal structure of Li₂MgTiO₄, which results in high Q·f value as an intrinsic factor. The extrinsic factors such as porosity and grain size influence the dielectric loss at lower sintering temperature, while the oxygen vacancies play dominant role when the ceramics densified at 1400?°C. The Li₂MgTi_0.7(Mg_1/3Nb_2/3)_0.3O₄ ceramics sintered at 1400?°C can achieve an excellent combination of microwave dielectric properties: ε_r =?16.19, Q·f?=?160,000?GHz and τ_f =??3.14?ppm/°C. In addition, a certain amount of LiF can effectively lower the sintering temperature of the matrix, and the Li₂MgTi_0.7(Mg_1/3Nb_2/3)_0.3O₄-3?wt% LiF ceramics sintered at 1100?°C possess balanced properties with ε_r?=?16.32, Q·f?=?145,384?GHz and τ_f =??16.33?ppm/°C.     

Growth behavior of aluminum borate whiskers on zirconia toughened alumina (ZTA) particle surface

In this work, B₄C-covered zirconia-toughened alumina (ZTA) particles are prepared and oxidised at 1050 °C for different times (0, 2, 4, and 8 h) in air. The X-ray diffraction and electron probe micro-analysis results show that the covering layer is mainly composed of oxide B₂O₃ intermetallics, residual B₄C particles, and Al₁₈B₄O₃₃ whiskers. The scanning electron microscopy results show that the growth of Al₁₈B₄O₃₃ whiskers on the ZTA particles enhances with increasing heat preservation time; the optimum holding time is determined to be 8 h Al₂O₃ in the ZTA particles diffuse into the covering layer and combine with B₂O₃ to form Al₁₈B₄O₃₃ whiskers; the Al₁₈B₄O₃₃ whiskers grow via the liquid-solid mechanism.