Highly textured and strongly anisotropic TiB2 ceramics prepared using magnetic field alignment (9T)

Highly textured TiB₂ ceramics were prepared by slip casting an aqueous suspension in a magnetic field of 9 T, followed by sintering using Field Assisted Sintering Technology (FAST). Particle size refinement by ball milling improved both the degree of texturing and densification of the material (RD > 98 %). The sintered material exhibited a Lotgering orientation factor of 0.90, with the c-axis of TiB₂ oriented parallel to the magnetic field and FAST pressing direction. The texturing effect induced by the uniaxial pressing was negligible. The textured TiB₂ material exhibited a significant anisotropy in mechanical properties; the values of hardness and indentation elastic modulus measured along directions transverse to the c-axis of TiB₂ were 37 % and 13 % higher than the ones measured along the c-axis direction. Moreover, the specific wear rate of a surface of textured TiB₂ parallel to the field was one order of magnitude lower than a surface perpendicular to the field.     

Synthesis,microstructure and electromechanical properties of undoped (K0·5Na0·5)NbO3

Conventional solid state mixed oxide route using manual and ball milling is investigated for the preparation of K_0·5Na_0·5NbO₃ (KNN) ceramics. Microstructure engineering was made using two milling methods and sintering techniques, and the crystal growth; then electromechanical properties were investigated as a function of sintering temperature, densification and grain size. The sintering conditions were set at 920°C/5 min for spark plasma sintering and 1090–1120°C/10 and 48 h for classical sintering. KNN crystal was grown using floating zone technique under nitrogen gas, where the translation and rotation speeds were fixed at 3 mm h^?1 and 20 rev min^?1 respectively. Piezoelectric and dielectric performances were measured and related to the microstructure. High k_t (33 to 48%), k_p of 18 to 48% and d₃₃ of 127–140 pC N^?1 were reached for relative densities of 84 to 96%. KNN ceramics are now available for the design of ultrasonic sensors.     

Mullitization kinetics from kaolinite incorporating nanometric Ba and Ca fluorides

The work presents the kinetic effect of nanometric BaF₂ and CaF₂ particles on kaolinite to mullite transformation. The kinetics were evaluated from dilatometric data using two different non-isothermal procedures: conversional model-fitting method and diffusional sintering analysis. From experimental data, the activation energy of mullite formation calculated from sintering (942 kJ/mol) and from conversional method (910 kJ/mol) were in good agreement with those values reported by other authors (mean value 1030 kJ/mol). After incorporation of 3 mol% of nanometric BaF₂ and CaF₂ in kaolinite and applying both analytical procedures, lower activation energies for mullite formation were obtained, assigning to the transformation the value of 635 kJ/mol for kaolinite/BaF₂ and 428 kJ/mol for kaolinite/CaF₂ composites.     

Al2O3–CaO macroporous ceramics containing hydrocalumite-like phases

A mechanism to explain the lower onset strengthening temperature induced by CaCO₃ in alumina-based macroporous ceramics is proposed, which relies on hydrocalumite-like phase formation during processing. Close to 600 °C, such phases are decomposed to lime and mayenite (12CaO·7Al₂O₃), where the latter, due to its intrinsic nanoporosity and high thermal reactivity, generates bonds between the ceramic particles at ∼700 °C, resulting in microstructure strengthening. Based on this premise, the authors concluded that other Ca²⁺ sources could act similarly. Indeed, compositions containing Ca(OH)₂ or CaO showed the same effect on the onset strengthening temperature, which reinforces the proposed mechanism. The results attained indicated that macroporous insulators could be thermally treated at lower temperatures, just to acquire enough mechanical strength for installation, finishing in-situ their firing process. Besides that, lower sintering temperatures could be used to produce macroporous ceramics that would be applied in low thermal demand environments, e.g. aluminum industries.     

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.     

Microstructure and mechanical properties of TiC0.7N0.3-HfC cermet tool materials

TiC_0.7N_0.3-HfC cermet tool materials were fabricated by hot-press sintering. Effects of different metal additives (Ni, Co, Ni-Co and Ni-Mo), sintering temperature and holding time on the microstructures and mechanical properties of TiC_0.7N_0.3-HfC cermets were investigated. Results showed that Ni-Mo or Ni-Co as metal additives was better for the mechanical properties of TiC_0.7N_0.3-HfC cermets than only Ni or only Co as the metal additives and Ni-Mo better than Ni-Co. HfC particle dispersion existed in these four cermets and only in the TiC_0.7N_0.3-HfC-Ni-Mo cermet the core-rim structure obviously existed. TiC_0.7N_0.3-HfC-Ni-Mo cermet had significantly smaller grains than the other three cermets because Ni-Mo can significantly refine the grain. With the sintering temperature increasing from 1450?°C to 1650?°C, grains grew gradually; Vickers hardness and flexural strength decreased gradually and the fracture toughness increased firstly and then decreased. With the holding time increasing from 15?min to 60?min, grains grew gradually; Vickers hardness, flexural strength and the fracture toughness increased firstly and then decreased. TiC_0.7N_0.3-HfC-Ni-Mo cermets sintered at 1450?°C with 30?min holding time had the better comprehensive mechanical properties with flexural strength of 1346.41?±?31?MPa, fracture toughness of 8.46?±?0.23?MPa?m^1/2 and Vickers hardness of 22.91?±?0.22?GPa.     

Microstructural evolution and densification behavior of porous kaolin-based mullite ceramic added with MoO3

Microstructural evolution and densification behavior of porous kaolin-based mullite ceramic added with MoO₃ were investigated. The results indicated that MoO₃ addition not only lowered the secondary mullitization temperature to below 950?°C, but also facilitated effectively the anisotropic growth of mullite grains. Fine mullite whiskers grew and interlocked with one another in the pre-existing pore regions, in-situ forming a stiff 3D skeleton structure of mullite whiskers, which arrested further densification of the sample. On the other hand, due to the great capillary attraction of small pores, the liquid phase tended to spread over small grains, which favored the growth from small mullite grains into whiskers at the expense of the liquid phase. Consequently, competitive mechanisms of sintering and crystal growth of mullite functioned, which further limited the sample densification. As a result, the total linear shrinkage of the sample added with MoO₃ after firing at 1400?°C was only ??2.75%, and its porosity was retained at as high as 67%.     

Synthesis and properties of (Hf1-xTax)C solid solution carbides

Thermodynamically stable (Hf_1–xTa_x)C (x?=?0.1–0.3) compositions were selected by First Principle Calculation and synthesized in nanopowders via high-energy ball milling and carbothermal reduction of commercial oxides at 1450?°C. The formation of a solid solution during powder synthesis was investigated. The solid solution carbide powders were sintered at 1900?°C by spark plasma sintering without a sintering aid. As a result, the (Hf_1–xTa_x)C solid solution carbides exhibited high densities, excellent hardness and fracture toughness (ρ: 98.7–100.0%, HVN: 19.69–19.98?GPa, K_IC: 5.09–5.15?MPa?m^1/2) compared with previously reported HfC and HfC–TaC solid solution carbides.     

Hydrogen production through dry reforming of biogas using a porous electrochemical cell: Effects of a cobalt catalyst in the electrode and mixing of air with biogas

This paper reports the performance of porous Gd-doped ceria (GDC) electrochemical cells with Co metal in both electrodes (cell No. 1) and with Ni metal in the cathode and Co metal in the anode (cell No. 2) for CO₂ decomposition, CH₄ decomposition, and the dry reforming reaction of a biogas with CO₂ gas (CH₄ + CO₂ → 2H₂ + 2CO) or with O₂ gas in air (3CH₄ +?1.875CO₂ +?1.314O₂ → 6H₂ +?4.875CO +?0.7515O₂). GDC cell No. 1 produced H₂ gas at formation rates of 0.055 and 0.33?mL-H₂/(min?m²-electrode) per 1?mL-supplied gas/(min?m²-electrode) at 600?°C and 800?°C, respectively, by the reforming of the biogas with CO₂ gas. Similarly, cell No. 2 produced H₂ gas at formation rates of 0.40?mL-H₂/(min?m²) per 1?mL-supplied gas/(min?m²) at 800?°C from a mixture of biogas and CO₂ gas. The dry reforming of a real biogas with CO₂ or O₂ gas at 800?°C proceeded thermodynamically over the Co or Ni metal catalyst in the cathode of the porous GDC cell. Faraday's law controlled the dry reforming rate of the biogas at 600?°C in cell No. 2. This paper also clarifies the influence of carbon deposition, which originates from CH₄ pyrolysis (CH₄ → C + 2H₂) and disproportionation of CO gas (2CO → C + CO₂), on the cell performance during dry reforming. The dry reforming of a biogas with O₂ molecules from air exhibits high durability because of the oxidation of the deposited carbon by supplied air.     

In-situ formation of Al2O3/Al core-shell from waste material: Production of porous composite improved by graphene

Aluminum dross produced from aluminum industry was used to fabricate Al₂O₃/Al porous composites. The dross was milled for 20?h to obtain nano powder. The milled material was examined by TEM and XRD. Graphene (up to 4?wt%) was mixed with the dross and utilized to reinforce sintered composites. The milled powders were compacted then fired at various temperatures up to 700?°C. Physical properties in terms of bulk density and apparent porosity for sintered composites were tested using Archimedes method. SEM attached by energy dispersive spectrometer (EDS) was used to inspect microstructure and elemental analysis of sintered composites. Microhardness and compressive strength were also measured. Ultrasonic nondestructive technique was utilized to examine the elastic moduli. Electrical conductivity of sintered composite was also studied. During milling up to 20?h, Al₂O₃/Al core-shell was in-situ formed with size of 65.9 and 23.8?nm, respectively. The apparent porosity of sintered composites was improved with rising graphene percent while it decreased with increasing sintering temperature. Increasing of graphene mass percent and firing temperature led to remarkable increase in all mechanical properties and electrical conductivity. The maximum compressive strength, hardness, elastic modulus and electrical conductivity were 200?MPa, 1200?MPa, 215?GPa and 1.42?×?10^?5 S/m, respectively, obtained for composite sintered at 700?°C having 4?wt% graphene.