Effect of focused ion beam sample preparation on the phase composition of zirconia

The investigation of phase transformations in metastable ceramic systems such as zirconia often requires local phase analysis within the areas of interest. Electron backscatter diffraction is a suitable method in combination with focused ion beam sample preparation. The interaction between ion beam and sample has to be carefully considered. In case of metastable Y-PSZ and Mg-PSZ, phase transformations were observed after FIB preparation with 30?kV, 30?nA and 5° incidence angle. Damage was the dominating effect for angles of 72°. The expected local temperature increase due to the ion bombardment with 30?kV and 30?nA is 700?K for ZrO₂. Thus, the observed phase transformations can be explained on the basis of the temperature increase in the corresponding Y-PSZ phase diagram. In case of Mg-PSZ, the transition temperature is 1083?°C. The local temperature increase was obviously lower. The excitation energy for the observed phase transformation was smaller than expected from the phase diagrams of the thermodynamic equilibrium. Using 5?kV, 4.8?nA and 5° incidence angle, no phase transformations and no damage were observed. Thus, these conditions are well suited for the FIB preparation of metastable zirconia.     

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.     

Microstructure and microwave dielectric properties of Al2O3 added Li2ZnTi3O8 ceramics

Recently, the rapid development of advanced communication systems increasingly strongly demands high-performance microwave dielectric ceramics in microwave circuits. Among them, Li₂ZnTi₃O₈ ceramics have been one of the most widely investigated species, due to its high quality factor, moderate firing conditions and low cost. However, the dielectric constants of the already reported Li₂ZnTi₃O₈ ceramics are fixed in a narrow range, limiting their wider applications. To adjust the dielectric constant of the Li₂ZnTi₃O₈ based ceramics, in this work Li₂ZnTi₃O₈ ceramics added with different amounts of Al₂O₃ (0–8?wt%) were prepared by conventional solid-state reaction. The microstructure and microwave dielectric properties of the samples were investigated. Due to the addition of Al₂O₃, the sintering temperature of the ceramics would be increased somewhat. Some Al³⁺ ions could substitute for Ti⁴⁺ ions in Li₂ZnTi₃O₈, and the added Al₂O₃ would react with ZnO to produce a ZnAl₂O₄ phase accompanying with the formation of TiO₂ phase, which would inhibit the growth of Li₂ZnTi₃O₈ grains. The dielectric constant of the finally obtained ceramics would be reduced from 26.2 to 17.9, although the quality factors of the obtained ceramics would decrease somewhat and the temperature coefficient of resonant frequency would deviate further from zero.     

Growth,microstructure, energy–storage and dielectric performances of chemical–solution NBT–based thin films: Effect of sodium nonstoichimometry

Na_0.5+δBi_0.5(Ti_0.96W_0.01Ni_0.03)O₃ thin films with various Na contents (abbreviated as Na_.5+δBTWN, δ?=?? 3.0, ??1.5, 0, 1.5%) were fabricated on ITO/glass substrates using a chemical–solution process. The effects of Na nonstoichiometry on the microstructure, insulating, ferroelectric and dielectric performances are investigated. The pure perovskite phase can be obtained in Na_0.5BTWN and Na_0.515BTWN, while for Na_0.470BTWN or Na_0.485BTWN, the main composition contains secondary phase of TiO₂. The grain size increases from 30?nm at δ?=?? 3.0% to 55?nm at δ?=?0%, then decreases to 52?nm with δ?=?1.5%. The leakage current of Na_0.485BTWN sample is reduced dramatically in comparison with Na_0.5+δBTWN (δ?=?? 3.0, 0, 1.5%). The big recoverable energy–storage density of 63.1?J/cm² and high energy–storage efficiency of 55.0% can be obtained for Na_0.485BTWN due to the improved electric break–down strength and large difference value between the remanent polarization and maximum polarization. Enhanced dielectricity is achieved in Na_0.485BTWN with a high tunability of 36.0% and a figure of merit of 4.0 at 450?kV/cm and 500?kHz. These results demonstrated that the crystallization, micrographs and energy storage and dielectric properties of Na_0.5Bi_0.5TiO₃ are highly sensitive to low levels of Na–site nonstoichiometry.     

Corrosion resistance of silicon-infiltrated silicon carbide (SiSiC)

Silicon carbide ceramics have found widespread use due to their high corrosion stability. Both solid state-sintered silicon carbide, which has an extremely high corrosion resistance, and silicon-infiltrated silicon carbide are used for various applications. The latter material contains SiC as well as free silicon, which is less stable. Hence, in the present work, the corrosion behavior of silicon-infiltrated silicon carbide ceramics was investigated in NaOH solutions. Long-term corrosion experiments were conducted, and a method for analyzing the corrosion behavior in short-term experiments was developed. The short-term method is based on the accurate measurement of the corrosion depth by laser scanning microscopy on polished surfaces. The results of both methods were in good agreement. The advantage of the short-term method is that it provides information on changes in corrosion mechanisms and corrosion rates in the initial period and as a function of the impurities present. Preferential corrosion of Si at the interface to SiC was observed. TEM investigations revealed that this enhanced corrosion was caused by the segregation of impurities.     

Characterization of biogenic hydroxyapatite derived from animal bones for biomedical applications

In this work, the viability of producing biogenic hydroxyapatite from bio-waste animal bones, namely bovine (cow), caprine (goat) and galline (chicken), through a heat treatment process has been investigated. The animal bones were locally sourced, cleaned to remove collagen and subsequently heat treated in air atmosphere at different temperatures ranging from 600?°C to 1000?°C. From the range of sintering temperatures investigated, it was found that hydroxyapatite derived from bovine bone showed good thermal stability while those produced from caprine and galline bones exhibited phase instability with traces of tri-calcium phosphate (TCP) being detected after heat treatment beyond 700?°C. The porous nature of the bone samples can be observed from the microstructures obtained and supported by low relative density. Heating the bovine and caprine bones at selected temperatures yielded porous HA body, having hardness values that are comparable with human cortical bone. However, the sintered galline bone sample showed higher porosity levels and low hardness when compared to the other two bone types.     

Strength of pure alumina ceramics above 1 GPa

Up to now, commercially available alumina ceramics were claimed to have strength between 400 and 550 MPa. However, our study shows strength ~ 2 times higher for commercially available alumina than commonly believed. The average and characteristic strength, measured on 31 pure alumina ceramic discs by ball on three balls (B3B) test, were 1205 ± 93 MPa and 1257 MPa, respectively, with a Weibull modulus of m = 11.8. Tested specimens were in form of discs with a diameter of 5 mm and thickness 0.5 mm. The grain size distribution of the alumina is bimodal with an average grain size of ~ 850 nm measured at the surface. The fracture reveals a mixed transgranular / intergranular failure mode. To avoid incorporation of additional flaws, the discs were tested as sintered. The characteristic flexural strength measured in B3B was recalculated according to Weibull theory for standard 4-point bending bars of size 3 × 4 × 45 mm as bend 856 MPa. The measured strength of nearly 900 MPa shows the potential of strength for high purity alumina ceramics.     

Infiltration behavior of Cu and Ti fillers into Ti2AlC/Ti3AlC2 composites during tungsten inert gas (TIG)brazing

Herein we study the infiltration behavior of Ti and Cu fillers into a Ti₂AlC/Ti₃AlC₂MAX phase composites using a TIG-brazing process. The microstructures of the interfaces were investigated by scanning electron microscopy and energy dispersive spectrometry. When Ti₂AlC/Ti₃AlC₂ comes into contact with molten Ti, it starts decomposing into TiC_x, a Ti-richandTi₃AlC; when in contact with molten Cu, the resulting phases are Ti₂Al(Cu)C, Cu(Al), AlCu₂Ti and TiC. In the presence of Cu at approximately 1630 °C, a defective Ti₂Al(Cu)C phase was formed having a P63/mmc structure. Ti₃AlC₂ MAX phase was completely decomposed in presence of Cu or Ti filler-materials. The decomposition of Ti₂AlC to Ti₃AlC₂ was observed in the heat-affected zone of the composite. Notably, no cracks were observed during TIG-brazing of Ti₂AlC/Ti₃AlC₂ composite with Ti or Cu filler materials.     

Synthesis and characterization of calcium aluminate compounds from gehlenite by high-temperature solid-state reaction

The mineral transition mechanism and self-pulverization property of the sintered products in the Ca₂Al₂SiO₇-CaO system were systematically studied using pre-synthesized gehlenite determined by XRD, SEM, FTIR and particle size analyses. The minerals of Ca₁₂Al₁₄O₃₃, CaAl₂O₄, Ca₃SiO₅ and Ca₂SiO₄ are formed by the direct reactions of Ca₂Al₂SiO₇ with CaO. CaAl₂O₄ reacts with CaO to form Ca₁₂Al₁₄O₃₃ or Ca₃Al₂O₆, while Ca₃SiO₅ reacts with Ca₂Al₂SiO₇ to form Ca₂SiO₄ and calcium aluminate compounds. The sintered products mainly contain CaAl₂O₄, Ca₁₂Al₁₄O₃₃ and Ca₂SiO₄ at 1350?°C or above 1500?°C when the molar ratio of CaO to Al₂O₃ is 1.0. Increasing the sintering duration or the CaO consumption promotes the transition of Ca₂Al₂SiO₇ to Ca₂SiO₄ and calcium aluminate compounds when sintered at 1350?°C, which accordingly improves the self-pulverization property of the sintered products. The formed minerals of Ca₁₂Al₁₄O₃₃, CaAl₂O₄ and Ca₂SiO₄ transform into Ca₂Al₂SiO₇ again when the sintering temperature is between 1400?°C and 1450?°C, and the corresponding self-pulverization property of the sintered products deteriorates sharply.     

Preparation of in situ grown silicon carbide whiskers onto graphite for application in Al2O3-C refractories

C-SiC composite powders were prepared by salt-assisted synthesis from Si powders, graphite, and a molten salt medium (NaCl and NaF) with the molar ratio of Si/C =?1/2 at 1300?°C for 3?h. After the C-SiC composite powders part and complete replacement of the graphite, the mechanical properties, oxidation resistance and slag-corrosion resistance of the Al₂O₃-C materials were studied by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS), as well as with dedicated equipment. The results indicated that SiC whiskers, with lengths of 10–50?nm, formed on the surface of the flake graphite, and the activation energy of oxidation of the C-SiC composite powder increased by 45.72?kJ?mol^?1 as compared to that of flake graphite. Furthermore, the decarburization area and slag erosion area of the Al₂O₃-C material decreased after 3?wt% of C-SiC composite powder was substituted for the flake graphite. Meanwhile, the cold modulus of rupture was maintained when 3?wt% of C-SiC composite powder was added. This improved both the oxidation and slag resistance of the Al₂O₃-C materials.