G Processing and characterization of CaTiO 3 perovskite ceramics
Calcium titanate (CaTiO3) ceramics with perovskite structure were produced by solid state reaction. Calcium carbonate (CaCO3) and titanium dioxide (TiO2) were mixed (in molar ratios 1/1 and 3/2), and the obtained mixtures were calcined at 1150 °C in successive thermal cycles. The obtained samples were characterized by differential thermal analysis, thermogravimetry, X-ray diffraction, measurement of particle size distribution and linear thermal shrinkage. XRD results indicated that the samples have perovskite CaTiO3 structure with small amount of secondary CaO and TiO2 phases, and their phase composition depends on the heat treatment conditions. The measured values of electrical resistivity were within the characteristic range of insulating materials and approach values corresponding to semiconducting ceramics.
Grain growth in CaTiO3-perovskite + FeO-wüstite aggregates
Abstract Grain growth kinetics in CaTiO3-perovskite + FeO-wüstite aggregates were studied at the conditions of T = 1223–1623 K, P = 0.1 MPa and P = 200 MPa. Starting samples were fabricated by hot-pressing mechanically mixed powders of CaTiO3 + FeO with FeO = 0%, 1%, 3%, 6%, 10%, 20% and 100% by weight in a gas-medium apparatus at 1323 K and 300 MPa for 5 h. The increase of grain size (G) of CaTiO3 with time (t) follows a growth law: Gn−Gn0 = κ·t(κ=κ0exp(−(Q/RT)). Two grain growth regimes are observed at T < 1523 K and T ≥ 1523 K. For T < 1523 K, the best fits of the data to the growth law yield growth exponents of n = 2.2 ± 0.2, 3.0 ± 0.3 and 3.5 ± 0.3 for samples with FeO = 0%, 3% and 10% respectively. Under these conditions the rate constants, κ, obey an Arrhenius relation with Q = 206 ± 35 kJ/mol and 385 ± 65 kJ/mol for samples with FeO = 3% and 10%. Grain growth of CaTiO3 becomes sluggish when FeO content exceeds 6%. For T ≥ 1523 K, the best fits of the data to the growth law yield n = 2.5 ± 0.2 for both samples with FeO = 3% and 10%. The activation energies (Q ) were determined as 71 ± 30 kJ/mol and 229 ± 45 kJ/mol for samples with FeO = 3% and 10%, respectively. The TEM observations show a remarkable difference in the distribution and geometry of FeO below and above 1523 K: nanometer-sized particles of FeO were observed along CaTiO3 grain boundaries in samples annealed at T < 1523 K. No FeO particles were detected along CaTiO3 grain boundaries in samples annealed at T ≥ 1523 K, but large clusters of FeO particles are observed locally indicating a fast separation of FeO from CaTiO3. Thus we conclude that the slow growth rate of CaTiO3 at T < 1523 K is due to the pinning by FeO particles at grain boundary, and that the change of grain growth kinetics in CaTiO3 at T ≥ 1523 K may relate to the separation of FeO from CaTiO3, which we interpret as due to the phase transformation of CaTiO3 at around 1523 K.
Prevention of Barite Sag in Oil-Based Drilling Fluids Using a Mixture of Barite and Ilmenite as Weighting Material
Drilling high-pressure high-temperature (HPHT) wells requires a special fluid formulation that is capable of controlling the high pressure and is stable under the high downhole temperature. Barite-weighted fluids are common for such purpose because of the good properties of barite, its low cost, and its availability. However, solids settlement is a major problem encountered with this type of fluids, especially at elevated downhole temperatures. This phenomenon is known as barite sag, and it is encountered in vertical and directional wells under static or dynamic conditions leading to serious well control issues. This study aims to evaluate the use of barite-ilmenite mixture as a weighting agent to prevent solids sag in oil-based muds at elevated temperatures. Sag test was conducted under static conditions (vertical and inclined) at 350 °F and under dynamic conditions at 120 °F to determine the optimum ilmenite concentration. Afterward, a complete evaluation of the drilling fluid was performed by monitoring density, electrical stability, rheological and viscoelastic properties, and filtration performance to study the impact of adding ilmenite on drilling fluid performance. The results of this study showed that adding ilmenite reduces sag tendency, and only 40 wt.% ilmenite (from the total weighting material) was adequate to eliminate barite sag under both static and dynamic conditions with a sag factor of around 0.51. Adding ilmenite enhanced the rheological and viscoelastic properties and the suspension of solid particles in the drilling fluid, which confirmed sag test results. Adding ilmenite slightly increased the density of the drilling fluid, with a slight decrease in the electrical stability within the acceptable range of field applications. Moreover, a minor improvement in the filtration performance of the drilling fluid and filter cake sealing properties was observed with the combined weighting agent. The findings of this study provide a practical solution to the barite sag issue in oil-based fluids using a combination of barite and ilmenite powder as a weighting agent to drill HPHT oil and gas wells safely and efficiently with such type of fluids.