Stabilization of tetragonal phase of nanostructured Fex/ZrO2 system (0 ≤ x ≤ 25) prepared by modified sol-gel method

In the present study, Fex/ZrO2 (0 ≤ x ≤ 25) nanoparticles were synthesized by a facile modified Sol-Gel method. Stabilization of the tetragonal phase of ZrO2 is studied as a function of both the Fe incorporation ratios and thermal treatment. The Fe incorporation ratios are tested up to the extreme just before FeO and Fe2O3 phases are formed separately. The prepared Fex/ZrO2 nanoparticles XRD analysis depicts the formation of zirconium oxide at different Fe ratios in the nanoscale with an excellent degree of crystallinity in the tetragonal phase. The effect of thermal treatment on stabilizing the tetragonal phase of Fex/ZrO2 nanoparticles is extensively studied. The phase transition to the monoclinic phase is determined as function of Fe incorporation ratios and annealing temperatures. The optical absorbance spectra showed that the optical band gap decreased with increasing Fe ratios without the formation of doping bands which confirms the formation of Fex/ZrO2 single matrix.

Recognition of kinetic transient process in corrosion scales of fuel elements by impedance spectroscopy

The presented study concerns with the corrosion kinetics of two zirconium alloys: Zr-Nb-Sn-Fe and Zr-Nb-Fe. Alloy samples were pre-exposed at 360 °C in a LiOH solution containing 70 mg/l of lithium ions. Ex-situ electrochemical impedance spectroscopy (EIS) performed in 0.5 M potassium sulphate solution at 25 °C was used to study the properties of the oxide and kinetic transient effect. Evaluation of the impedance spectroscopy data was based on application of a simple equivalent circuit. The setup of the equivalent circuit conformed to Jonscher´s universal law of dielectric response. The analysis of the impedance data was aimed at estimation of non-dispersive capacitance of the oxide formed during the pre-exposure. Effective values of dielectric constant were calculated using the non-dispersive capacitance and the oxide thickness values, calculated from weight gains. For the pre-transient samples relatively higher values of dielectric constants were obtained. Typical pre-transient dielectric constants for Zr-Nb-Sn-Fe alloy ranged between 20–21, while slightly lower values were obtained for Zr-Nb-Fe alloy. In both alloys steep and significant decrease in effective dielectric constant (e_ef = 9–13) was found for the transient samples. The decrease correlated very well with the drop in percentage of tetragonal oxide determined by Raman spectroscopy and corresponded to the increase of the weight gains of the transient samples. Literature data indicate values of dielectric constants for tetragonal zirconium oxide between 38–46, while those for monoclinic oxide are usually presented between 12–22. The evidenced changes in dielectric constants are therefore in agreement with the expected decrease of tetragonal phase fraction in the oxide layer during the transient. In the Zr-Nb-Sn-Fe post-transient samples values of dielectric constant increased again to 18–20, therefore almost to the pre-transient level. This increase was not evidenced with Raman spectroscopy data, which show constant low content of the tetragonal fraction. Possible explanation of this disagreement is the location of the newly formed post-transient tetragonal oxide presumably at the metal/oxide interface. Oxide thickness of the post-transi-ent samples is 4–7 m and the oxide/metal interface is beyond access of the laser beam of Raman spectrometer. We can conclude that using ex-situ EIS, the transient was observable in both alloys; the change in the ratio of monoclinic and tetragonal phase can be evaluated based on the difference of effective dielectric constant of the two phases. The Zr-Nb-Sn-Fe alloy showed the onset of the transient after the 105th day of pre-exposure, but the change in the ratio of the monoclinic and tetragonal phases was less significant than in the Zr-Nb-Fe alloy, in which, however, the transient could be observed only after 147 days of pre-exposure. The resulting values of the effective dielectric constant of oxides correlated well with the percentage of tetragonal oxide determined by Raman spectroscopy and with the results of the weight gain method.

Effect of Variation MWCNTs in Synthesis Zirconia Prepared by Uniaxial Pressed Technique

The effect of addition different weight percentage (wt. %) of treated MWCNTs on zirconia matrix as a composite structure using method uniaxial pressed for fabrication and enhancement mechanical, microstructural properties of zirconia have been investigated in the present study. The composite material have prepared by adding yttrium oxide (3% mol. Y2O3) to zirconia for stabilized in the tetragonal phase with homogeneous distribute and reinforcement changed weight percentage of (2%, 5%, 7%, and 10%) wt. of F-MWCNTs to result (3% mol.Y2O3-ZrO2/F-MWCNTs) nanocomposite samples by pressing uniaxiall at pressure of (624) MPs in the metal-die cylinder to results pellets of (10 mm diameter). The resulting pellets were sintered in air at (1550 °C) temperatures for two hours. The samples were characterized by XRD analysis to demonstrate the phase composition of samples, where The retention was observed on the tetragonal phase in zirconia and the microstructure of the materials have been studied using SEM it is observed that F-MWCNTs were homogeneously distributed in the composite powders without the formation of ropes and bundles up to the highest contents of F-MWCNTs, and EDS showed the percentages for presence of carbon in samples, The micro hardness was studied by Vickers indentation method and Brazilian test that shows improved due to a homogeneous distribution of MWCNT in ZrO2 and the densities (Green, Bulk, and theoretical), porosity and liner shrinkage to demonstrate the toughness that reveal many pores and low densification with increasing F-MWCNTs contents, physical and mechanical properties of samples depend on distribution of F-MWCNTs in the matrix.

Low-temperature degradation resistance and plastic deformation of ATZ ceramics stabilized by CaO

In this work, the phase composition (relative fractions of monoclinic m-ZrO2, tetragonal t-ZrO2, and cubic c-ZrO2 phases) and mechanical properties (hardness, fracture toughness, compressive strength) of alumina toughened zirconia (ATZ) ceramics, with an addition of silica were investigated. Calcium oxide was used as a stabilizer for the zirconia tetragonal phase. It was shown that CaO-ATZ+SiO2 ceramics demonstrate increased resistance to low-temperature degradation. The plasticity signs at room temperature were found due to the SiO2 addition to CaO-ATZ ceramics. A yield plateau appears in the uniaxial compression diagram at 5 mol. % SiO2 concentration. It is hypothesized that discovered plasticity is due to the increased t→m transformability.

Electrocaloric Effect of (K1−xNax)NbO3 Single Crystal

The electrocaloric effect of (K1−xNax)NbO3 single crystal is calculated based on Landau-Devonshire theory. The electrocaloric coefficient and adiabatic temperature change are calculated with the variation of temperature in rhombohedral, orthorhombic and tetragonal phase. A maximum of electrocaloric coefficient is obtained in each ferroelectric phase. Moreover, the tetragonal phase presents the larger electrocaloric coefficient and adiabatic temperature change than that rhombohedral and orthorhombic phase. However, the large electrocaloric effect is also obtained at room temperature with the adiabatic temperature change of 0.5 K, which tallies with the experimental findings.

Experimental and Simulation Analysis of the Evolution of Residual Stress Due to Expansion via CMAS Infiltration in Thermal Barrier Coatings

The failure behavior of thermal barrier coatings (TBCs) involves multilayered systems infiltrated with calcium–magnesium–alumino-silicates (CMAS). The metastable tetragonal phase is mainly composed of 7YSZ (7 mol.% Y2O3-stabilized ZrO2), and it destabilizes into the Y-lean tetragonal phase, which may be induced by CMAS infiltration, and transforms into a monoclinic phase during cooling. The phase transformation leads to volume expansion around the CMAS-rich layer. Furthermore, it is shown that the spalling of the coating system emerges when the surface of the coating system is subjected to significant residual stress. In this study, a double-cantilever beam model is established to describe the macroscopic phenomenon of thermal buckling induced via CMAS. The result of the buckle height is used to demonstrate the consistency of the experiment and finite element simulation. The experimental parameters are imported into a multilayer cantilever beam model to analyze the interfacial stresses due to CMAS infiltration. The finite element results indicate that the phase transformation leads to damage in the coating system wherein the interfacial stresses due to phase transformation are 27% higher than those in the model without phase transformation.