Improvement of anti-corrosive properties of epoxy-coated AA 2024-T3 with TiO2 nanocontainers loaded with 8-hydroxyquinoline

Epoxy coatings containing TiO₂ nanocontainers were applied on aluminium alloy (AA) 2024-T3 for corrosion protection. The nanocontainers were loaded with the corrosion inhibitor 8-hydroxyquinoline (8-HQ). Epoxy coatings were deposited via the dip-coating process. The morphology of the coatings was examined by scanning electron microscopy (SEM). The composition of the films was determined by energy dispersive X-ray analysis (EDX). Electrochemical impedance spectroscopy (EIS) was employed for the characterization of the corrosion resistance of these coatings. The total impedance values were measured as a function of time exposure in corrosive environment. We observed a continuous increase of the total impedance value with the time of exposure suggesting a possible self-healing effect due to the release of the inhibitors from the nanocontainers. Furthermore, addition of loaded nanocontainers into the coatings leads to the enhancement of the barrier properties of the coatings. Conclusively, we observed an improvement of the performance of the coatings due to the loaded nanocontainers.     

Electrochemical and morphological assessments of inhibition level of 8-hydroxylquinoline for AA2024-T4 alloy in 3.5% NaCl solution

The corrosion inhibition of AA2024-T4 in 3.5% NaCl solution by 8-hydroxylquinoline (8-HQ) was investigated by potentiodynamic polarisation (PDP), electrochemical impedance spectroscopy and dynamic electrochemical impedance spectroscopy. Experimental results were supported with scanning electron microscopy (SEM), atomic force microscopy and Fourier transform-infrared (FTIR) spectroscopy analysis. It was found that 8-HQ molecules adsorbed on the alloy surface and protected it against corrosion. SEM, energy dispersive spectroscopy, and FTIR results confirm the adsorption of 8-HQ molecules on AA2024-T4. The inhibition efficiency of 8-HQ is found to increase with increase in concentration and the highest concentration studied (0.05 M) offered corrosion inhibition efficiency of 84%. PDP results show that 8-HQ acts as mixed type inhibitor in the studied medium.     

Sol–gel based layer-by-layer deposits of lanthanum cerium molybdate nanocontainers and their anticorrosive attributes

The present study focuses on the synthesis of novel lanthanum cerium molybdate (LCM) nanoparticles by sol–gel synthesis method and their use in the development of nanocontainers in an anticorrosive coating application. The obtained nanoparticles were used as core material with two different polyelectrolytic shells comprising of polypyrrole (PPY) and polyacrylic acid (PAA) or polyethyleneimine (PEI) and polystyrene sulfonate (PSS) involving the entrapment of benzotriazole (BTA) as the corrosion inhibitor using layer-by-layer (LBL) deposition method. At each step of this nanocontainer synthesis, the thickness of the layers, surface charges and the presence of the functional groups were determined by particle size, zeta potential and Fourier transform infrared spectroscopy (FTIR) analysis, respectively. The X-ray diffractograms (XRD) indicated the change in the crystallinity of the nanoparticles and nanocontainers while thermogravimetric analysis (TGA) showed the thermal degradation behavior of the nanocontainers. The morphological studies conducted using scanning electron microscopy (SEM) exhibited the formation of nanocontainers containing nanoparticles in their cores. The release of BTA from the nanocontainers was evaluated at different pH values. The anticorrosive performance of the nanocontainers was examined by incorporation of the nanoparticles and nanocontainers in a commercial epoxy coating system and to be applied on mild steel and magnesium panels by electrochemical corrosion analysis. Tafel plots demonstrated the decrease in the current density with an increase in the loading percentage of nanocontainers in the epoxy system while Bode plots confirmed the significant improvement in the corrosion protection of the mild steel and magnesium by LCM nanoparticles and nanocontainers.

     

Sintering of Spherical Glass Powder under a Uniaxial Stress

The sintering of spherical borosilicate glass powder (particle size 5 to 10 μm) under a uniaxial stress was studied at 800°C. The experiments allowed the measurement of the kinetics of densification and creep, the viscosities for creep and bulk deformation, and the sintering stress which was found to increase with density. The data show excellent qualitative agreement with Scherer's theory of viscous sintering. In addition, the quantitative comparison between theory and experiment shows good agreement; the measured viscosity of the bulk glass was ∽1×10⁹ P (∽1×10⁸ Pa·s) compared to ∽3×10⁹ P (∽3 Pa·s) obtained by fitting the data with Scherer's theory.     

Synthesis, Characterization, and Antibacterial Action of Hollow Ceria Nanospheres with/without a Conductive Polymer Coating

Hollow ceria nanospheres were synthesized using anionic polystyrene lattices which were prepared by emulsion polymerization of styrene using potassium persulfate as the initiator. These anionic colloidal particles were dispersed in water in the presence of poly(vinylpyrrolidone) and mixed with aqueous solutions of cerium (III) acetylacetonate [Ce(acac)₃]. Subsequently, hollow nanospheres of cerium compounds were obtained by calcination of the coated polystyrene lattices at an elevated temperature in air. The hollow ceria nanospheres were characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, thermogravimetric analysis, and differential thermal analysis. The hollow ceria nanospheres were coated with conductive polymers (polyaniline and polypyrrole) via an electropolymerization process. Moreover, the antibacterial action of illuminated hollow ceria nanospheres and hollow ceria nanospheres coated with conductive polymers (CPCeO₂) on a pure culture of Escherichia coli was studied. A decrease of E. coli concentration was observed after illumination of bacteria in the presence of hollow ceria nanospheres and CPCeO₂.     

Thermal Expansion of the Hexagonal (6H) Polytype of Silicon Carbide

The thermal expansion of the hexagonal (6H) polytype of α-SiC was measured from 20° to 1000°C by the X-ray diffraction technique. The principal axial coefficients of thermal expansion were determined and can be expressed for that temperature range by second-order polynomials: α¹¹= 3.27 × 10^–6+ 3.25 × 10^–9T – 1.36 × 10^–12 T ² (1/°C), and ş₃₃= 3.18 × 10^–6+ 2.48 × 10^–9 T – 8.51 × 10^–13 T ² (1/°C). The σ₁₁ is larger than α₃₃ over the entire temperature range while the thermal expansion anisotropy, the δş value, increases continuously with increasing temperature from about 0.1 × 10^–6/°C at room temperature to 0.4 × 10^–6/°C at 1000°C. The thermal expansion and thermal expansion anisotropy are compared with previously published results for the (6H) polytype and are discussed relative to the structure.     

Deviation from Stoichiometry in Cr2O3 at High Oxygen Partial Pressures

The deviation from stoichiometry, δ, in Cr₂−δO₃ was measured by a tensivolumetric method in the high pO₂ range of ≊10⁴ to 10⁴ Pa at 1100°C. The value of δ, or chromium vacancy concentration, was≊9×10⁻⁵ mol/mol Cr₂O₃ in air for Cr₂O₃ with 99.999% purity. The chemical diffusion coefficient, DT, determined from equilibration data was ≊4.6× cm²·s⁻¹ at 1100°C for pO₂= 2.2 ×10¹ Pa. The self-diffusion coefficient of Cr ions was calculated from and δ and found to be≊1.6×10-17 cm²-s⁻¹, in good agreement with recently measured values.     

Solubilities of Magnesia, Titania, and Magnesium Titanate in Aluminum Oxide

On heat treatment in air the solubility of MgO or TiO₂, in Al₂₃ is too small to detect by lattice parameter shifts. The solubility of MgTiO₃ in Al₂O₃ in air increased to the measured values, expressed as atomic fractions Mg:A1or Ti:A1of0.82 × lo-², 1.43 × 10^-2, and 1.75 × 10^-2 at 1250°, 1650°, and 1850°C, respectively. In 1 atm hydrogen the TiO₂ solubility expressed as the atomic fraction Ti:A1 is 0.55 × lo^-2, 0.75 × 10W², 1.15 × 10^-2, and 1.50 × 10^p2 at 1400°, 1500°, 1600°, and 1700°C, respectively. The increased solubility in H₂ was attributed to reduction of the titanium ion. The solubility of MgO in A1₂O₃ in vacuum (0.3μ) expressed as the atomic fraction Mg:A1 was measured as 1.10 × loW⁴, 3.00 × 10"⁴, 6.80 × 10–⁴, and 1.40 × 10^-3 at 1530°, 1630°, 1730°, and 183O°C, respectively. These contents did not cause an observable change in lattice parameter, but a slight change was observed when MgO was dissolved in A1₂O₃ in a hydrogen atmosphere.     

Volatilization of 137Cs and 106Ru from Borosilicate Glass Containing Actual High-Level Waste

Volatility of ¹³⁷ Cs and ¹⁰⁶Ru from borosilicate glass containing actual high-level waste was measured in an almost closed stainless-steel canister. The temperature dependence of the volatility of ¹³⁷Cs was close to that obtained in our previous study using ¹³⁴Cs. The volatility of ¹⁰⁶Ru was about one-fifth that of ¹³⁷Cs at 600° and 800°C. The air contamination by ¹³⁷Cs and ¹⁰⁶Ru in the canister at 400°C was estimated at 1.8 × 10² and 2 × 10 Bq/cm³, respectively, when it was assumed that the glass contained a realistic amount of ¹³⁷Cs and ¹⁰⁶Ru expected in commercial waste glass. These results are useful for predicting safety in a storage facility under operation.     

Thermal Expansion of the Low-Temperature Form of BaB2O4

Thermal expansion of the low-temperature form of BaB₂O₄ (β-BaB₂O₄) crystal has been measured along the principal crystallographic directions over a temperature range of 9° to 874°C by means of high-temperature X-ray powder diffraction. This crystal belongs to the trigonal system and exhibits strongly anisotropic thermal expansions. The expansion along the c axis is from 12.720 to 13.214 Å (1.2720 to 1.3214 nm), whereas it is from 12.531 to 12.578 Å (1.2531 to 1.2578 nm) along the a axis. The expansions are nonlinear. The coefficients A, B , and C in the expansion formula L _t = L ₀(1 + At + Bt ²+ Ct ³) are given as follows: a axis, A = 1.535 × 10⁻⁷, B = 6.047 × 10⁻⁹, C = -1.261 × 10⁻¹²; c axis, A = 3.256 × 10⁻⁵, B = 1.341 × 10⁻⁸, C = -1.954 × 10⁻¹²; and cell volume V, A = 3.107 × 10⁻⁵, B = 3.406 × 10⁻⁸, C = -1.197 × 10⁻¹¹. Based on α _t = (d L _t /d t )/ L ₀, the thermal expansion coefficients are also given as a function of temperature for the crystallographic axes a , c , and cell volume V.     

Third-Harmonic Generation from Some Chalcogenide Glasses

Third-order optical nonlinear susceptibilities (χ⁽³⁾) of some high-refractive-index chalcogenide glasses were evaluated from third-harmonic generation. Compared with oxide glasses whose χ⁽³⁾ has been known, χ⁽³⁾ of the present glasses was higher by an order of magnitude. The addition of selenium drastically increased χ⁽³⁾. The highest χ⁽³⁾ was 1.4 × 10^–11 esu, being comparable with those of high-χ⁽³⁾-organic compounds. Further, χ⁽³⁾ generally increased with increasing density in the present glasses.     

Nonradiative Energy Losses and Radiation Trapping in Neodymium-Doped Phosphate Laser Glasses

Fluorescence radiation trapping and nonradiative energy losses from the Nd³⁺⁴F_3/2 state are reported for two widely used commercial phosphate laser glasses (LHG-8 and LG-770). The effects of hydroxyl-group, transition-metal (Cu, Fe, V, Co, Ni, Cr, Mn, and Pt), and rare-earth (Dy, Pr, Sm, and Ce) impurities on the ⁴F_3/2 nonradiative decay rate in these glasses are quantified. Nd concentration quenching effects are reported for doping levels ranging from about 0.5 × 10²⁰ to 8.0 × 10²⁰ ions/cm³. The results are analyzed using the Förster–Dexter theory for dipolar energy transfer. Quenching rates for transition-metal ions correlate with the magnitude of spectral overlap for Nd emission (donor) and the metal ion absorption (acceptor). The nonradiative decay rates due to hydroxyl groups follow Förster–Dexter theory except at low Nd-doping levels (≲2 × 10²⁰ ions/cm³) where the quenching rate becomes independent of the Nd concentration. The data suggest a possible correlation of OH sites with Nd ions in this doping region. The effects of radiation trapping on the fluorescence decay are reported as a function of sample size, shape, and doping level. The results agree well with the theory except for samples with small doping-length products; in these cases, multiple internal reflections from the sample surfaces enhance the trapping effect.     

Oxidation Behavior of Si-C-O Fibers (Nicalon) under Oxygen Partial Pressures from 102 to 105 Pa at 1773 k

Polycarbosilane-derived SiC fibers (Nicalon) were oxidized at 1773 K under oxygen partial pressures from 10² to 10⁵ Pa. The effect of oxygen partial pressure on the oxidation behavior of the Nicalon fibers was investigated by examining mass change, surface composition, crystal phase, morphology, and tensile strength. The Nicalon fibers were passively oxidized under oxygen partial pressures of >2.5 ×10² Pa and actively oxidized under an oxygen partial pressure of 10² Pa. Under oxygen partial pressures from 2.5 × 10² to 10³ Pa, active oxidation occurred at the earliest stage of oxidation, resulting in the formation of both a silica film and a carbon intermediate layer. Although the unoxidized core retained considerable levels of strength under the passive-oxidation condition, fiber strength was lost under the active-oxidation condition.     

Annealing of Irradiation-Induced Thermal Conductivity Changes in ThO2-1.3 wt% UO2

The thermal conductivities of sintered pellets of ThO₂-1.3 wt% U0₂ were measured at 60°C before and after irradiation. The irradiation temperature was below 156°C, and the exposures varied from 3.1 × 10¹⁴ to 4.7 × lo^L7 fissions/cm³. Each fission fragment damaged a region of 2.2 × 10^-16 cm³ with the reduction in conductivity saturating by about 10¹⁷ fissions/cm³. Samples having exposures from 10¹⁵ to 10¹⁶ fissions/cm³ were annealed isothermally at 651 °C or isochronally from 300° to 1200° C to study the annealing of damage. Most of the annealing occurred between 500° and 900°C. The width of this interval plus the slow isothermal annealing suggest that the damage is annealed by a number of single order processes with a spectrum of activation energies from 1.8 to 3.9 eV or, less probably, by a high order process with an activation energy of 3.55 ± 0.4 eV.     

Enhanced Oxygen Diffusion at 1400°C in Deformed Single-Crystal Magnesium Oxide

The rate of oxygen difusion at 1400°C into pure, deformed, and scandium-doped MgO was measured using a secondary-ion mass spectrometer with ¹⁶O^- primary ions as sputtering agents to monitor the penetration of ¹⁸O into the sample from an ¹⁸O-enriched surface layer. In samples doped with scandium, oxygen diffusivity did not differ significantly from the value, 1.3 × 10-¹⁵ cm²/s, found for the pure sample. In deformed samples, the diffusion coefficient was 5.8 × 10^-15 cm²/s .     

Raman Spectrometric Determination of the Oxygen Self-Diffusion Coefficients in Oxides

New methods of determining the oxygen self-diffusion coefficients (D*_o) in oxides have been developed using Raman spectroscopy combined with the ¹⁶O–¹⁸O exchange technique. From the depth-profiles of the ¹⁸O concentration in the ¹⁶O–¹⁸O exchanged oxides, which was measured by Raman microscope with a spatial resolution of 5 μm, D *_o was determined for 2.8 mol% Y₂O₃-containing tetragonal zirconia polycrystall (the depth-profile method). Thus-obtained results are expressed as D *_O,D-P= 1.82(^+0.41_−0.40) × 10⁻¹·exp{−(139.3 ± 0.2) [kJ/mol]/ RT } [cm²/s] in the temperature range of 700–950^°C. We also determined D *_o for the same sample from the Raman spectrometric monitoring of the ambient gas during the ¹⁶O–¹⁸O exchange reaction (the gas-monitoring method). Thus-obtained results are expressed as D *_O,G-M= 1.14(^+0.05_−0.04) × 10⁻² exp{−(117.5 ± 0.4) [kJ/mol]/ RT } [cm²/s] in the temperature range of 700–1165°C. The results obtained from the above two different methods virtually agree with each other, indicating that reliable D *_o can be obtained by either of these two methods. We demonstrate that Raman spectroscopy is a useful tool for determining D *_o in oxides.     

Wick Debinding of Molybdenum-Silicon-Boron Extrudates

Wick debinding was investigated as possible means of binder removal for the Mo-Si-B extrudates. With increased temperature the amount of binder wicked out of the extrudate increased because of a decrease in viscosity, 2513 mPa·s at 75°C down to 7 mPa·s at 250°C. The permeability of the binder in the 1 μm wicking powder was higher than that in the 0.05 μm powder, 3.1 × 10⁻¹³ m² compared to 6.024 × 10⁻¹⁵ m². The amount of binder removed at a given temperature was considerably lower, which could be attributed to the larger capillary pressure difference between the 0.05 μm wick and the extrudate (1.55 × 10⁵ Pa compared to 1.46 × 10⁴ Pa for the 1 μm powder). Wicking removed approximately 80% of the binder in <10 h at 250°C with no defect formation.     

Effect of Reoxidation on the Grain-Boundary Acceptor-State Density of Reduced BaTiO3 Ceramics

To investigate the effect of reoxidation on the grain-boundary acceptor-state density of reduced barium titanate, n -doped BaTiO₃ ceramics are sintered in a reducing atmosphere (2% H₂+ 98% N₂) and then annealed in oxygen. After annealing at 1150°C for different times, the experimental results show a relationship between temperature-averaged acceptor-state density and annealing time as N _s= N _so Bt ^1/n with n between 2 and 3. An inherent acceptorstate density N _so= 4.25 × 10¹² cm⁻² is obtained with an increase rate B = 4.8 × 10¹² cm⁻². min^−1/3, when n reaches 3. The inherent grain-boundary acceptor states in the reduced n -doped BaTiO₃ ceramics are believed not due to adsorbed oxygen ions.     

Crystallization and Properties of Fe2O3—CaO—SiO2 Glasses

Nucleation and crystal growth rates and properties were studied in a two-stage heat treatment process for Fe₂O₃-CaO-SiO₂ glasses. Glass transition (T_g) and crystallization temperatures (T _c ) for the glasses lay between about 612.0° and 710.0°C, and 858.5° and 905.0°C, respectively, and magnetite was the main crystal phase. For a glass of 40Fe₂O₃. 20CaO·40SiO₂ (in wt%) the maximum nucleation rate was (68.6 ± 7) × 10⁶/mm³·s at 700°C, and the maximum crystal growth rate was 9.0 nm/min^1/2 at 1000°C. The mean crystal size of the magnetite increased from 30 to 140 nm with variation of nucleation and crystal growth conditions. The glass showed the maxima in saturation magnetization and coercive force, 212.1 × Wb/m² and 30.8 × 10³ A/m, when heat-treated for 4 h at 1000°C and 1050°C, respectively. The variation of the saturation magnetization could be quantitatively interpreted well in terms of the volume fraction of the magnetite, whereas that of the coercive forces could be explained only qualitatively in terms of the particle size of the magnetite. Hysteresis losses showed the maximum value of 1493 W/m³ when heat-treated at 1000°C for 4 h prenucleated at 700°C for 60 min, and increased linearly with increasing heat treatment time under a magnetic field up to 800 × 10³ A/m.     

Effects of Water Vapor on the Initial Sintering of Calcia

The effect of water vapor on the initial sintering kinetics of calcium oxide was studied at 920" to 1123°C. In the range of P_HI() from 8 × 10W⁴ to 487 mm Hg, water vapor increased the rate of sintering. The initial sintering kinetics followed the model for volume diffusion with calculated diffusion coefficients dependent on P _H2O, which varied from (P,_H2O)^1/2 at pressures between 6.1 and 50 mm Hg to (PI_H2O)^1/2 at pressures between 244 and 487 mm Hg. The activation enthalpy varied from 123 ± 7 kcal/mole when P_H2O= 0.04 mm Hg to 103 ± 3.5 kcal/mole at P_H2O 243.9 mm Hg.