Microstructural characterization of plasma sprayed Al2O3-40 wt.% TiO2 coatings on high density graphite with different post-treatments

Graphite is one of the candidate materials proposed for application in pyrochemical reprocessing plants involving aggressive molten chloride environment. Post treatments are promising techniques for the improvement of properties of thermal spray coatings for different industrial applications. In the present work, the effect of post treatments like vacuum annealing (VA) and laser melting (LM) on the microstructure and chemical modification of plasma sprayed Al₂O₃-40 wt.% TiO₂ coatings over high density (HD) graphite substrates has been investigated. When compared with sprayed coatings (SC), VA coatings showed cluster morphology and LM coatings exhibited homogenous microstructure. On laser melted surfaces networks of cracks were observed. XRD studies showed that the metastable γ-Al₂O₃ phase present in the SC is transformed to stable α-Al₂O₃ after post treatments. In LM coatings Al₂TiO₅ phase was more predominant in contrast to SC and VA coatings. The microhardness enhancement was observed in case of LM coating compared to the VA and SC. Due to elimination of coating defects in LM samples, there is a considerable reduction in the surface roughness.     

Evaluation of plasma sprayed alumina–40 wt% titania and partially stabilized zirconia coatings on high density graphite for uranium melting application

Ceramic coatings have been proposed on high density graphite crucibles for the application of uranium consolidation and distillation of molten salt in pyrochemical reprocessing of metallic fuels. Towards this, uranium melting experiments were carried out on plasma sprayed partially stabilized zirconia (PSZ) and Al₂O₃–40 wt% TiO₂ (A40T) coated high density graphite samples at 1350 °C using induction heating system for evaluating the compatibility of these coatings with molten uranium. The coated high density graphite samples were characterized before and after uranium melting test by scanning electron microscopy attached with energy dispersive X-ray spectroscopy, X-ray diffraction and Raman spectroscopy. Microstructural observations revealed that no significant reaction layer or product was formed between uranium and PSZ coating, while uranium significantly adhered to A40T coating. PSZ coating offers better stability and protection to high density graphite crucibles from the chemical attack by molten uranium.     

Preparation of a platinum electrocatalyst by coaxial pulse arc plasma deposition

We have developed a new method of preparing Pt electrocatalysts through a dry process. By coaxial pulse arc plasma deposition (CAPD), highly ionized metal plasma can be generated from a target rod without any discharged gases, and Pt nanoparticles can be deposited on a carbon support. The small-sized Pt nanoparticles are distributed over the entire carbon surface. From transmission electron microscopy (TEM), the average size of the deposited Pt nanoparticles is estimated to be 2.5 nm, and their size distribution is narrow. Our electrocatalyst shows considerably improved catalytic activity and stability toward methanol oxidation reaction (MOR) compared with commercially available Pt catalysts such as Pt black and Pt/carbon (PtC). Inspired by its very high efficiency toward MOR, we also measured the catalytic performance for oxygen reduction reaction (ORR). Our PtC catalyst shows a better performance with half-wave potential of 0.87 V, which is higher than those of commercially available Pt catalysts. The higher performance is also supported by a right-shifted onset potential. Our preparation is simple and could be applied to other metallic nanocrystals as a novel platform in catalysis, fuel cells and biosensors.     

Intergranular corrosion damage evaluation through laser scattering technique

AISI type 316 austenitic stainless steel in sensitized condition was subjected to ASTM A262 practice A test (electrolytic etching in 10% ammonium persulphate at 1 A/cm²) for various durations from 10 s to 90 s. The different degrees of intergranular corrosion attack produced on these tested specimens were evaluated by laser scattering technique using a 1 mW He-Ne laser. The scattering intensity pattern of the laser beam incident on the specimen was acquired using a CCD camera and transferred to a computer for further analysis. The specular intensity of the scattering pattern and its full width at half maximum (FWHM) was calculated. The results indicated that the specular intensity decreased and the FWHM increased as the degree of IGC attack increased. A good correlation was found between the extent of IGC with the laser scattering parameters.     

Interrelationship of cardiovascular effects, plasma levels of nicorandil, and vascular cGMP formation in conscious rats

OBJECTIVE: To determine the reproducibility of duplex Doppler waveform analysis and fetal cardiac interventricular septal thickness measurement and to compare these parameters in matched pregnancies with and without well-controlled maternal Type 1 diabetes at 18-20 weeks of gestation. DESIGN: A prospective blind twin cohort study and a blinded inter-observer and intra-observer agreement study. SETTING: A tertiary referral prenatal diagnostic unit within a university hospital. RESULTS: Good inter- and intra-observer agreement was found for the measurement of transvalvular peak flow velocities and the duration of ventricular ejection in the fetal heart. Inter-observer agreement for aortic flow acceleration rate was poor. M-mode measurement of interventricular septal thickness showed moderate reproducibility. The mean (SD) width of the interventricular septum in the fetuses of well controlled diabetic women was 2 1 mm (0.2 mm), and was significantly greater (P=0.01) when compared with the corresponding value in matched controls [1.9 mm (0.2 mm)]. No cardiac functional differences were evident. CONCLUSIONS: On-screen video analysis of Doppler cardiac flow waveforms and M-mode measurement of intraventricular septal thickness demonstrated good reproducibility. The fetuses of well controlled diabetic pregnancies demonstrated signs of altered cardiac morphology early in pregnancy, before any evident alterations in cardiac function.     

Corrosion-Resistant Ti-<Emphasis Type="Italic">x</Emphasis>Nb-<Emphasis Type="Italic">x</Emphasis>Zr Alloys for Nitric Acid Applications in Spent Nuclear Fuel Reprocessing Plants

This article reports the development, microstructure, and corrosion behavior of two new alloys such as Ti-4Nb-4Zr and Ti-2Nb-2Zr in boiling nitric acid environment. The corrosion test was carried out in the liquid, vapor, and condensate phases of 11.5 M nitric acid, and the potentiodynamic anodic polarization studies were performed at room temperature for both alloys. The samples subjected to three-phase corrosion testing were characterized using scanning electron microscopy (SEM) and energy-dispersive X-ray microanalysis (EDAX). As Ti-2Nb-2Zr alloy exhibited inferior corrosion behavior in comparison to Ti-4Nb-4Zr in all three phases, weldability and heat treatment studies were carried out only on Ti-4Nb-4Zr alloy. The weldability of the new alloy was evaluated using tungsten inert gas (TIG) welding processes, and the welded specimen was thereafter tested for its corrosion behavior in all three phases. The results of the present investigation revealed that the newly developed near alpha Ti-4Nb-4Zr alloy possessed superior corrosion resistance in all three phases and excellent weldability compared to conventional alloys used for nitric acid application in spent nuclear reprocessing plants. Further, the corrosion resistance of the beta heat-treated Ti-4Nb-4Zr alloy was superior when compared to the sample heat treated in the alpha + beta phase.     

Corrosion behavior of Zr-based metallic glass coating on type 304L stainless steel by pulsed laser deposition method

The surface morphology and corrosion behavior of Zr-based amorphous metallic glass (MG) of Zr₅₉Ti₃Cu₂₀Al₁₀Ni₈ alloy and MG coated type 304L stainless steel in different nitric acid media of 1 M, 6 M and 11.5 M HNO₃ is reported. Zirconium based MG of Zr₅₉Ti₃Cu₂₀Al₁₀Ni₈ alloy was successfully deposited on type 304L stainless steel using pulsed laser deposition technique. The SEM morphology revealed a scattered particles of “Donut” shaped features distributed in the amorphous matrix. The atomic force microscope measurement indicated the formation of dense metallic deposited layer of agglomerate of granular clusters with negligible pores or micro-crack in metallic glass coated sample. The results of the potentiodynamic polarization shows that the amorphous MG coated type 304L stainless steel exhibited marginally lower corrosion resistance than MG alloy which is attributed to the presence of corrosion-induced defects in the coated layer. This work reports suitability of using pulsed laser deposition for the preparation of thin film amorphous metallic coating to achieve improved corrosion resistance in nitric acid medium.     

Corrosion behaviour of AISI type 304L stainless steel in nitric acid media containing oxidizing species

The corrosion behaviour of AISI type 304L stainless steel (SS) in different concentration of 0.01 M, 1 M and 5 M HNO₃ in presence of oxidizing ions at different temperatures has been evaluated. The main objective of this study is to assess the corrosion resistance of type 304L SS in non-radioactive conditions encountered during storage of liquid nuclear waste. Electrochemical impedance spectroscopy (EIS) and laser Raman spectroscopy (LRS) has clearly brought out the deleterious effect of oxidizing species on the passive film leading to increased corrosion along with increase in HNO₃ concentration and higher temperature.     

Interpretation of Electrochemical Potentiokinetic Reactivation data in the presence of sulphide/oxysulphide inclusions in 316LN stainless steel

This paper presents the Electrochemical Potentiokinetic Reactivation (EPR) parameters obtained for non-sensitised 316LN stainless steel containing sulphide/oxysulphide inclusions. Even in the absence of sensitization, reactivation peaks were obtained in single loop and double loop EPR experiments for longitudinal and cross transverse sections. Using Laser Raman Spectroscope, Raman maps of Cr (VI) oxide were obtained around the inclusions. It was inferred that the reactivation peak is due to dissolution of sulphide inclusions and chromium depleted zones arising around chromium segregated flow lines. The need to interpret EPR parameters carefully in the presence of sulphide inclusions is emphasised.