Lakshman Neelakantan

Titania nanotubes from weak organic acid electrolyte: Fabrication, characterization and oxide film properties

In this study, TiO2 nanotubes were fabricated using anodic oxidation in fluoride containing weak organic acid for different durations (0.5h, 1h, 2h and 3h). Scanning electron microscope (SEM) micrographs reveal that the morphology of titanium oxide varies with anodization time. Raman spectroscopy and X-ray diffraction (XRD) results indicate that the as-formed oxide nanotubes were amorphous in nature, yet transform into crystalline phases (anatase and rutile) upon annealing at 600°C. Wettability measurements show that both as-formed and annealed nanotubes exhibited hydrophilic behavior. The electrochemical behavior was ascertained by DC polarization and AC electrochemical impedance spectroscopy (EIS) measurements in 0.9% NaCl solution. The results suggest that the annealed nanotubes showed higher impedance (10(5)-10(6)Ωcm(2)) and lower passive current density (10(-7)Acm(-2)) than the as-formed nanotubes. In addition, we investigated the influence of post heat treatment on the semiconducting properties of the oxides by capacitance measurements. In vitro bioactivity test in simulated body fluid (SBF) showed that precipitation of Ca/P is easier in crystallized nanotubes than the amorphous structure. Our study uses a simple strategy to prepare nano-structured titania films and hints the feasibility of tailoring the oxide properties by thermal treatment, producing surfaces with better bioactivity.

Design and fabrication of a bending rotation fatigue test rig for in situ electrochemical analysis during fatigue testing of NiTi shape memory alloy wires

The current investigation proposes a novel method for simultaneous assessment of the electrochemical and structural fatigue properties of nickel-titanium shape memory alloy (NiTi SMA) wires. The design and layout of an in situ electrochemical cell in a custom-made bending rotation fatigue (BRF) test rig is presented. This newly designed test rig allows performing a wide spectrum of experiments for studying the influence of fatigue on corrosion and vice versa. This can be achieved by performing ex situ and∕or in situ measurements. The versatility of the combined electrochemical∕mechanical test rig is demonstrated by studying the electrochemical behavior of NiTi SMA wires in 0.9% NaCl electrolyte under load. The ex situ measurements allow addressing various issues, for example, the influence of pre-fatigue on the localized corrosion resistance, or the influence of hydrogen on fatigue life. Ex situ experiments showed that a pre-fatigued wire is more susceptible to localized corrosion. The synergetic effect can be concluded from the polarization studies and specifically from an in situ study of the open circuit potential (OCP) transients, which sensitively react to the elementary repassivation events related to the local failure of the oxide layer. It can also be used as an indicator for identifying the onset of the fatigue failure.

An in situ tensile tester for studying electrochemical repassivation behavior: Fabrication and challenges

An in situ tensile rig is proposed, which allows performing electrochemical (repassivation) experiments during dynamic mechanical testing of wires. Utilizing the basic components of a conventional tensile tester, a custom-made minitensile rig was designed and fabricated. The maximal force that can be measured by the force sensor is 80 N, with a sensitivity of 0.5 mV/V. The maximum travel range of the crosshead induced by the motor is 10 mm with a minimum step size of 0.5 nm. The functionality of the tensile test rig was validated by investigating Cu and shape memory NiTi wires. Wires of lengths between 40 and 50 mm with varying gauge lengths can be tested. An interface between wire and electrochemical setup (noncontact) with a smart arrangement of electrodes facilitated the electrochemical measurements during tensile loading. Preliminary results on the repassivation behavior of Al wire are reported.

Note: Design and fabrication of a simple versatile microelectrochemical cell and its accessories

A microelectrochemical cell housed in an optical microscope and custom-made accessories have been designed and fabricated, which allows performing spatially resolved corrosion measurements. The cell assembly was designed to directly integrate the reference electrode close to the capillary tip to avoid air bubbles. A hard disk along with an old optical microscope was re-engineered into a microgrinder, which made the vertical grinding of glass capillary tips very easy. A stepper motor was customized into a microsyringe pump to dispense a controlled volume of electrolyte through the capillary. A force sensitive resistor was used to achieve constant wetting area. The functionality of the developed instrument is demonstrated by studying μ-electrochemical behavior of worn surface on AA2014-T6 alloy.

Imidazolium-based ionic liquids as an anticorrosive agent for completion fluid design

Most of the onshore and offshore oil and gas reservoirs are facing operational challenges due to high temperature and high salinity, thus requiring advanced techniques for realizing the expected oil recovery with the use of specially designed chemicals. During oil and gas well development, completion fluids, which are solids-free liquids, are used to complete an oil or gas well. Completion fluids consisting of brines are primarily used for oil and gas well stabilization and are corrosive in nature. There is a need to develop additives to be added with completion fluids to address the corrosive nature. The present investigation involved the usage of two imidazolium ionic liquids (ILs) as corrosion inhibitors for mild steel in various completion brine (CaCl2, HCOOCs and ZnBr2) fluids. The study was performed using various techniques, such as, potentiodynamic polarization, weight loss measurements and exposure studies. All the above techniques showed promising results which indicated that the ILs as corrosion inhibitors used were of the mixed-type following both physisorption and chemisorption over the mild steel surface. Among the two inhibitors studied here, 1-octyl-3-methyl imidazolium chloride ([OMIM]+[Cl]-) with longer alkyl chain exhibited better inhibition efficiency and much lesser corrosion rate than 1-butyl-3-methyl imidazolium chloride ([BMIM]+[Cl]-) with a shorter alkyl chain. The results obtained from various methodologies indicate that ionic liquids can be explored to develop anti-corrosive completion fluids suitable for oil and gas reservoirs.