Manjima Bhattacharya

Nanocolumnar Crystalline Vanadium Oxide-Molybdenum Oxide Antireflective Smart Thin Films with Superior Nanomechanical Properties.

Vanadium oxide-molybdenum oxide (VO-MO) thin (21–475 nm) films were grown on quartz and silicon substrates by pulsed RF magnetron sputtering technique by altering the RF power from 100 to 600 W. Crystalline VO-MO thin films showed the mixed phases of vanadium oxides e.g., V2O5, V2O3 and VO2 along with MoO3. Reversible or smart transition was found to occur just above the room temperature i.e., at ~45–50 °C. The VO-MO films deposited on quartz showed a gradual decrease in transmittance with increase in film thickness. But, the VO-MO films on silicon exhibited reflectance that was significantly lower than that of the substrate. Further, the effect of low temperature (i.e., 100 °C) vacuum (10−5 mbar) annealing on optical properties e.g., solar absorptance, transmittance and reflectance as well as the optical constants e.g., optical band gap, refractive index and extinction coefficient were studied. Sheet resistance, oxidation state and nanomechanical properties e.g., nanohardness and elastic modulus of the VO-MO thin films were also investigated in as-deposited condition as well as after the vacuum annealing treatment. Finally, the combination of the nanoindentation technique and the finite element modeling (FEM) was employed to investigate yield stress and von Mises stress distribution of the VO-MO thin films.

Nanoscale contact resistance of V2O5 xerogel films developed by nanostructured powder

Here we report the synthesis of V2O5 nanostructures by a fast, simple, cost-effective, low-temperature chemical process; followed by the deposition of V2O5 xerogel thin films on a glass substrate by a sol-gel route. Phase analysis, phase transition, microstructural and electronic characterization studies are carried out by x-ray diffraction, texture coefficient analysis, field emission scanning electron microscopy, transmission electron microscopy (TEM), related selected area electron diffraction pattern (SAED) analysis, Fourier transform infrared spectroscopy, thermogravimetry and differential thermal analysis, differential scanning calorimetry, and x-ray photoelectron spectroscopy techniques. Confirmatory TEM and SAED data analysis prove further that in this polycrystalline powder there is a unique localized existence of purely single crystalline V2O5 powder with a preferred orientation in the (0 1 0) direction. The most interesting result obtained in the present work is that the xerogel thin films exhibit an inherent capability to enhance the intrinsic resistance against contact induced deformations as more external load is applied during the nanoindentation experiments. In addition, both the nanohardness and Youngs modulus of the films are found to be insensitive to load variations (e.g. 1 to 7 mN). These results are explained in terms of microstructural parameters, e.g. porosity and structural configuration.

Nanotribological response of a plasma nitrided bio-steel.

AISI 316L is a well known biocompatible, austenitic stainless steel (SS). It is thus a bio-steel. Considering its importance as a bio-prosthesis material here we report the plasma nitriding of AISI 316L (SS) followed by its microstructural and nanotribological characterization. Plasma nitriding of the SS samples was carried out in a plasma reactor with a hot wall vacuum chamber. For ease of comparison these plasma nitrided samples were termed as SSPN. The experimental results confirmed the formations of an embedded nitrided metal layer zone (ENMLZ) and an interface zone (IZ) between the ENMLZ and the unnitrided bulk metallic layer zone (BMLZ) in the SSPN sample. These ENMLZ and IZ in the SSPN sample were richer in iron nitride (FeN) chromium nitride (CrN) along with the austenite phase. The results from nanoindentation, microscratch, nanoscratch and sliding wear studies confirmed that the static contact deformation resistance, the microwear, nanowear and sliding wear resistance of the SSPN samples were much better than those of the SS samples. These results were explained in terms of structure-property correlations.

Effect of low temperature vacuum annealing on microstructural, optical, electronic, electrical, nanomechanical properties and phase transition behavior of sputtered vanadium oxide thin films

Vanadium oxide thin films were deposited on quartz substrate by pulsed RF magnetron sputtering technique at 400–600 W and subsequently annealed at 100 °C in vacuum (1.5 × 10−5 mbar). Phase analysis, surface morphology and topology of the films e.g., both as-deposited and annealed were investigated by x-ray diffraction, field emission scanning electron microscopy and atomic force microscopy techniques. X-ray photoelectron spectroscopy (XPS) was employed to understand the elemental oxidation of the films. Transmittance of the films was evaluated by UV–vis-NIR spectrophotometer in the wavelength range of 200–1600 nm. Sheet resistance of the films was measured by two-probe method both for as-deposited and annealed conditions. XPS study showed the existence of V5+ and V4+ species. Metal to insulator transition temperature of the as-deposited film decreased from 339 °C to 326 °C after annealing as evaluated by differential scanning calorimetric technique. A significant change in transmittance was observed in particular at near infrared region due to alteration of surface roughness and grain size of the film after annealing. Sheet resistance values of the annealed films decreased as compared to the as-deposited films due to the lower in oxidation state of vanadium which led to increase in carrier density. Combined nanoindentation and finite element modeling were applied to evaluate nanohardness (H), Youngs modulus (E), von Mises stress and strain distribution. Both H and E were improved after annealing due to increase in crystallinity of the film.

Microstructural, thermo-optical, mechanical and tribological behaviours of vacuum heat treated ultra thin SS304 foils

The purpose of this present study was to evaluate the effect of vacuum (i.e., 10−5 mbar) heat treatment at 300 to 1100 °C on morphological, thermo-optical, mechanical and tribological properties of 75 μm thin SS304 foils. Microstructural, morphological and surface properties of the foils were characterized by field emission scanning electron microscopy (FESEM), profilometry, x-ray photoelectron spectroscopy (XPS) and water contact angle (WCA) measurement techniques, respectively. The x-ray diffraction (XRD) was employed to identify the phase of SS304 foils after different heat treatment temperatures. Thermo-optical properties such as solar absorptance (α s), reflectance (ρ s) and IR emittance (e ir) were also evaluated. The nanomechanical properties i.e., nanohardness (H) and Youngs modulus (E) of as-received and heat treated SS304 foils were evaluated by the nanoindentation technique. Tribological and tensile properties i.e., yield strength (σ y) and percentage of elongation of different heat treated foils were also investigated by single pass scratch tests and universal testing machine, respectively. Noteworthy grain growth of SS304 was observed beyond vacuum heat treatment temperature of 700 °C. As a consequence, the magnitudes of both H and E data of SS304 were significantly decreased beyond the vacuum heat treatment temperature of 700 °C. Further, the hardness data followed the well known Hall–Petch relationship. On the other hand, the tribological property of SS304 was significantly deteriorated beyond the vacuum heat treatment temperature of 700 °C. The tensile strength of the foils was also altered after the heat treatment.

Failure and deformation mechanisms at macro- and nano-scales of alkali activated clay

Here we report two qualitative models on failure and deformation mechanisms at macro- and nano-scales of alkali activated clay (AACL), a material of extraordinary importance as a low cost building material. The models were based on experimental data of compressive failure and nanoindentation response of the AACL materials. A 420% improvement in compressive strength (sigma(c)) of the AACL was achieved after 28 days (d) of curing at room temperature and it correlated well with the decrements in the residual alkali and pH concentrations with the increase in curing time. Based on extensive post-mortem FE-SEM examinations, a schematic model for the compressive failure mechanism of AACL was proposed. In addition, the nanoindentation results of AACL provided the first ever experimental evidence of the presence of nano-scale plasticity and a nano-scale contact deformation resistance that increased with the applied load. These results meant the development of a unique strain tolerant microstructure in the AACL of Indian origin. The implications of these new observations were discussed in terms of a qualitative model based on the deformation of layered clay structure.

Self-adjusting unique nanoscale contact resistance of a single alumina grain

This work evaluates the nanohardness of a single alumina grain for a coarse grain alumina ceramic of similar to 10 mu m grain size. The results reveal that the nanoscale contact deformation resistance of the single grain has a unique self-adjusting characteristic. It increases in response to enhancement in the externally applied load. The nanoscale contact deformation resistance of a single alumina grain is determined by controlled nano-indentation experiments. The corresponding load versus depth plots are carefully analysed to identify the critical load at which the very first burst of incipient nanoscale plasticity is initiated. To avoid any spurious effect from neighbouring grain boundaries the nano-indentations experiments are deliberately carried out with only single grains. A range of ultra low loads that span from 1000 to 12 000 mu N is used for this purpose. Both partial unload and load controlled nano-indentation experiments are performed with a Berkovich indenter on single alumina grains. The indenter has a tip radius of 150 nm. The results show for the very first time that a mild indentation size effect exists even in single grain hardness at nanoscale. In addition the intrinsic nanoscale contact deformation resistance increases as the externally applied load is enhanced. The way it increases follows an empirical power law. These results are analysed in terms of the dislocation loop radius, critical resolved shear stress and the maximum shear stress that is generated just underneath the indenter.

Nanomechanical responses of human hair

Here we report the first ever studies on nanomechanical properties e.g., nanohardness and Young׳s modulus for human hair of Indian origin. Three types of hair samples e.g., virgin hair samples (VH), bleached hair samples (BH) and Fe-tannin complex colour treated hair samples (FT) with the treatment by a proprietary hair care product are used in the present work. The proprietary hair care product involves a Fe-salt based formulation. The hair samples are characterized by optical microscopy, atomic force microscopy, field emission scanning electron microscopy, energy dispersive X-ray spectroscopy (EDAX) genesis line map, EDAX spot mapping, nanoindentation, tensile fracture, and X-ray diffraction techniques. The nanoindentation studies are conducted on the cross-sections of the VH, BH and FT hair samples. The results prove that the nanomechanical properties e.g., nanohardness and Young׳s modulus are sensitive to measurement location e.g., cortex or medulla and presence or absence of the chemical treatment. Additional results obtained from the tensile fracture experiments establish that the trends reflected from the evaluations of the nanomechanical properties are general enough to hold good. Based on these observations a schematic model is developed. The model explains the present results in a qualitative yet satisfactory manner.

Contact Deformation of Alumina

The study of contact-induced deformations during hardness evaluation and the subsequent damage mechanisms of alumina under low loads deserves significant importance for its applications as wear-resistant inserts, biomedical implants, thin films, and armour plates, because the contact-induced brittle failure is an issue of major scientific concern that prevents their widespread commercial applications. However, the studies on hardness of dense, coarse grain alumina at ultralow load, for example, 1 N, are still lacking. Therefore, the present study was conducted on a dense (~95% of theoretical) coarse-grain (~20 μm) alumina at a low peak load of 1 N with varying loading rates (10−3–100 N·s−1) applied in depth sensitive indentation experiments. The results showed profuse presence of multiple micro-pop-in and pop-out events possibly linked to dislocation nucleations underneath the indenter. The critical resolved shear stress () was found to enhance with the increase in applied loading rates. The occurrences of the localized shear deformation band formation and microcracking in and around the indentation cavity were explained in terms of the correlation between the nanoscale plasticity events, the small magnitude of (), the maximum shear stress () developed just underneath the indenter, and the dislocation loop radius ().

Single-crystal alumina under nanoindentation: loading rate effect

Manjima Bhattacharya1, Arjun Dey2, Anoop Mukhopadhyay3 1Department Of Chemical Sciences, Indian Institute Of Science Education And Resea, Kolkata, India, 2Thermal Systems Group, ISRO Satellite Centre, Vimanapura Post, Bangalore560 017, India, Bangalore, India, 3Advanced Mechanical and Materials Characterization Division, CSIR-Central Glass and Ceramic Research Institute, Kolkata700 032, India, Kolkata, India E-mail: mbmanjima7@gmail.com