Scanning thermal probe microscope method for the determination of thermal diffusivity of nanocomposite thin films.

A commercial scanning thermal microscope has been upgraded to facilitate its use in estimating the radial thermal diffusivity of thin films close to room temperature. The modified setup includes a microcontroller driven microhotplate coupled with a Bluetooth module for wireless control. The microcontroller board (Arduino Leonardo) is used to generate a bias of suitable voltage amplitude and pulse duration which is applied across the microhotplate contact pads. A corresponding heat pulse from the Pt heating element (1 mm(2)) embedded within the microhotplate is delivered to the lower surface of the thin film (25 mm(2)) deposited over it. The large difference in the dimensions of the heating source and the thin film surface causes heat to flow radially outwards on the top surface of the latter. The decay of this radial heat wave as it flows outwards is recorded by the scanning thermal microscope in terms of temperature-time (T-t) profiles at varying positions around the central heating zone. A fitting procedure is suggested to extract the thermal diffusivity value from the array of T-t profiles. The efficacy of the above setup has been established by evaluating the thermal diffusivities of Bi2Te3 and Bi2Te3:Si thin film samples. Further, with only minor alterations in design the capabilities of the above setup can be extended to estimate the axial thermal diffusivity and specific heat of thin films, as a function of temperature.

Exploring Nanoscale Electrical Properties of CuO-Graphene Based Hybrid Interfaced Memory Device by Conductive Atomic Force Microscopy.

The phenomenon of resistive switching is based on nanoscale changes in the electrical properties of the interface. In the present study, conductive atomic force microscope based nanoscale measurements of copper oxide (CuO-multilayer graphene (MLG) hybrid interface based devices have been carried out to understand changes in the electrical properties during resistive switching of the Ti-CuO/MLG-Cu memory cells having different dimensions fabricated on the same substrate using stencil lithography technique. The dependence of resistive switching characteristics in LRS and HRS and current level of the conductive filaments (CF) on the electrode area have been studied. As the device dimension is reduced, the filamentary contribution is enhanced in comparison to the background contribution, resulting in'an increase in the current density ratio between LRS and HRS. It is also observed that as the device dimension is decreased from 150 to 25 µm, the filament size decreases from 95 nm to 20 nm, respectively, which causes a decrease in the reset current and reset voltage. The results of the nanoscale CAFM measurements have shown a good correlation with the switching parameters obtained by the macroscale pad I-V measurements, thereby, suggesting the origin of resistive switching is due to the formation and rupture of an entity called filament, whose dimension is in nanorange. It is observed that changes in the electrical properties of the overall interface layer along with changes in the electrical conductivity of these filaments contribute towards resistive switching phenomenon. This study suggests that a significant reduction of reset current can be achieved by decreasing the memory device dimensions.

CAFM investigations of filamentary conduction in Cu2O ReRAM devices fabricated using stencil lithography technique.

With the objective of understanding the role of size and current level of filamentary regions on the resistive switching parameters, detailed conductive atomic force microscope investigations of resistive memory cells having different dimensions have been carried out in this study. Cu-Cu(2)O-Ti memory cells having dimensions of 150, 50 and 25 µm have been fabricated on the same substrate using a stencil lithography technique. The dependence of resistive switching parameters on the device dimensions can be directly related to the average size, current level of the filaments and difference in these parameters between the low resistance state (LRS) and high resistance state (HRS). It is observed that the large increase in the ratio of current in the two states in cells having lower dimensions is mainly due to the smaller number of conducting regions in the HRS, indicating efficient switching from the LRS to the HRS at lower dimensions.

Fast response and recovery of hydrogen sensing in Pd-Pt nanoparticle-graphene composite layers.

This study reports the fast response and recovery of hydrogen sensing in nanoparticle-graphene composite layers fabricated using chemical methods and comprising of isolated Pd alloy nanoparticles dispersed onto graphene layers. For 2% hydrogen at 40 °C and 1 atm pressure, a response time of <2 s and a recovery time of 18 s are observed. The fast response and recovery observed during sensing are due to hydrogen-induced changes in the work function of the Pd alloy and modification in the distribution of defect states in the graphene band gap due to gas adsorption. The results of hydrogen sensing in the new class of Pd-Pt nanoparticle-graphene composite material are important for understanding the effect of gas adsorption on electronic conduction in graphene layers and for developing a new type of gas sensor based on changes in the electronic properties of the interface.

Photovoltaic response of a topotaxially formed CdS-Cu(x)S single nanorod heterojunction.

In the present study, a combination of a hydrothermal route and a topotaxial conversion reaction has been used to grow a cadmium sulfide-copper sulfide (CdS-Cu(x)S) single nanorod heterojunction. The J-V characteristics of the CdS nanorods show Shockley behaviour consistent with the energy band diagram of the platinum conducting atomic force microscope (CAFM) probe-CdS nanorod combination. The photovoltaic response measured on the CdS-Cu(x)S nanorods using a CAFM probe shows the formation of a heterojunction with an open circuit voltage of 320 mV, a short circuit current density of 5.5 mA cm⁻² and a crossover of dark and light J-V curves related to the photoconductivity of the interfacial CdS layer. The lengthwise heterojunction fabricated in the present study has many potential advantages in comparison to other single nanorod junctions.

Resistive switching in copper oxide nanorods: a bottom up approach applicable for enhanced scalability.

Reversible, stable and reproducible resistive switching in a parallel network of Cu2O nanorods, observed in the present study, highlights the advantages of using nanorods in comparison to normally used thin films. Unipolar and symmetric current-voltage characteristics of the metal/insulator/metal structure consisting of Hg top contact/Copper oxide (Cu2O) nanorods/Ag bottom contact in a sandwich configuration shows electroforming at about 11 V, reproducible reset and set points at 0.53 +/- 0.03 and 4.2 +/- 0.02 V and a high OFF/ON resistance ratio > 10(3). Slope of current-voltage characteristics and current contrast in CAFM mapping indicate that filamentary conduction mechanism is responsible for resistive switching. This study sets the foundation for fabricating a nanorods based resistive random access memory device and thus a manifold increase in the device scalability.

Synthesis and luminescence properties of alumina encapsulated InN nanorods.

The present study reports a two-step procedure to synthesize InN nanorods inside the pores of an anodic alumina membrane. In the first step, pores of the membrane are filled with indium via electrodeposition. The second step involves nitridation of the as-deposited nanorods by room temperature plasma annealing. X-ray diffraction studies reveal that as-deposited nanorods consist of In, In2O3 and In(OH)3 phases which get converted to mixed hexagonal and cubic phase InN on plasma annealing. Cross sectional scanning electron microscope study reveals nanorod diameter and length to be 150 nm and 1 microm respectively. X-ray mapping results establish that uniform distribution of nitrogen throughout the length of nanorod has been achieved as a result of plasma annealing. Observation of photoluminescence peaks at 1.4 and 1.6 eV corresponding, to the absorption edges of cubic and hexagonal phases of InN show that room temperature photoemission is due to band to band recombination. The use of alumina as a template for nanorod growth prevents post-deposition agglomeration and provides mechanical strength. Possibility of total internal reflection at the InN-Al2O3 interface makes these structures ideally suitable to reduce the emitted light intensity losses.

Anomalous high pressure behaviour in nanosized rare earth sesquioxides.

We report Raman spectroscopic studies of the nanosized rare earth sesquioxides, namely yttrium sesquioxide (Y(2)O(3)), gadolinium sesquioxide (Gd(2)O(3)) and samarium sesquioxide (Sm(2)O(3)), under high pressure. The samples were characterized using x-ray diffraction, Raman spectroscopy and atomic force microscopy at atmospheric pressures. Y(2)O(3) and Gd(2)O(3) were found to be cubic at ambient, while Sm(2)O(3) was found to be predominantly cubic with a small fraction of monoclinic phase. The strongest Raman peaks are observed at 379, 344 and 363 cm(-1), respectively, for Y(2)O(3), Sm(2)O(3) and Gd(2)O(3). All the samples were found to be nanosized with 50-90 nm particle sizes. The high pressures were generated using a Mao-Bell type diamond anvil cell and a conventional laser Raman spectrometer is used to monitor the pressure-induced changes. Y(2)O(3) seems to undergo a crystalline to partial amorphous transition when pressurized up to about 19 GPa, with traces of hexagonal phase. However, on release of pressure, the hexagonal phase develops into the dominant phase. Gd(2)O(3) is also seen to develop into a mixture of amorphous and hexagonal phases on pressurizing. However, on release of pressure Gd(2)O(3) does not show any change and the transformation is found to be irreversible. On the other hand, Sm(2)O(3) shows a weakening of cubic phase peaks while monoclinic phase peaks gain intensity up to about a pressure of 6.79 GPa. However, thereafter the monoclinic phase peaks also reduce in intensity and mostly disordering sets in which does not show significant reversal as the pressure is released. The results obtained are discussed in detail.

A high performance lipase preparation: characterization and atomic force microscopy.

The goal of obtaining enzyme forms which show greater stability, higher catalytic efficiency, and reusability has been pursued since last several decades. Some novel biocatalyst designs have been evolved and protein coated micro-crystals (PCMCs) is one of them. Pseudomonas cepacia lipase coated micro-crystals were prepared by simultaneous precipitation of mixture of aqueous lipase solution and salts such as potassium sulphate by organic solvents. This resulted in lipase coated micro-crystals. The structures of micro-crystals were studied by atomic force microscopy (AFM). The AFM picture confirmed the enzyme coating over the potassium sulphate crystals. These PCMCs are in the size range of 500-1000 nm. These enzyme coated micro-crystals showed enhanced transesterification rates. Also, the PCMC were stable at 60 degrees C whereas the free enzyme lost all its activity. The enzyme coated micro-crystals prepared by 50 mg Pseudomonas cepacia lipase gave 96% conversion in 90 min whereas free enzyme gave 8% conversion. Even PCMCs prepared from 3.12 mg lipase gave 90% conversion in 10 h at 60 degrees C where as free lipase was inactive at 60 degrees C.

Modification of the crystal habit of celecoxib for improved processability.

Crystallization is often used in the pharmaceutical industry for purification and isolation of drugs, and also as a means of generating polymorphs or isomorphs. The aim of this study was to investigate the role of extrinsic crystallization parameters on the crystallized product, with special emphasis on improving the mechanical properties of acicular celecoxib. Celecoxib isomorphs were prepared using different techniques (solvent crystallization and vapour diffusion) and crystallization conditions (solvents, stirring, degree of supersaturation, crystallization temperature and seeding). Powder X-ray diffractometry, spectroscopic and thermal methods were used to investigate physical characteristics of crystals. Growth kinetics and aggregation dynamics of crystallization in polar and non-polar solvents were simulated using a dynamic light scattering method. The quick appearance of broad peaks over the range of 10-8000 nm in chloroform during crystallization simulation studies indicated faster aggregation in non-polar solvents. Aspect ratio, flow, compressibility and surface area of recrystallized products were also determined. Surface topography was determined by atomic force microscopy and the lath-shaped crystals (aspect ratio of 2-4) exhibited a roughness index of 1.79 in comparison with 2.92 for needles. Overall, the lath-shaped isomorphs exhibited improved flow and better compressibility.

A bioconjugate of Pseudomonas cepacia lipase with alginate with enhanced catalytic efficiency.

A bioconjugate of Pseudomonas cepacia lipase with alginate was prepared by simple adsorption. Atomic force microscope (AFM) images showed that this bioconjugate resulted from adsorption rather than entrapment of the enzyme as enzyme molecules were visible on the gel surface. The soluble bioconjugate exhibited increased enzyme activity in terms of high effectiveness factor (effectiveness factor was 3 for the immobilized preparation) and greater Vmax/Km value (Vmax/Km increased 25 times upon immobilization). This constitutes one of the less frequently observed instances of lipase activation by lid opening as a result of binding to a predominantly hydrophilic molecule. The bioconjugate was also more stable at 55 degrees C as compared to the free enzyme and could be reused for oil hydrolysis up to 4 cycles without any loss in activity. Fluorescence emission spectroscopy showed that the immobilized enzyme had undergone definite conformational changes.

Structural transition in nanostructured Eu2O3 under high pressures.

We report here studies on the effect of high pressure on the structural properties of nano-sized Europium sesquioxide (Eu2O3) up to a pressure of about 16.4 GPa. At ambient conditions, the starting sample was found to be predominantly cubic type Eu2O3 or in Eu3+ state with a trace of Eu2+. The presence of Eu2+ state is assumed to be arising due to the non-stoichiometric Eu(1-x)O phase which is obtained from XPS studies by the deconvolution of the Eu 3d-core levels. The Raman studies at ambient show a strong peak at about 333 cm(-1), which is known to occur due to the Fg mode of cubic Eu2O3 and in a similar way, the XRD data shows major peaks corresponding to the cubic phase of Eu2O3. A Mao-Bell type diamond anvil cell (DAC) was used to generate high pressures for XRD and Raman spectroscopy studies. It was observed that the material undergoes a structural change from cubic to monoclinic structure with an on set transition pressure at around 2 GPa and completes at around 8 GPa. This has been inferred from the fact that above about 2.0 GPa pressure, Raman studies show the emergence of a new peak corresponding to the monoclinic phase which increases in intensity and shifts further with increase in pressure, while the XRD studies show that above about 2.0 GPa, the peaks corresponding to monoclinic phase emerge, which show a slight increase in preferred orientation as the pressure is increased. A detailed discussion has been provided to explain this fact.