The photoelectrochemical response of nanoporous films, obtained by anodization of Ti and W substrates in a variety of corrosive media and at preselected voltages in the range from 10 to 60 V, was studied. The as-deposited films were subjected to thermal anneal and characterized by scanning electron microscopy and X-ray diffraction. Along with the anodization media developed by previous authors, the effect of poly(ethylene glycol) (PEG 400) or D-mannitol as a modifier to the NH4F electrolyte and glycerol addition to the oxalic acid electrolyte was studied for TiO2 and WO3, respectively. In general, intermediate anodization voltages and film growth times yielded excellent-quality photoelectrochemical response for both TiO2 and WO3 as assessed by linear-sweep photovoltammetry and photoaction spectra. The photooxidation of water and formate species was used as reaction probes to assess the photoresponse quality of the nanoporous oxide semiconductor films. In the presence of formate as an electron donor, the incident photon to electron conversion efficiency (IPCE) ranged from approximately 130% to approximately 200% for both TiO2 and WO3 depending on the film preparation protocol. The best photoactive films were obtained from poly(ethylene glycol) (PEG 400) containing NH4F for TiO2 and from aqueous NaF for WO3.

Traditional single-fiber pull-out type experiments were conducted on individual multiwalled carbon nanotubes (MWNT) embedded in an epoxy matrix using a novel technique. Remarkably, the results are qualitatively consistent with the predictions of continuum fracture mechanics models. Unstable interface crack propagation occurred at short MWNT embedments, which essentially exhibited a linear load-displacement response prior to peak load. Deep embedments, however, enabled stable crack extension and produced a nonlinear load-displacement response prior to peak load. The maximum pull-out forces corresponding to a wide range of embedments were used to compute the nominal interfacial shear strength and the interfacial fracture energy of the pristine MWNT-epoxy interface.

We report on the development and application of a silicon microdevice for the in situ quantitative mechanical characterization of single 1-D nanomaterials within a scanning electron microscope equipped with a quantitative nanoindenter. The design makes it possible to convert a compressive nanoindentation force applied to a shuttle to uniaxial tension on a specimen attached to a sample stage. Finite-element analysis and experimental calibration have been employed to extract the specimen stress versus strain curve from the indentation load versus displacement curve. The stress versus strain curves for three 200-300-nm-diameter Ni nanowire specimens are presented and analyzed.[2009-0271]

In this paper, we have demonstrated the usage of a novel micro-mechanical device (MMD) to perform quantitative in situ tensile tests on individual metallic nanowires inside a transmission electron microscope (TEM). Our preliminary experiment on a 360 nm diameter nickel nanowire showed that the sample fractured at an engineering stress of ∼ 1.2 GPa and an engineering strain of ∼ 4%, which is consistent with earlier experiments performed inside a scanning electron microscope (SEM). With in situ high resolution TEM imaging and diffraction capabilities, this novel experimental set-up could provide unique opportunities to reveal the underlying deformation and damage mechanisms for metals at the nanoscale.

A novel micromechanical device was developed to convert the compressive force applied by a nanoindenter into pure tensile loading at the sample stages inside a scanning electron microscope or a transmission electron microscope, in order to mechanically deform a one-dimensional nanostructure, such as a nanotube or a nanowire. Force vs. displacement curves for samples with Young's modulus above a threshold value can be obtained independently from readings of a quantitative high resolution nanoindenter with considerable accuracy, using a simple conversion relationship. However, in-depth finite element analysis revealed the existence of limitations for the device when testing samples with relatively low Young's modulus, where forces applied on samples derived from nanoindenter readings using a predetermined force conversion factor will no longer be accurate. In this paper, we will demonstrate a multi-step method which can alleviate this problem and make the device capable of testing a wide range of samples with considerable accuracy.