ABSTRACT
We present the design and construction of a high-pressure (200 bars) and high-temperature (600 °C) x-ray diffraction (XRD) cell for the in situ investigation of the hydrogen sorption of hydrides. In combination with a pressure, composition, and temperature system, simultaneous XRD and volumetric measurements become accessible. The cell consists of an x-ray semi-transparent hemispherical beryllium (Be) dome covering a heatable sample stage, which simultaneously allows sample temperatures of up to 600 °C in an applied hydrogen atmosphere of up to 200 bars. The system volume is as low as possible to maximize the precision of the volumetric measurements. Due to the high thermal conductivity of hydrogen, and in order to preserve the mechanical stability of the beryllium, the cell is water cooled. Its operability was studied on the example of the hydrogen absorption of Mg(2)Ni. The advantages and limitations of the proposed design are discussed.
ABSTRACT
The design and construction of a high-pressure (200 bar) and high-temperature (600 degrees C) heat-flow differential scanning calorimeter (DSC) for the in situ investigation of the hydrogenation and dehydrogenation reactions of hydrides is presented. In combination with a pressure-concentration-temperature (pcT) system, simultaneous thermodynamic and volumetric measurements become accessible. Due to the high thermal conductivity of hydrogen, only the sample cell and the reference cell are exposed to hydrogen and the remaining system is under ambient conditions. This separation has the advantage that the calibration factor is independent of the hydrogen pressure. The internal empty volume of the combined system is as low as possible to maximize the precision of the pcT measurements. The calorimetric block of the DSC is designed with a silver/copper alloy and the temperature measurements are made resistively with platinum temperature sensors (Pt 100). The instrument was calibrated and its operability was successfully studied on the example of the hydrogen sorption behavior of LaNi(5).
ABSTRACT
The dehydriding reaction of single-phase alpha- AlH3 was investigated by in situ microscopic observations combined with thermal and surface analyses. Before the dehydriding reaction, primary AlH3 particles of size 100 nm-1 microm were thought to be covered by an oxide layer with a thickness of less than 5 nm. Both the precipitation/grain-growth of metallic Al of size 1-50 nm and an increase in 'boundary space' were clearly observed inside the particles, while the morphologies of the particles covered by the layer did not change during the dehydriding reaction. This preliminary report provides fundamental information for a further study of AlH3 as a possible hydrogen storage material.
Subject(s)
Aluminum/chemistry , Crystallization/methods , Hydrogen/chemistry , Hydrogen/isolation & purification , Nanostructures/chemistry , Nanostructures/ultrastructure , Nanotechnology/methods , Computer Simulation , Macromolecular Substances/chemistry , Materials Testing , Models, Chemical , Molecular Conformation , Particle Size , Surface PropertiesABSTRACT
The adsorption of protein A on silicon surfaces was studied by atomic force microscopy (AFM) and X-ray photoelectron spectroscopy. The deposition was made statically from various concentrations of protein A in water solution. The biological activity was checked by the immobilization of rabbit immunoglobulin G. The protein adsorption occurs in least two different phases and leads to a multilayer film. The first monolayer of proteins is rapidly adsorbed on the surface. The adsorption of the second layer of proteins occurs much more slowly (a thousand times slower) and also involves the third monolayer. The protein A of the first monolayer is denaturated and biologically inactive. On the contrary, the proteins of the second monolayer keep their natural diameter and remain biologically active. AFM artifacts such as the convolution with small objects and the resulting estimation of the coverage ratio are discussed. Copyright 2001 Academic Press.
