Glasses are can serve as exceptionally tight hydrogen barriers e.g. used for hydrogen storage in micro glass containers or cover glasses in micro electronic systems. Respective glass development, however, requires precise measurements of minimal hydrogen permeability, PH2. Recent studies showed that PH2 can be measured down to 2 10-21 mol s-1 Pa-1m-1 by means of Vacuum Hot Extraction (VHE) powder methods [1]. In this respect the isothermal gas release from glass powder particles is fitted in terms of classical diffusion models assuming spherical particles of uniform size thus obtaining the hydrogen diffusion coefficient, DH2. PH2 is then given by D H2 × S H2, where hydrogen solubility, SH2, is obtained from VHE studies of glass powders exposed to hydrogen atmosphere for different exposure time and hydrogen pressure. Measurements of minimal values of hydrogen permeability, however, require a careful evaluation and error discussion of this method. Against that background, we modeled hydrogen degassing during heating and subsequent isothermal annealing of glass powder particles of different shape and particle size distribution by means of COMSOL Multiphysics® [2] and verified related effects on DH2 obtained by the VHE powder method.
Thermo Analytic Investigation of Hydrogen Effusion Behavior - Sensor Evaluation and Calibration
(2011)
The well established carrier gas analysis (CGA) method was used to test different hydrogen detectors comprising a thermal conductivity detector (TCD) and a metal oxide semiconducting (MOx) sensor. The MOx sensor provides high hydrogen sensitivity and selectivity, whereas the TCD exhibits a much shorter response time and a linear hydrogen concentration dependency. Therefore, the TCD was used for quantitative hydrogen concentration measurements above 50?µmol/mol. The respective calibration was made using N2/H2 gas mixtures. Furthermore, the hydrogen content and degassing behaviour of titanium hydride (TiH2-x) was studied. This material turned out to be a potential candidate for a solid sample calibration. Vacuum hot extraction (VHE) coupled with a mass spectrometer (MS) was then calibrated with TiH2-x as transfer standard. The calibration was applied for the evaluation of the hydrogen content of austenitic steel samples (1.4301) and the comparison of CGA-TCD and VHE-MS.