ABSTRACT
In this work, we report on studies of graphene exposed to tritium gas in a controlled environment. The single layer graphene on a SiO2/Si substrate was exposed to 400 mbar of T2, for a total time of â¼55 h. The resistivity of the graphene sample was measured in situ during tritium exposure using the van der Pauw method. We found that the sheet resistance increases by three orders of magnitude during the exposure, suggesting significant chemisorption of tritium. After exposure, the samples were characterised ex situ via spatio-chemical mapping with a confocal Raman microscope, to study the effect of tritium on the graphene structure (tritiation yielding T-graphene), as well as the homogeneity of modifications across the whole area of the graphene film. The Raman spectra after tritium exposure were comparable to previously observed results in hydrogen-loading experiments, carried out by other groups. By thermal annealing we also could demonstrate, using Raman spectral analysis, that the structural changes were largely reversible. Considering all observations, we conclude that the graphene film was at least partially tritiated during the tritium exposure, and that the graphene film by and large withstands the bombardment by electrons from the ß-decay of tritium, as well as by energetic primary and secondary ions.
ABSTRACT
We have developed a new compact and cost-efficient Laser-Raman system for the simultaneous measurement of all six hydrogen isotopologues. The focus of this research was set on producing a tool that can be implemented in virtually any existing setup providing in situ process control and analytics. The "micro Raman (µRA)" system is completely fiber-coupled for an easy setup consisting of (i) a spectrometer/CCD unit, (ii) a 532 nm laser, and (iii) a commercial Raman head coupled with a newly developed, tritium-compatible all-metal sealed DN16CF flange/Raman window serving as the process interface. To simplify the operation, we developed our own software suite for instrument control, data acquisition, and data evaluation in real-time. We have given a detailed description of the system, showing the system's capabilities in terms of the lower level of detection, and presented the results of a dedicated campaign using the accurate reference mixtures of all of the hydrogen isotopologues benchmarking µRA against two of the most sensitive Raman systems for tritium operation. Due to its modular nature, modifications that allow for the detection of various other gas species can be easily implemented.
