A parallel high-sensitivity hydrogen sorption, and in situ Raman/IR emissivity measurement system has been developed using a stainless-steel sample cell with a sapphire window to act as a bridge between the PCT and optical measurements. The cell can be pressurized up to 4.5 MPa and heated up to 723 K. The system can measure small changes in hydrogen content, down to 0.5 μg, allowing for characterization of small quantities of powers and thin films. Hydrogen desorption in LiNH2 - LiBH4 - MgH2 nanocomposites has been studied by in-situ Raman and PCT measurement, while that of MgH2 powers and thin films has been studied by in-situ PCT and IR emissivity. In powder samples, qualitative trend is observed between changes in the Raman peak intensity/IR emissivity and the amount of hydrogen absorbed or desorbed.
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Chiu, C., Hattrick-Simpers, J.R., Heilweil, E.J. et al. Development of Combined Optical Cell and Sieverts-type Apparatus for in-situ Measurement of Hydrogen Storage Materials. MRS Online Proceedings Library 1216, 832 (2009). https://doi.org/10.1557/PROC-1216-W08-32