Hashimoto S, Noda Y, Maekawa H, Takamura H, Fujito T, Moriya J, Ikeda T
Department of Materials Science, Graduate School of Engineering, Tohoku University, 6-6-11-301-2 Aramaki Aoba, Sendai 980-8579, Japan.
Rev Sci Instrum. 2010 Oct;81(10):104101. doi: 10.1063/1.3484282.
A NMR system for in situ analysis of hydrogen storage materials under high pressure and temperature conditions was developed. The system consists of a gas pressure and flow rate controlling unit, a temperature controller, a high temperature NMR probe tunable for both (1)H and other nuclei, and a sample tube holder. Sample temperature can be controlled up to 623 K by heated N(2) gas flow. Sample tube atmosphere can be substituted by either H(2) or Ar and can be pressurized up to 1 MPa under constant flow rate up to 100 ml/min. During the NMR measurement, the pressure can be adjusted easily by just handle a back pressure valve. On the blank NMR measurement, (1)H background noise was confirmed to be very low. (1)H and (11)B NMR spectrum of LiBH(4) were successfully observed at high temperature for the demonstration of the system. The intensity of the (1)H NMR spectra of H(2) gas was also confirmed to be proportional to the applied pressure.
