He jishu (Mar 2023)

In-situ high-temperature NMR spectroscopy and its applications in molten salt ionic structure studies

  • WU Huiyan,
  • YINGSU Junheng,
  • LIU Yiyang,
  • HUANG Hailong,
  • GE Min,
  • QIAN Yuan,
  • FU Xiaobin,
  • LIU Hongtao

DOI
https://doi.org/10.11889/j.0253-3219.2023.hjs.46.030605
Journal volume & issue
Vol. 46, no. 3
pp. 030605 – 030605

Abstract

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BackgroundMolten salt systems have been extensively applied in the generation of nuclear and solar energy owing to their excellent heat transfer and storage performance. Therefore, it is essential to explore their physical and chemical properties, which are largely determined by their composition and ionic structure. In this regard, high-temperature (HT) nuclear magnetic resonance (NMR) has been demonstrated as an effective solution for qualitative analysis. Due to the existence of vent holes on the top of the commercialized standard NMR sample cell, it is not suitable for the study of some volatile, toxic or radioactive molten salt systems.PurposeThis study aims to implement ceramic NMR sample cells that are suitable for different molten salt systems.MethodsFirstly, a novel sealed sample cell that meets the requirements of molten salt systems was designed and produced by using an inner tube comprising AlN, BN, and Al2O3 ceramic materials, and an outer tube composed of ZrO2 ceramic materials. Then, with KBr as the standard sample, temperature calibration for this sample cell was conducted on the basis of 79Br NMR method. Finally, LiCl-KCl two-component molten salt (59.2 mol% LiCl-40.8 mol% KCl, eutectic melting point 353 ℃) was selected for HT-NMR experiment to verify the accuracy of temperature calibration, and check the performance of the HT-NMR method.ResultsExperimental results show that the sample cells are applicable in molten salt systems at a maximum temperature of 700 ℃, which meets the detection requirements of most molten salt systems. Additionally, the measurement results of the 79Br chemical shift of the KBr samples and captured HT 35Cl NMR spectra of the LiCl-KCl molten salt verify the reliability of the sample cell.ConclusionsBased on the results, the HT-NMR (High Temperature NMR) sample cells proposed in this study can be widely applied in various fields when the molten salt system requirements are met.

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