中国物理B ›› 2022, Vol. 31 ›› Issue (4): 40706-040706.doi: 10.1088/1674-1056/ac4a70

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High-precision nuclear magnetic resonance probe suitable for in situ studies of high-temperature metallic melts

Ao Li(李傲)1,2,†, Wei Xu(许巍)1,†,‡, Xiao Chen(陈霄)1,†, Bing-Nan Yao(姚冰楠)1, Jun-Tao Huo(霍军涛)1, Jun-Qiang Wang(王军强)1,2,§, and Run-Wei Li(李润伟)1,2   

  1. 1 CAS Key Laboratory of Magnetic Materials and Devices, and Zhejiang Province Key Laboratory of Magnetic Materials and Application Technology, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China;
    2 Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China
  • 收稿日期:2021-12-10 修回日期:2022-01-09 接受日期:2022-01-12 出版日期:2022-03-16 发布日期:2022-03-25
  • 通讯作者: Wei Xu, Jun-Qiang Wang E-mail:weixu@nimte.ac.cn;jqwang@nimte.ac.cn
  • 基金资助:
    Project supported by the Instrument Developing Project of the Chinese Academy of Sciences (Grant No. YZ201639), the National Key R&D Program of China (Grant No. 2018YFA0703604), the National Natural Science Foundation of China (Grant Nos. 51922102, 92163108, and 52071327), and the Zhejiang Provincial Natural Science Foundation of China (Grant No. LR18E010002).

High-precision nuclear magnetic resonance probe suitable for in situ studies of high-temperature metallic melts

Ao Li(李傲)1,2,†, Wei Xu(许巍)1,†,‡, Xiao Chen(陈霄)1,†, Bing-Nan Yao(姚冰楠)1, Jun-Tao Huo(霍军涛)1, Jun-Qiang Wang(王军强)1,2,§, and Run-Wei Li(李润伟)1,2   

  1. 1 CAS Key Laboratory of Magnetic Materials and Devices, and Zhejiang Province Key Laboratory of Magnetic Materials and Application Technology, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China;
    2 Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2021-12-10 Revised:2022-01-09 Accepted:2022-01-12 Online:2022-03-16 Published:2022-03-25
  • Contact: Wei Xu, Jun-Qiang Wang E-mail:weixu@nimte.ac.cn;jqwang@nimte.ac.cn
  • Supported by:
    Project supported by the Instrument Developing Project of the Chinese Academy of Sciences (Grant No. YZ201639), the National Key R&D Program of China (Grant No. 2018YFA0703604), the National Natural Science Foundation of China (Grant Nos. 51922102, 92163108, and 52071327), and the Zhejiang Provincial Natural Science Foundation of China (Grant No. LR18E010002).

摘要: High-temperature nuclear magnetic resonance (NMR) has proven to be very useful for detecting the temperature-induced structural evolution and dynamics in melts. However, the sensitivity and precision of high-temperature NMR probes are limited. Here we report a sensitive and stable high-temperature NMR probe based on laser-heating, suitable for in situ studies of metallic melts, which can work stably at the temperature of up to 2000 K. In our design, a well-designed optical path and the use of a water-cooled copper radio-frequency (RF) coil significantly optimize the signal-to-noise ratio (S/NR) at high temperatures. Additionally, a precise temperature controlling system with an error of less than ±1 K has been designed. After temperature calibration, the temperature measurement error is controlled within ±2 K. As a performance testing, 27Al NMR spectra are measured in Zr-based metallic glass-forming liquid in situ. Results show that the S/NR reaches 45 within 90 s even when the sample's temperature is up to 1500 K and that the isothermal signal drift is better than 0.001 ppm per hour. This high-temperature NMR probe can be used to clarify some highly debated issues about metallic liquids, such as glass transition and liquid-liquid transition.

关键词: high-temperature NMR probe, laser beams, temperature measurement, metallic melts

Abstract: High-temperature nuclear magnetic resonance (NMR) has proven to be very useful for detecting the temperature-induced structural evolution and dynamics in melts. However, the sensitivity and precision of high-temperature NMR probes are limited. Here we report a sensitive and stable high-temperature NMR probe based on laser-heating, suitable for in situ studies of metallic melts, which can work stably at the temperature of up to 2000 K. In our design, a well-designed optical path and the use of a water-cooled copper radio-frequency (RF) coil significantly optimize the signal-to-noise ratio (S/NR) at high temperatures. Additionally, a precise temperature controlling system with an error of less than ±1 K has been designed. After temperature calibration, the temperature measurement error is controlled within ±2 K. As a performance testing, 27Al NMR spectra are measured in Zr-based metallic glass-forming liquid in situ. Results show that the S/NR reaches 45 within 90 s even when the sample's temperature is up to 1500 K and that the isothermal signal drift is better than 0.001 ppm per hour. This high-temperature NMR probe can be used to clarify some highly debated issues about metallic liquids, such as glass transition and liquid-liquid transition.

Key words: high-temperature NMR probe, laser beams, temperature measurement, metallic melts

中图分类号:  (Submillimeter wave, microwave and radiowave spectrometers; magnetic resonance spectrometers, auxiliary equipment, and techniques)

  • 07.57.Pt
61.25.Mv (Liquid metals and alloys) 76.60.-k (Nuclear magnetic resonance and relaxation)