材料中氢同位素行为热脱附谱实验方法研究

夏体锐; 杨洪广; 占勤; 韩志博; 何长水

doi:10.7538/yzk.2012.46.suppl.0510

材料中氢同位素行为热脱附谱实验方法研究

中国原子能科学研究院,北京102413

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- 刊出日期: 2012-09-19

Thermal Desorption Spectroscopy for Investigating Hydrogen Isotope Behavior in Materials

China Institute of Atomic Energy, Beijing 102413, China

摘要

摘要: 材料中氢同位素行为研究是确保聚变堆安全和经济性的关键问题和重要研究方向。为研究材料中氢同位素的扩散、释放、居留等特性，建立了一种联合四极质谱仪（QMS）的热脱附谱（TDS）实验方法，解决了TDS系统超高真空、低氢同位素质谱本底、线性升温速率控制以及灵敏度标定等关键科学技术问题。通过涡轮分子泵和二级溅射离子泵实现了优于1×10^-7Pa的超高真空，本底H₂分压降至1×10^-9Pa。通过MCGS直流PID控温程序实现样品升温速率在1～100 K/min范围可调，采用漏率可变的特制通导型玻璃漏孔标定TDS系统的氘气脱附速率灵敏度，确定该灵敏度系数α和最小可检测氘气热脱附速率（脱附速率灵敏度）分别为6.22×10²⁴s^-1·A^-1、1.24×10^-10s^-1。采用镀镍Zr-4合金吸氘样品验证了TDS方法的有效性，初步分析了Zr-4中的氘热脱附特性。

关键词:
材料 ,

氢同位素行为 ,

热脱附谱
Abstract: The behavior of hydrogen isotope generated in fusion reactor materials is the key issue for safety and economic operation of fusion reactors and becomes an interesting field. In order to investigate the mechanism of hydrogen isotope such as diffusion, release and retention, a high-sensitivity thermal desorption spectroscopy (TDS) in combination with a quadruple mass spectrometer (QMS) was developed. A major technical breakthrough in ultrahigh vacuum (UHV), low hydrogen background, linear heating and sensitivity calibration of TDS system was made. UHV of 1×10^-7 Pa and low hydrogen background of 1×10^-9 Pa were obtained by combining turbo molecule pump and sputter ion pump. Specimens can be linearly heated up to 1 173 K at the rate of 1 to 50 K/min under the MCGS PID software. Sensitivity calibration of the TDS system was accomplished using a special deuterium leak in the detector mode of QMS second electron multiplie. The desorption sensitivity coefficient and the minimum detection limit of deuterium desorption rate are 6.22×10²⁴s^-1·A^-1 and 1.24×10^-10s^-1, respectively. The measurement was also routinely conducted on a specimen of standard, deuterium containing Zr-4 alloy maintained in the laboratory, so as to validate the TDS method.

Keywords:
materials ,

hydrogen isotope behavior ,

thermal desorption spectroscopy

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参考文献(12)

[1] POITEVIN Y, BOCCACCINIB L V, DELL’ORCO G, et al. The test blanket modules project in Europe: From the strategy to the technical plan over next 10 years[J]. Fusion Eng Des, 2007, 82(15-24): 2164-2170.

[2] MUNAKATA K, SHINOZAKIA T, INOUE K, et al. Tritium release from lithium silicate pebbles produced from lithium hydroxide[J]. Fusion Eng Des, 2008, 83(7-9): 1317-1320.

[3] 杨本福，曹小华，罗顺忠. 用热解吸法研究锂陶瓷中氚扩散行为[J]. 核技术,2001,24(3):21-325.YANG Benfu, CAO Xiaohua, LUO Shunzhong. A study on tritium releasing behavior from lithium ceramics by thermo-desorption method[J]. Nucl Tech, 2004, 24(4): 321-326(in Chinese).

[4] NICHOLL S I, TALLEY J W. Development of thermal programmed desorption mass spectrometry methods for environment applications[J]. J Chemosphere, 2006, 63(1): 132-141.

[5] TAKUJI O, YASUHISA O. Thermal desorption behavior of hydrogen isotopes: Interacting with radiation defects in Li₂O[J]. Fusion Eng Des, 2005, 75-79(Suppl.): 835-839.

[6] ZHU Deqiong, TAKUJI O, SATORU T. Effect of grain size on hydrogen isotope behavior in LiNbO₃[C]∥Proceedings of 9^th Tritium Science and Technology. Japan: National Institute for Fusion Science (NIFS), 2011.

[7] ZHU Deqiong. Behavior of hydrogen isotopes in ternary lithium oxides as a function of grain size[C]∥Proceedings of the 3^rd China-Japan Workshop on the Tritium and Breeding Blanket Technology. Kunming, China: Southwestern Institute of Physics, 2010.

[8] 刘超卓. 含氦钛膜的制备、表征及退火行为研究[D]. 上海：复旦大学现代物理研究所，2007.

[9] 汪小琳. 国防科学研究中的核化学与放射化学进展[J]. 核化学与放射化学，2009，31（增刊）：64-74.WANG Xiaolin. Progress on nuclear and radiochemistry in the scientific research of national defense[J]. Journal of Nuclear and Radiochemistry, 2009, 31(Suppl.): 64-73(in Chinese).

[10] 程贵钧，王维笃，杨本福，等. 金属氚化物中³He的热解吸方法[J]. 原子能科学技术,2005,39(4):372-376.CHENG Guijun, WANG Weidu, YANG Benfu, et al. Thermo-desorption method for ³He release from metal tritides[J]. Atomic Energy Science and Technology, 2005, 39(4): 372-376(in Chinese).

[11] ALVANI C, CASADIO S, CASADIO S. Kinetics of tritium release from irradiated Li₂TiO₃ pebbles in out-of-pile TPD tests[J]. Fusion Eng Des, 2003, 69(1-4): 275-280.

[12] OLIVER B M, GARNER F A, GREENWOOD L R, et al. High-sensitivity quadrupole mass spectrometry system for the determination of hydrogen in irradiated materials[J]. J Nucl Mater, 2000, 283-287(2): 1006-1010.

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计量

文章访问数: 692

HTML全文浏览量: 4

PDF下载量: 1883

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刊出日期: 2012-09-19

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[1]	POITEVIN Y, BOCCACCINIB L V, DELL’ORCO G, et al. The test blanket modules project in Europe: From the strategy to the technical plan over next 10 years[J]. Fusion Eng Des, 2007, 82(15-24): 2164-2170.
[2]	MUNAKATA K, SHINOZAKIA T, INOUE K, et al. Tritium release from lithium silicate pebbles produced from lithium hydroxide[J]. Fusion Eng Des, 2008, 83(7-9): 1317-1320.
[3]	杨本福，曹小华，罗顺忠. 用热解吸法研究锂陶瓷中氚扩散行为[J]. 核技术,2001,24(3):21-325.YANG Benfu, CAO Xiaohua, LUO Shunzhong. A study on tritium releasing behavior from lithium ceramics by thermo-desorption method[J]. Nucl Tech, 2004, 24(4): 321-326(in Chinese).
[4]	NICHOLL S I, TALLEY J W. Development of thermal programmed desorption mass spectrometry methods for environment applications[J]. J Chemosphere, 2006, 63(1): 132-141.
[5]	TAKUJI O, YASUHISA O. Thermal desorption behavior of hydrogen isotopes: Interacting with radiation defects in Li₂O[J]. Fusion Eng Des, 2005, 75-79(Suppl.): 835-839.
[6]	ZHU Deqiong, TAKUJI O, SATORU T. Effect of grain size on hydrogen isotope behavior in LiNbO₃[C]∥Proceedings of 9^th Tritium Science and Technology. Japan: National Institute for Fusion Science (NIFS), 2011.
[7]	ZHU Deqiong. Behavior of hydrogen isotopes in ternary lithium oxides as a function of grain size[C]∥Proceedings of the 3^rd China-Japan Workshop on the Tritium and Breeding Blanket Technology. Kunming, China: Southwestern Institute of Physics, 2010.
[8]	刘超卓. 含氦钛膜的制备、表征及退火行为研究[D]. 上海：复旦大学现代物理研究所，2007.
[9]	汪小琳. 国防科学研究中的核化学与放射化学进展[J]. 核化学与放射化学，2009，31（增刊）：64-74.WANG Xiaolin. Progress on nuclear and radiochemistry in the scientific research of national defense[J]. Journal of Nuclear and Radiochemistry, 2009, 31(Suppl.): 64-73(in Chinese).
[10]	程贵钧，王维笃，杨本福，等. 金属氚化物中³He的热解吸方法[J]. 原子能科学技术,2005,39(4):372-376.CHENG Guijun, WANG Weidu, YANG Benfu, et al. Thermo-desorption method for ³He release from metal tritides[J]. Atomic Energy Science and Technology, 2005, 39(4): 372-376(in Chinese).
[11]	ALVANI C, CASADIO S, CASADIO S. Kinetics of tritium release from irradiated Li₂TiO₃ pebbles in out-of-pile TPD tests[J]. Fusion Eng Des, 2003, 69(1-4): 275-280.
[12]	OLIVER B M, GARNER F A, GREENWOOD L R, et al. High-sensitivity quadrupole mass spectrometry system for the determination of hydrogen in irradiated materials[J]. J Nucl Mater, 2000, 283-287(2): 1006-1010.