A novel sample preparation method for ultra-high vacuum (UHV) secondary ion mass spectrometry (SIMS) analysis
A novel sample preparation method for ultra-high vacuum (UHV) secondary ion mass spectrometry (SIMS) analysis
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一种用于超高真空 (UHV) 二次离子质谱 (SIMS) 分析的新型样品制备方法
DOI：
10.1039/c8ja00087e
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发表时间：
2018-08
影响因子：
3.4
通讯作者：
Yang Qing
中科院分区：
文献类型：
--
作者：
Zhang Wanfeng;Xia Xiaoping;Zhang Yanqiang;Peng Touping;Yang Qing
二次离子质谱（西姆斯）具有高灵敏度、高精度和原位微量分析能力，已被广泛应用于地球科学研究中各种物质的分析。该技术在超高真空（UHV）条件下运行，尤其适用于标称无水矿物（NAM）的含水量测量。然而，当使用环氧树脂底座时，UHV条件难以实现，环氧树脂底座在真空过程中容易脱气。在这项研究中，我们开发了一种新的样品制备方法，使用锡基合金代替环氧树脂。使用锡合金底座和自动液氮加注系统，结果表明真空条件从1.2 × 10−8 mbar显著改善到1.9 × 10−9 mbar。用安装在中国科学院广州地球化学研究所（GIGCAS）的CAMECA IMS 1280-HR西姆斯测量的矿泉水含量的本底降低到<10 ppm。此外，锡合金底座比铟底座更硬且更容易抛光，铟底座通常用于以前的UHV分析。对于锡合金镶嵌件，产生了<2 μm的起伏，这对于高精度同位素分析是必要的。氧同位素比值的常规外测精度优于0.15‰（1 SD），与环氧树脂固定片测量结果相当。
Secondary ion mass spectrometry (SIMS) has been applied to analyze a wide range of materials for earth science research due to its high sensitivity, high precision and capacity for in situ micro-analysis. This technique operates under ultra-high vacuum (UHV) conditions, especially for water content measurements on nominally anhydrous minerals (NAMs). However, UHV conditions are hard to achieve when using epoxy mounts, which degas readily during the vacuum processes. In this study, we developed a novel sample preparation method using a tin-based alloy instead of epoxy resin. Using a tin alloy mount coupled with an automatic liquid nitrogen refilling system, the results show that the vacuum conditions have been significantly improved from ∼1.2 × 10−8 mbar to ∼1.9 × 10−9 mbar. The background for mineral water content, measured with a CAMECA IMS 1280-HR SIMS installed at the Guangzhou Institute of Geochemistry, Chinese Academy of Sciences (GIGCAS), is lowered to <10 ppm. Moreover, tin alloy mounts are harder and easier to polish than indium mounts, which was commonly used for previous UHV analyses. A relief of <2 μm is yielded for tin alloy mounts, which is essential for high precision isotope analysis. Our results also show that the routine external precision of oxygen isotope ratios is better than 0.15‰ (1SD), comparable with that obtained using epoxy mounts.
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影响因子：
3.9
作者：
Hauri, E;Wang, JH;Newman, S
通讯作者：
Newman, S
影响因子：
3.4
作者：
M. Turner;T. Ireland;J. Hermann;P. Holden;J. Padrón-navarta;E. Hauri;S. Turner
通讯作者：
M. Turner;T. Ireland;J. Hermann;P. Holden;J. Padrón-navarta;E. Hauri;S. Turner
影响因子：
64.8
作者：
A. Peslier;A. Woodland;D. Bell;M. Lazarov
通讯作者：
A. Peslier;A. Woodland;D. Bell;M. Lazarov
影响因子：
3.9
作者：
Hauri, E
通讯作者：
Hauri, E
影响因子：
3.9
作者：
Kita, Noriko T.;Ushikubo, Takayuki;Valley, John W.
通讯作者：
Valley, John W.