锆石环氧树脂靶表面形貌特征及对LA-ICP-MS分析影响研究

胡志中; 王坤阳; 晏雄; 杨波; 杜谷

doi:10.15898/j.cnki.11-2131/td.201909210135

锆石环氧树脂靶表面形貌特征及对LA-ICP-MS分析影响研究

中国地质调查局成都地质调查中心, 四川成都 610081

详细信息

作者简介: 胡志中, 硕士, 工程师, 主要从事微区原位分析。E-mail:hzz_pot@aliyun.com

通讯作者: 杜谷, 硕士, 教授级高级工程师, 主要从事岩石、矿物分析研究。E-mail:dugucgs@163.com

中图分类号: O657.63

收稿日期: 2019-09-21

修回日期: 2020-02-07

录用日期: 2020-05-13

Study on the Morphology of Zircon-bearing Epoxy Resin Surface and Its Effect for LA-ICP-MS Analysis

Chengdu Center of Geological Survey, China Geological Survey, Chengdu 610081, China

More Information

Corresponding author: Gu DU, dugucgs@163.com

Received Date: 21 September 2019

Revised Date: 07 February 2020

Accepted Date: 13 May 2020

摘要

摘要: 激光剥蚀电感耦合等离子体质谱（LA-ICP-MS）是目前锆石研究常用方法之一，该法普遍采用环氧树脂靶为载体，对锆石环氧树脂靶表面形貌及平整度影响进行研究，有助于评估其制作工艺以及LA-ICP-MS锆石分析的准确性。本次研究采用原子力显微镜（AFM）对锆石环氧树脂靶表面进行形貌分析，并通过分析和对比193nm激光不同剥蚀模式和不同剥蚀条件下的锆石表面形貌，研究锆石表面形貌及平整度对LA-ICP-MS锆石分析的影响；同时实验采用氩离子抛光技术对锆石环氧树脂靶进行二次抛光，并探讨该技术对锆石环氧树脂靶影响。实验结果表明本次靶中表面总体平整性较好但存在细微的不平，锆石表面存在程度较小（几至几十纳米的不等）的擦痕，锆石颗粒边缘与靶面存在高差和间隙；而通过研究后认为锆石表面细微的不平对于分析的影响小于能量密度、频率、移动速率等其他激光参数的影响，对分析准确性的影响较小。实验分析并对比了锆石和玻璃标准等不同基体的线扫描形貌，发现其剥蚀深度以及剥蚀形貌存在差异，相同剥蚀条件下线扫描剥蚀深度：NIST610 > CGSG系列>锆石91500。经氩离子二次抛光后锆石样品表面擦痕不明显，但可能会对锆石造成损伤等影响。本次研究认为锆石环氧树脂靶表面总体平整性较好，锆石表面细微的不平对分析准确性的影响较小，不同基体的线扫描形貌研究则为LA-ICP-MS锆石及其他分析提供了参考，而氩离子抛光技术对LA-ICP-MS分析的影响及应用还有待进一步的研究。
- 锆石环氧树脂靶 /
- 原子力显微镜 /
- 氩离子抛光技术 /
- 表面形貌 /
- 激光剥蚀电感耦合等离子体质谱法
Abstract: BACKGROUNDLaser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is currently one of the commonly used methods for zircon research. This method generally uses epoxy resin targets as carriers. Studying the effect of the surface morphology and flatness of epoxy resin targets helps to evaluate its production process and the accuracy of LA-ICP-MS zircon analysis. OBJECTIVESTo study the influence of the surface morphology of epoxy resin for zircon analysis by LA-ICP-MS. METHODSAtomic force microscope (AFM) was used to analyze the surface morphology of zircon epoxy resin target, and the zircon surface morphology was studied by analyzing and comparing the zircon surface morphology under different ablation modes and different ablation conditions of 193nm laser. The influence of flatness on LA-ICP-MS zircon analysis was discussed. Argon ion polishing technology was used to perform secondary polishing on the zircon epoxy resin target, and the influence of this technology on the zircon epoxy resin target was investigated. RESULTSThe surface of the zircon epoxy resins was generally smooth but slightly uneven. There were scratches from a few to tens nm on the surface of the zircon. The differences in height and gaps existed between zircons and epoxy resin. The slightly uneven surface had less impact on the analysis accuracy than other laser parameters such as energy density, frequency and movement rate. The depth and morphology of different matrices by linear scanning were dissimilar. The scanning depths on the NIST610, CGSG series, zircon 91500 decreased under the same laser condition. The scratches of zircon surface were not obvious after Ar-ion milling, but the zircons may have been damaged. CONCLUSIONSThe surface morphology of zircon epoxy resins has less impact on the analysis accuracy for LA-ICP-MS. The influence and application of Ar-ion milling for LA-ICP-MS needs further study.
- zircon in epoxy resin /
- atomic force microscope /
- the Ar-ion milling technology /
- the morphology of surface /

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图 1 锆石颗粒和树脂靶表面的形貌图

Figure 1.

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图 2 不同点剥蚀条件下锆石91500剥蚀坑的形貌图

Figure 2.

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图 3 不同线扫描条件下锆石91500剥蚀坑的形貌图

Figure 3.

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图 4 CGSG系列线扫描剥蚀坑的形貌图

Figure 4.

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图 5 经氩离子抛光后页岩和锆石表面的形貌图

Figure 5.

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图 6 氩离子抛光前后的锆石阴极发光图及抛光后反射光图像

Figure 6.

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表 1 点剥蚀不同条件下锆石91500的剥蚀深度

Table 1. Depth of pits in zircon 91500 under different ablation conditions

锆石91500的剥蚀条件	剥蚀次数	深度范围 (nm)	平均深度 (nm)
16μm，3J/cm²，10Hz	1	19~29	24
16μm，3J/cm²，10Hz	5	130~155	143
16μm，3J/cm²，10Hz	10	138~197	168
16μm，3J/cm²，10Hz	15	326~369	348
16μm，3J/cm²，10Hz	20	584~668	626
16μm，6J/cm²，5Hz	250	6215~6291	6253

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表 2 不同基体线扫描的剥蚀深度

Table 2. Depth of pits with different sample matrixes by linear scanning

标准样品	剥蚀条件	平均剥蚀深度 (nm)
CGSG-1	16μm，10Hz，1μm/s	6929
CGSG-2	16μm，10Hz，1μm/s	7064
CGSG-4	16μm，10Hz，1μm/s	6139
CGSG-5	16μm，10Hz，1μm/s	6400
锆石91500	16μm，10Hz，1μm/s	5713
NIST610	16μm，10Hz，1μm/s	＞7668
注：NIST610标准样品的数据来自文献[36]。

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