通过 EDXS 进行轻元素(C、N、O)定量:应用于陨石含水量和有机成分。

IF 2.9 4区 工程技术 Q3 MATERIALS SCIENCE, MULTIDISCIPLINARY Microscopy and Microanalysis Pub Date : 2024-08-21 DOI:10.1093/mam/ozae071
Corentin Le Guillou, Pierre-Marie Zanetta, Hugues Leroux, Anne-Marie Blanchenet, Maya Marinova
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引用次数: 0

摘要

在透射电子显微镜(TEM)中对碳、氮和氧等轻元素进行定量是一项极具挑战性的任务,但在生物、材料或地球和行星科学领域却是必不可少的。我们开发了一种方法,利用灵敏的无窗硅漂移探测器和自制的 Python 高光谱数据处理例程,通过能量色散 X 射线光谱(EDXS)进行精确定量。使用楔形聚焦离子束截面测定 K 因子。为校正样品内部的 X 射线吸收,采用重温两线法(Morris,1980 年)确定样品质量厚度。无需测量束流。将此方法应用于铁的 K 线和 L 线时,我们发现铁 L 线能量处的表列质量吸收系数过低。这是由于铁边缘的 X 射线自吸收造成的。我们利用参考材料,通过实验确定了一个能给出预期结果的吸收系数。然后,我们分析了 Orgueil 陨石中复杂的植硅酸盐混合物。我们的研究表明,有机物的氮/碳比率可以精确到优于 5%,氧气的定量也足够精确,足以推断出植硅酸盐的羟基含量。
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Light Element (C, N, O) Quantification by EDXS: Application to Meteorite Water Content and Organic Composition.

Quantifying light elements such as carbon, nitrogen, and oxygen in a transmission electron microscope (TEM) is a challenging however essential task in biology, materials, or earth and planetary sciences. We have developed an approach that allows precise quantification by energy-dispersive X-ray spectroscopy (EDXS), using sensitive windowless silicon drift detectors and homemade Python routines for hyperspectral data processing. K-factors were determined using wedge-shaped focused ion beam sections. To correct for X-ray absorption within the sample, the sample mass thickness is determined by the-revisited-two-lines method (Morris, 1980). No beam current measurement is required. Applying this method to the K and L lines of iron, we found that the tabulated mass absorption coefficient at the energy of the iron L lines was too low. This is due to X-ray self-absorption at the iron edge. Using reference material, we experimentally determined an absorption coefficient that gave the expected results. We then analyzed the complex phyllosilicate mixture of the Orgueil meteorite. We show that the N/C ratio of organics can be obtained with an accuracy better than 5 at.% and that oxygen can be quantified accurately enough to infer the hydroxyl content of phyllosilicates.

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来源期刊
Microscopy and Microanalysis
Microscopy and Microanalysis 工程技术-材料科学:综合
CiteScore
1.10
自引率
10.70%
发文量
1391
审稿时长
6 months
期刊介绍: Microscopy and Microanalysis publishes original research papers in the fields of microscopy, imaging, and compositional analysis. This distinguished international forum is intended for microscopists in both biology and materials science. The journal provides significant articles that describe new and existing techniques and instrumentation, as well as the applications of these to the imaging and analysis of microstructure. Microscopy and Microanalysis also includes review articles, letters to the editor, and book reviews.
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