Name: atom probe tomography analysis of exsolved mineral phases
Uploaded: 2019-10-25T12:30:00
Description: Watch this Scientific Journal Video about Atom Probe Tomography Analysis of Exsolved Mineral Phases at JoVE.com

这项工作得到了国家科学基金会（NSF）的资助，这些资金来自EAR-1560779和EAR-1647012，研究和经济发展副总裁办公室、艺术和科学学院以及地质科学系。作者还感谢奇亚拉·卡佩利、里奇·马滕斯和约翰尼·古德温提供技术援助，蒙特塞拉特火山观测站提供火山灰样本。

1. 矿物谷物的采购、选择和制备
注：样本取自蒙特塞拉特火山观测站（MVO）的目录收集，取自2009年10月5日发生苏弗里埃尔山火山剧烈火山灰喷发的沉积物;这是14日为期三天的13起类似事件之一。这次火山灰排泄之前，10月9日开始的熔岩圆顶生长（第5阶段）进入一个新的阶段。先前对这个样本的分析表明，它是密密圆顶岩石碎片、玻璃颗粒和意外...

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3D APT 数据重建允许以比传统 SEM 图像测量的分辨率高三个数量级的分辨率精确测量分析晶体中的层间间距。这表明，化学原子变化发生在空间范围内，比光学可观测矿物学变化小三个数量级。此外，测得的间层距离（29 nm 和 14 nm）与氧外溶液的长度刻度一致，而不是单独相的成核和生长，后者在长度上成尺度，数量级大于19 ，20.这里检查的钛铁磁铁矿?...

一个多世纪以来，化学矿物学研究一直是地球科学领域的主要信息来源，因为矿物在结晶期间和之后积极记录地质过程。这些过程的物理化学条件，如火山和变质期间的温度变化，在矿物成核和生长过程中记录，形式为化学宗化、条纹和层状，等等。当相位在固态中混合成两个单独的相位时，就形成解解层。分析这种外解层的方向、大小、形态和间距，可以为了解火山和变质过程中的温度和压力变化提供基本信息1、2、3和形成矿床4.
传统上，通过简单的扫描电子成像5对显微图的观察，对外解层进行研究。最近，这已被取代使用能量过滤传输电子显微镜（TEM）提供详细的观察在纳米尺度1，2，3。然而，在这两种情况下，观察都是两维（2D），对于由这些外解层表示的三维（3D）结构来说，这并不完全足够。纳米断层6正在成为矿物颗粒内纳米尺度特征的三维观测新技术，但关于这些特征的组成信息不足。这些方法的另一种方法是使用原子探针断层扫描（APT），代表了材料表征中存在的最高空间分辨率分析技术。该技术的优势在于，在原子尺度上，纳米尺度特征的三维重建与其化学成分相结合的可能性接近百万分之一的分析灵敏度7。以前APT在地质样品分析中的应用，在元素的化学表征方面，提供了优异的结果8、9、10、11。扩散和浓度9，12，13。然而，这一应用尚未用于研究在变质和成火岩中含有大量矿物质的外解层。在这里，我们探讨APT的使用，及其局限性，用于分析外溶液层的大小和组成，以及火山钛铁晶体中层间间距。

<table>
	<tbody>
		<tr>
			<td>InTouchScope Secondary Electron Microscope (SEM)</td>
			<td>JEOL</td>
			<td>JSM-6010PLUS/LA</td>
			<td></td>
		</tr>
		<tr>
			<td>Focus Ion Beam (FIB) Secondary Electron Microscope (SEM)</td>
			<td>TESCAN</td>
			<td>LYRA XMU</td>
			<td></td>
		</tr>
		<tr>
			<td>Local Electrode Atom Probe (LEAP)</td>
			<td>CAMECA</td>
			<td>5000 XS</td>
			<td></td>
		</tr>
		<tr>
			<td>Integrated Visualization and Analysis Software (IVAS, version 3.6.12).</td>
			<td></td>
			<td></td>
			<td>processing software</td>
		</tr>
	</tbody>
</table>

atom probe tomography analysis of exsolved mineral phases

元素扩散率和温度/压力控制一系列基本的火山和变质过程。这种过程通常记录在从宿主矿物相中分离的层状。因此，分析外解层的方向、大小、形态、组成和间距是地球科学中一个活跃的研究领域。通过扫描电子显微镜（SEM）和透射电子显微镜（TEM），以及最近基于聚焦电束（FIB）的纳米断层扫描，但化学信息有限，对这些层压进行常规研究。在这里，我们探讨使用原子探针断层扫描（APT）对从活跃的苏弗里埃尔山火山（英属西印度群岛蒙特塞拉特）喷发的火山灰沉积物中火石中除解的硅石的纳米级分析。APT 允许精确计算层间间距（14~29 ± 2 nm），并揭示平滑的扩散轮廓，在除露的层状和 Ti/O 之间交换 Fe 和 Ti/O 期间，没有尖锐的相位边界。我们的结果表明，这种新方法允许纳米级测量层状物组成和层间间距，这可能提供一种手段来估计模型挤出率和熔岩圆顶故障所需的熔岩圆顶温度，这两者都是在减轻火山灾害的努力中发挥关键作用。

与来自苏弗里埃尔火山（SHV）喷发不同阶段的许多钛铁磁铁晶体一样，这里分析的晶体含有外溶液层，厚度为<10 μm，在次生SEM图像（图1d）中可见，其中单独的区域富铁磁铁矿，表示C2级氧化18。根据 SEM 图像，这些层之间的间距范围为 2 到 6 μm（n = 15）。从该单晶中成功提取了四个钛铁石试样尖，分别称为207、217、218和219，并由APT进行分析（<strong cl...

Watch this Scientific Journal Video about Atom Probe Tomography Analysis of Exsolved Mineral Phases at JoVE.com

Atom Probe Tomography Analysis of Exsolved Mineral Phases

分析外解层的形态、组成和间距，可以为了解与火山和变质有关的地质过程提供基本信息。我们提出了APT在表征中的新应用，并将这种方法与电子显微镜和FIB纳米断层扫描的传统应用进行比较。

原子探针断层扫描分析的解脱矿物相

Element diffusion rates and temperature/pressure control a range of fundamental volcanic and metamorphic processes. Such processes are often recorded in ...

研究矿物化学的变化可以揭示火山活动的变化，使研究人员能够获得火山过程的时间尺度，以更好地了解任何潜在的危险。原子探针断层扫描允许在原子尺度测量矿物化学成分的同时，对矿物exsolvsolvex相进行前所未有的三D可视化。我们目前正在将这项技术应用于病理矿化的表征，例如肾结石。这种方法可以应用于火山系统，其中火山爆发过渡可能发生在小的时间尺度上。这些过渡记录在矿物中，空间尺度非常小。首先将一克样品倒入10厘米的玻璃培养皿中，然后将一张三厘米重的纸包裹在10高磁体周围。使用磁铁从灰烬样品中拉出直径在 100 到 500 微米的磁铁富颗粒，将颗粒放在直径为 32 微米、直径 8 厘米的不锈钢筛中。使用挤压瓶去电化水，通过筛子冲洗较小的附着灰颗粒 20 至 30 秒，让颗粒风干 24 小时。第二天，将任何清洁和干燥的灰烬颗粒贴在适合二次扫描电子显微镜的样品上，并在15至20千伏加速电压和工作距离为10毫米的二次电子模式下对粒子进行成像，以选择5至10个最佳候选物进行进一步分析。所选颗粒应主要是磁铁矿。将选定的灰粒贴在一块透明胶带上，然后用一英寸直径的空心模具环绕样品，该模子内部涂有真空润滑脂，然后用环氧树脂树脂模具填充模具。环氧树脂固化后，从模具中取出样品，然后从底部剥落胶带。灰粒应部分暴露。用五种不同砂砾尺寸的碳化硅研磨纸抛光环氧铸灰粒，从最高到最低的砂砾尺寸，每份研磨纸至少 10 分钟。在砂砾尺寸之间，在去维化水的浴中对样品进行声波化10分钟。每次最后一次抛光后，在显微镜下检查样品，以确保不存在抛光砂砾，并且样品表面没有划痕。接下来使用抛光布抛光环氧铸灰粒与连续1和0.3微米氧化铝抛光悬浮液在图8运动至少10分钟，在脱压水中的样品在悬浮液尺寸之间声波10分钟。第二次悬架抛光后，在显微镜下检查样品，以确保不存在悬浮液，并且样品表面没有划痕。在抛光过程结束时，环氧树脂表面应光滑，灰粒应平整且暴露良好。使用可用的溅射涂层装置，用大约 10 纳米厚的碳传导涂层覆盖样品表面，并使用电子显微镜以 15 到 20 千伏加速电压和 10 毫米的工作距离获得灰粒的背面散射电子图像，以确定磁石中脱毛层压层的位置。在开始聚焦离子束程序之前，溅射用 15 纳米的铜层对样品表面进行溅射，以避免电子充电和样品漂移。接下来，在双束扫描电子显微镜中使用聚焦的氦离子束，在30千伏和7帕斯卡的抛光部分上，该部分含有1.5至20微米区域的层压。使用离子束在铂矩形的三面下方碾磨三个材料楔块，然后插入气体喷射系统，使用气体喷射系统沉积铂金将楔块焊接到原位纳米操纵器上，然后切割最终边缘。使用氦离子束，从楔子上切割 10 个一到两千米宽的段，并依次将带铂金的楔块贴在微尖阵列优惠券的硅柱顶部。使用越来越小的内径和外径的环形铣削模式，从 30 千伏开始，以产生原子探针断层扫描所需的试样几何形状，并在 5 千伏的加速电压下进行精加工，以减少钛植入并获得一致的尖端到尖端形状。对于原子探针断层扫描采集，将微息券与焊接在硅柱上的锐化尖端安装到试样球上，然后将球装入旋转木马中，以放置在局部电极原子探针内。将旋转木马插入装有皮秒 355 纳米紫外激光的局部电极原子探针缓冲室内，然后转动激光器的头部。校准后，在分析室中达到真空，在6乘10到负11托尔，并使用转移杆将冰球试样插入主分析室。然后移动试样球，使微息券与局部电极对齐，以选择尖端并更新数据库以指示尖端编号。本分析成功从单晶中提取了四个钛瘤石标本尖端，并通过原子探针断层分析。其中两个试样显示铁和钛的均匀浓度，表明层压没有相交。其他两个试样在铁、氧和钛中表现出不同浓度的区域。原子探针断层扫描数据的 3D 重建允许精确测量区域内的拉梅拉间距，并提供平均 14 至 29 纳米的长度尺度，两个试样的一西格玛值为 2 纳米。除了这些测量之外，原子探针断层扫描允许通过使用点零作为拉梅拉和宿主矿物之间的交集的接近图进行分析，以高空间分辨率提取这些层层的化学信息。晶体中钛的原子浓度证实该碎片确实是钛合金，与先前对苏弗里埃尔火山喷发产品的石油学分析一致。这些近图也证实，拉梅拉的组成与伊门尼特的成分相匹配。准备楔块以捕获层，对于 FIB SEM 样品制备以及将尖端锐化到正确的尺寸至关重要。还可以进行传输电显微镜，以验证层状尺寸和层间间距。这项技术可以让火山学家计算喷发活动的时间尺度，以便更好地了解活火山的潜在危害。

Research

JoVE Journal

Environment

Analysis of Fatty Acid Content and Composition in Microalgae

脂肪酸组分和含量微藻分析

A method to determine the content and composition of total fatty acids present in microalgae is described. Fatty acids are a major constituent of ...

科研

环境科学

Measuring Fluxes of Mineral Nutrients and Toxicants in Plants with Radioactive Tracers

植物与放射性示踪剂测量矿质营养和毒物的通量

Unidirectional influx and efflux of nutrients and toxicants, and their resultant net fluxes, are central to the nutrition and toxicology of plants. ...

Use of Chironomidae (Diptera) Surface-Floating Pupal Exuviae as a Rapid Bioassessment Protocol for Water Bodies

Use of Chironomidae Diptera Surface-Floating Pupal Exuviae as a Rapid Bioassessment Protocol for Water Bodies

使用摇蚊科（双翅目）的表面浮蛹蜕为快速生物议定书水体

Rapid bioassessment protocols using benthic macroinvertebrate assemblages have been successfully used to assess human impacts on water quality. ...

Extracting Metrics for Three-dimensional Root Systems: Volume and Surface Analysis from In-soil X-ray Computed Tomography Data

从在土X射线计算机断层扫描数据量和表面分析：提取指标三维根系

Plant roots play a critical role in plant-soil-microbe interactions that occur in the rhizosphere, as well as processes with important implications to ...

Extraction and Analysis of Microbial Phospholipid Fatty Acids in Soils

提取及土壤微生物磷脂脂肪酸分析

Phospholipid fatty acids (PLFAs) are key components of microbial cell membranes. The analysis of PLFAs extracted from soils can provide information about ...

Modification and Application of a Leaf Blower-vac for Field Sampling of Arthropods

修改和叶鼓风机-VAC的节肢动物领域采样中的应用

Rice fields host a large diversity of arthropods, but investigating their population dynamics and interactions is challenging. Here we describe the ...

Dispersion of Nanomaterials in Aqueous Media: Towards Protocol Optimization

纳米材料在水介质中的分散: 对协议优化的研究

The sonication process is commonly used for de-agglomerating and dispersing nanomaterials in aqueous based media, necessary to improve homogeneity and ...

Stress Distribution During Cold Compression of Rocks and Mineral Aggregates Using Synchrotron-based X-Ray Diffraction

基于同步辐射 x 射线衍射的岩石和矿物团聚体冷压缩应力分布

We report detailed procedures for performing compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus (D-DIA) ...

An Experimental Protocol for Studying Mineral Effects on Organic Hydrothermal Transformations

研究矿物对有机热液转化影响的实验协议

Organic-mineral interactions are widely occurring in hydrothermal environments, such as hot springs, geysers on land, and the hydrothermal vents in the ...

Composition and Distribution Analysis of Bioaerosols Under Different Environmental Conditions

不同环境条件下生物气溶胶的组成及分布分析

Variable microorganisms in particulate matter (PM) under different environmental conditions may have significant impacts on human health. In this study, ...