Name: synchrotron x-ray microdiffraction and fluorescence imaging of mineral and rock samples
Uploaded: 2018-06-19T15:00:00
Description: Watch this Scientific Journal Video about Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples at JoVE.com

本研究使用了先进光源的资源, 这是一个能源部的科学用户设施根据合同没有。DE-AC02-05CH11231。我们还想确认 Drs. l. Dobrzhinetskaya 和罗伊为碳硅石样品提供了帮助, c. 斯图尔特为她的橄榄蜗牛壳数据, h. 沈为橄榄蜗牛壳的准备, 和周和陈教授对橄榄蜗牛的 EDS 测量壳。

1. 设置光束线和收集数据
注: 校准标准和样品以同样的方式收集, 主要区别在处理方法。
<ol><li>装上样品并关闭实验箱。
	<ol>
<li>将一个样本附加到运动底座的上半部分 (见材料表), 这样, ROI 相对于底座垂直偏移至少15毫米。 注: 标准块存在于光束线中, 用于样品 < 20 毫米厚。运动学基础的下半部分永久安装在光束线的舞台系统上。</li>
		<li>将样品?...

<ol>
	<li>Li, Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+synchrotron+study+of+defect+and+strain+inhomogeneity+in+laser-assisted+three-dimensionally-printed+Ni-based+superalloy.">A synchrotron study of defect and strain inhomogeneity in laser-assisted three-dimensionally-printed Ni-based superalloy.</a> Applied Physics Letters. 107 (18), 181902 (2015).</li><li>Zhou, G., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Real-time+microstructure+imaging+by+Laue+microdiffraction:+A+sample+application+in+laser+3D+printed+Ni-based+superalloys.">Real-time microstructure imaging by Laue microdiffraction: A sample application in laser 3D printed Ni-based superalloys.</a> Scientific Reports. 6, 28144 (2016).</li><li>Tippabhotla, S. K., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synchrotron+X-ray+Micro-diffraction+-+Probing+Stress+State+in+Encapsulated+Thin+Silicon+Solar+Cells.">Synchrotron X-ray Micro-diffraction - Probing Stress State in Encapsulated Thin Silicon Solar Cells.</a> Procedia Engineering. 139, 123-133 (2016).</li><li>Xu, C. Z., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Elemental+Topological+Dirac+Semimetal:+&#945;-Sn+on+InSb(111)+.">Elemental Topological Dirac Semimetal: &#945;-Sn on InSb(111) .</a> Phys Rev Lett. 118 (14), 146402 (2017).</li><li>Chen, X., Tamura, N., MacDowell, A., James, R. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In-situ+characterization+of+highly+reversible+phase+transformation+by+synchrotron+X-ray+Laue+microdiffraction.">In-situ characterization of highly reversible phase transformation by synchrotron X-ray Laue microdiffraction.</a> Appl Phys Lett. 108 (21), 211902 (2016).</li><li>Zhou, X., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Reversal+in+the+Size+Dependence+of+Grain+Rotation.">Reversal in the Size Dependence of Grain Rotation.</a> Phys Rev Lett. 118 (9), 096101 (2017).</li><li>Stan, C. V., Beavers, C. M., Kunz, M., Tamura, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=X-Ray+Diffraction+under+Extreme+Conditions+at+the+Advanced+Light+Source.">X-Ray Diffraction under Extreme Conditions at the Advanced Light Source.</a> Quantum Beam Science. 2 (1), 4 (2018).</li><li>Chen, K., Kunz, M., Tamura, N., Wenk, H. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Residual+stress+preserved+in+quartz+from+the+San+Andreas+Fault+Observatory+at+Depth.">Residual stress preserved in quartz from the San Andreas Fault Observatory at Depth.</a> Geology. 43 (3), 219-222 (2015).</li><li>Chen, K., Kunz, M., Tamura, N., Wenk, H. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Evidence+for+high+stress+in+quartz+from+the+impact+site+of+Vredefort,+South+Africa.">Evidence for high stress in quartz from the impact site of Vredefort, South Africa.</a> Eur J Mineral. 23 (2), 169-178 (2011).</li><li>Jackson, M. D., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Material+and+Elastic+Properties+of+Al-Tobermorite+in+Ancient+Roman+Seawater+Concrete.">Material and Elastic Properties of Al-Tobermorite in Ancient Roman Seawater Concrete.</a> J Am Ceram Soc. 96 (8), 2598-2606 (2013).</li><li>Jackson, M. 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A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nacre+tablet+thickness+records+formation+temperature+in+modern+and+fossil+shells.">Nacre tablet thickness records formation temperature in modern and fossil shells.</a> Earth Planet Sc Lett. 460, 281-292 (2017).</li><li>Mass, T., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Amorphous+calcium+carbonate+particles+form+coral+skeletons.">Amorphous calcium carbonate particles form coral skeletons.</a> P Natl Acad Sci. 114 (37), E7670-E7678 (2017).</li><li>Marcus, M. A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Parrotfish+Teeth:+Stiff+Biominerals+Whose+Microstructure+Makes+Them+Tough+and+Abrasion-Resistant+To+Bite+Stony+Corals.">Parrotfish Teeth: Stiff Biominerals Whose Microstructure Makes Them Tough and Abrasion-Resistant To Bite Stony Corals.</a> ACS Nano. 11 (12), 11856-11865 (2017).</li><li>Kunz, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+dedicated+superbend+x-ray+microdiffraction+beamline+for+materials,+geo-,+and+environmental+sciences+at+the+advanced+light+source.">A dedicated superbend x-ray microdiffraction beamline for materials, geo-, and environmental sciences at the advanced light source.</a> Rev Sci Instrum. 80 (3), 035108 (2009).</li><li>Beckhoff, B., Kanngie&#223;er, B., Langhoff, N., Wedell, R., Wolff, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Handbook of Practical X-Ray Fluorescence Analysis. , (2007).</li><li>Tamura, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=XMAS:+A+Versatile+Tool+for+Analyzing+Synchrotron+X-ray+Microdiffraction+Data.">XMAS: A Versatile Tool for Analyzing Synchrotron X-ray Microdiffraction Data.</a> Strain and Dislocation Gradients from Diffraction. , 125-155 (2014).</li><li>Dobrzhinetskaya, L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Moissanite+(SiC)+with+metal-silicide+and+silicon+inclusions+from+tuff+of+Israel:+Raman+spectroscopy+and+electron+microscope+studies.">Moissanite (SiC) with metal-silicide and silicon inclusions from tuff of Israel: Raman spectroscopy and electron microscope studies.</a> Lithos. , (2017).</li><li>Thibault, N. 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我们提出了一种联合 x 射线衍射和 XRF 分析的晶体样品在 ALS 光束线12.3.2 的方法。虽然劳厄衍射、粉末衍射和 XRF 本身都不是新颖的方法, 但光束线12.3.2 结合了微米尺度的 x 射线光束大小、扫描阶段系统与探测器曝光触发相关联, 并全面分析软件, 以允许在实验室仪器上不可能的实验。光束线中的光子通量比实验室仪器所能达到的数量级要高一些。此外, 典型的劳厄衍射实验室仪器仅设计用于单晶体...

晶体样品经常显示微米尺度上的异质性。在地球科学中, 矿物的识别, 它们的晶体结构, 以及它们在2D 系统中的相位关系, 对于理解一个特定系统的物理和化学是很重要的, 需要一个空间分辨的定量技术。例如, 可以根据局部2D 区域内的相分布来检查矿物之间的关系。这可能会影响到在岩石体内可能发生的历史和化学相互作用。或者, 一个单一矿物的物质结构可以被审查;这可能决定矿物可能已经或目前正在遭受的变形类型 (例如, 在原位变形实验的情况下, 像钻石铁砧单元的设备)。在地学中, 这些分析通常是使用扫描电子显微镜 (SEM) 与能量或波长色散 x 射线光谱 (E/WDS) 和电子背向散射衍射 (EBSD) 相结合进行的。然而, 样品的制备可能是困难的, 涉及广泛的抛光和安装真空测量。此外, EBSD 是一种表面技术, 需要相对浊的晶体, 这并不总是情况下, 地质材料可能经历了隆起, 侵蚀, 或压缩。
使用 2D x 射线 microdiffraction 和 XRF 映射的空间分辨特性, 如 ALS 的光束线12.3.2 所提供的, 是一种快速而直接的方法, 用于制作单个或多相系统的大面积图, 其中晶体尺寸在少量纳米 (在多晶样品的情况下) 到上百个微米。与其他常用技术相比, 该方法具有许多优点。不同于其他2D 晶体制图技术, 如 EBSD, microdiffraction 样品可以测量在环境条件下, 因此不需要特殊的准备, 因为没有真空室。Microdiffraction 适用于原始的水晶, 以及那些经历过严重的应变或塑性变形的晶体。像薄切片这样的样品通常被检查, 如嵌在环氧树脂中的材料, 甚至是不变的岩石或谷物。数据收集速度快, 通常小于0.5 秒/像素的劳厄衍射, 不到1分钟/像素的粉末衍射, 和小于 0.1 s/像素的 XRF。数据存储在本地, 临时存放在本地存储上, 并且更永久性地保存在国家能源研究科学计算 (NERSC) 中心, 便于下载。衍射数据处理可以在局部群上或 NERSC 群中进行, 在20分钟以下。这使得数据收集和分析的快速吞吐量, 以及与实验室仪器相比, 在短时间内进行大面积测量。
该方法具有广泛的应用价值, 在材料科学和工程中得到了广泛应用, 分析了从3维印刷金属1、2到太阳能电池板变形3的各种情况, 以应变拓扑材料4, 到记忆合金相变5, 到高压行为的纳米晶材料6,7。最近的地球科学项目包括分析各种石英样品中的应变8,9的火山胶凝过程10,11, 以及生物矿物, 如方解石和文石在壳和珊瑚12,13或磷灰石在牙齿14, 和额外的研究陨石相分布, 矿物结构识别的新矿物, 和塑性变形响应的高压二氧化硅也被收集。在光束线12.3.2 使用的技术适用于范围广泛的样品, 与矿物学或岩石学群落中的任何人有关。在这里, 我们概述了光束线12.3.2 的数据采集和分析协议, 并提出了几个应用, 以证明联合 XRF 和劳厄/粉 microdiffraction 技术在地球科学领域的实用性。
在进入实验细节之前, 讨论终端站的设置 (参见图 1和图 4中的 Kunz等) 是密切相关的。15). x 射线光束退出储存环, 并使用环形镜 (M201) 定向, 其目的是将光源重新聚焦在实验笼的入口处。它通过一组辊缝, 作为一个次要的来源点。然后 monochromatized (或不) 取决于实验类型, 然后通过一组克里斯·柯克帕特里克-贝兹 (KB) 镜像, 在通过第二套狭缝并聚焦于微米尺寸。然后光束通过一个离子室, 其信号用于确定光束强度。附着在离子室是一个针孔, 它阻止散射信号撞击到探测器上。聚焦光束然后遇到样本。样品放在一个舞台的顶部, 由8马达组成: 一组粗 (下) x, y, z 马达, 一组精细 (上部) x, y, z 马达, 和两个旋转马达 (Φ和χ)。它可以可视化与三光学摄像头: 一个低变焦, 放置在离子室的顶部, 一个具有高变焦, 放置在一个近似45°角度的 x 射线光束的平面上, 和第二个高变焦相机放置在90°角度, 关于 tx 射线光束。最后一个最适合垂直方向的样品 (例如, 用于传输模式实验), 而成像是使用附着在针孔上的楔形镜面进行的。x 射线衍射探测器位于较大的旋转阶段, 可控制探测器的角度和垂直位移。还存在一种用于收集 XRF 的硅漂移探测器。样品可以以任何方式制备, 只要所暴露的感兴趣区域 (ROI) 是平坦的 (在微米级), 并发现或覆盖在不超过50-100 µm 的 x 射线透明材料, 如聚酰亚胺胶带。
下面概述的过程描述了在反射几何中发生的实验, 并假定 z 方向是正常的样本, x 和 y 分别是水平和垂直扫描方向。然而, 由于舞台和探测器系统的灵活性, 在传输几何中进行了一些实验, 其中 x 和 z 方向为水平和垂直扫描方向, y 与直接光束平行 (见杰克逊等等。10,11)。

<table border="0" cellpadding="0" cellspacing="0" width="784">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:285px;">ThorLabs KB3x3 kinematic base, top half</td>
			<td style="width:213px;">ThorLabs</td>
			<td style="width:119px;">KBT3X3</td>
			<td style="width:167px;">Several of these bases are available for borrowing. The base must be the imperial and not the metric type, otherwise it will not properly fit on the stage.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:285px;">Scotch double sided tape</td>
			<td style="width:213px;"></td>
			<td style="width:119px;"></td>
			<td>Available at any office supply store, and also at the beamline</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:285px;">Polyimide/Kapton tape</td>
			<td style="width:213px;">Dupont</td>
			<td style="width:119px;"></td>
			<td>Several widths are commercially available. Any width that is enough to cover the sample is fine.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:285px;">Samples</td>
			<td style="width:213px;"></td>
			<td style="width:119px;"></td>
			<td>Provided by user, site of interest should be polished if larger mapping is desired.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:285px;">Software: XMAS</td>
			<td style="width:213px;"></td>
			<td style="width:119px;"></td>
			<td>Downloadable here https://sites.google.com/a/lbl.gov/bl12-3-2/user-resources</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:285px;">Software: IDL 6.2</td>
			<td style="width:213px;">Harris Geospatial Solutions</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:285px;">X-ray Diffraction Detector</td>
			<td>DECTRIS Pilatus 1M&#160;</td>
			<td style="width:119px;"></td>
			<td>hybrid pixel array detector</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Huber stage</td>
			<td style="width:213px;"></td>
			<td style="width:119px;"></td>
			<td>stage for detector</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Vortex silicon drift detector&#160;</td>
			<td style="width:213px;"></td>
			<td style="width:119px;"></td>
			<td>silicon drift detector</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">IgorPro v. 6.37</td>
			<td style="width:213px;"></td>
			<td style="width:119px;"></td>
			<td>Plotting software</td>
		</tr>
	</tbody>
</table>

synchrotron x-ray microdiffraction and fluorescence imaging of mineral and rock samples

在本报告中, 我们描述了获取和处理 x 射线 microfluorescence (μXRF) 和劳厄和粉末 microdiffraction 二维 (2D) 地图在光束线12.3.2 的先进光源 (ALS) 的详细程序, 劳伦斯伯克利国家实验室。测量可以在任何小于10厘米 x 10 厘米 x 5 厘米的样品上执行, 并具有平坦暴露的表面。实验几何是用标准材料 (XRF 的元素标准, 和晶体样品如 Si, 石英, 或 Al2O3的衍射) 来校准的。样品与 x 射线束的焦距对齐, 并执行光栅扫描, 其中每个像素对应一个测量,例如,一个 XRF 光谱或一个衍射图案。然后使用内部开发的软件 "圣诞" 处理这些数据, 它输出文本文件, 其中每一行对应于一个像素位置。碳硅石和橄榄蜗牛壳的代表性数据展示了数据质量、收集和分析策略。

劳厄 Microdiffraction
最近对天然碳硅石 (SiC) 样品18进行了测量和分析。该样品包括一个嵌在环氧树脂插头的凝灰岩, 然后切割和抛光, 以揭露 ROI。用光学显微镜和拉曼光谱 (图 1a) 鉴定了三碳硅石颗粒。其中一粒, SiC 2 (图 1b), 被认为含有本机硅 (Si)<sup class=...

Watch this Scientific Journal Video about Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples at JoVE.com

Synchrotron X-ray Microdiffraction and Fluorescence Imaging of Mineral and Rock Samples

我们描述了一个光束线的设置, 目的是进行快速的二维 x 射线荧光和 x 射线 microdiffraction 映射的单晶或粉末样品使用劳厄 (多色辐射) 或粉末 (单色辐射) 衍射。生成的地图提供了有关应变、方向、相分布和塑性变形的信息。

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Reservoir Condition Pore-scale Imaging of Multiple Fluid Phases Using X-ray Microtomography

多重流体相储层孔隙条件级成像使用X射线微断层

X-ray microtomography was used to image, at a resolution of 6.6 &#181;m, the pore-scale arrangement of residual carbon dioxide ganglia in the pore-space ...

Energy Dispersive X-ray Tomography for 3D Elemental Mapping of Individual Nanoparticles

能量色散X射线断层摄影术对个人纳米3D元素映射

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial ...

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

电池的使用同步为基础的硬X射线微断层故障分析

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

Measurement of X-ray Beam Coherence along Multiple Directions Using 2-D Checkerboard Phase Grating

使用2-D棋盘相位光栅X射线束相干测量沿多个方向

A procedure for a technique to measure the transverse coherence of synchrotron radiation X-ray sources using a single phase grating interferometer is ...

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

电化学测试的协议及表征非质子锂的O<sub&gt; 2</sub&gt;电池

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic ...

Dynamic Pore-scale Reservoir-condition Imaging of Reaction in Carbonates Using Synchrotron Fast Tomography

用同步快速反应层析成像动态孔隙规模油藏条件下成像碳酸盐

Underground storage permanence is a major concern for carbon capture and storage. Pumping CO2 into carbonate reservoirs has the potential to dissolve ...

In Depth Analyses of LEDs by a Combination of X-ray Computed Tomography (CT) and Light Microscopy (LM) Correlated with Scanning Electron Microscopy (SEM)

In Depth Analyses of LEDs by a Combination of X-ray Computed Tomography CT and Light Microscopy LM Correlated with Scanning Electron Microscopy SEM

在通过X射线计算机断层扫描（CT）和与扫描电子显微镜相关光学显微镜（LM）的一个组合的LED深度分析（SEM）的

In failure analysis, device characterization and reverse engineering of light emitting diodes (LEDs), and similar electronic components of ...

Applying X-ray Imaging Crystal Spectroscopy for Use as a High Temperature Plasma Diagnostic

运用X射线成像光谱水晶的使用为高温等离子体诊断

X-ray spectra provide a wealth of information on high temperature plasmas; for example electron temperature and density can be inferred from line ...