这项工作是由德国研究基金会（DFG）（CH 943/2-1合同）成立。笔者想感谢沃尔夫冈迪图斯和斯特凡Paetel的Zentrum酒店献给Sonnenenergie和Wasserstoff-Forschung巴登 - 符腾堡州准备对这项工作的CIGS吸收层。

1。 CIGS层沉积<ol><li>溅射沉积500纳米到3mm厚的钠钙玻璃基板（SLG），钼（背接触层）。 </li><li>合作蒸发2微米的铜铟镓硒联多级CIGS工艺24。沫背接触层上沉积所得到的铜铟镓硒是图1中所示。 </li><li>测量CIGS层的组成组合物，用X-射线荧光光谱仪（XRF）。将得到的铜铟镓硒组合物示于表1。 </li></ol> 2。网站特定的样品制备APT分析<ol><li>剪切的TEM沫网格分为两半，以便取得一排的几个标签，即购买试样的支持。到一个保持器和锥形的标签的端部安装的TEM半网格通过电解在5重量。 ％的NaOH到顶端直径小于2微米。这个过程可以是合理控制使用立体。然后安装到另一架吨电解电网帽子是优化顺序FIB，透射电子显微镜（TEM），电子背散射衍射和APT表征。 </li><li>穆勒分两期进入CIGS薄膜使用FIB底切（ 图2a）。的组块的左侧的第一自由裁切。 </li><li>显微附加的组块通过离子束诱导化学气相沉积法沉积的Pt焊接。然后，使最终的自由相反的站点和升降机的自由站立的块（ 图2b）。 </li><li>现在切TEM莫半格尖锐的针（直径2-3微米），有一个良好的联合提取块楔形。安装大块引脚上的使用PT沉积（ 图2c）。自由切割，最终得到钼针的顶端上只有一小部分（约2微米）的chunk。之后电网架安装颠倒，莫引脚和安装一块铂之间填补了国内空白。追求其它块的相同的程序。欲了解更多详细信息，电梯过程中，读者可以查阅以下引用18,25。 </li><li>将网格直立和清洁的chunk（选铂焊缝稀释剂在网站上）的横截面，通过使用低加速电压和电子束电流（5 kV和&lt;50 pA的），在FIB中。因此，人们得到表面光滑，少污染由于GA +注入EBSD测量，这是需要的，。 </li><li>从EBSD测量截面上进行选择一个GB的兴趣。对GB的方向优选垂直于相对于分析在原子探针（z轴）方向的减少，这是描述中更详细地讨论的一部分的局部放大的效果26。与GB的一个适当的区域突出显示在图2d。 </li><li>执行在区域选择步骤2.6）中，以形成一个锋利的尖的GB的环形铣削。的曲率半径应足够小（&lt;100 nm）的进一步的TEM investigat离子。为了达到这个目标，减少的的环形铣刀图案一步的步骤（ 图2e）的内径，并且伴随着可视化的二次电子（SE）的前端成形。因此，可以纠正光束变化或调整铣图案，删除违规尖上像涟漪或材料来自不同溅射产量，阴影效果等的再沉积。 </li><li>本地化的前端通过使用TEM工具（参见图2f）的顶点相对于晶界的精确位置，知道CIGS晶界与其它材料（如超耐热合金）相比，在SEM中是不可见的。 </li><li>精确了解其中GB是位于的APT尖内，标本转移到FIB和继续磨样品位于GB最大200纳米以下的尖端的顶点。在这个阶段，在非常低的千伏（5千伏）和低电流（&lt;50 pA的）进行铣削。事实上，我们的目标不仅是本地化的GB接近吨Ø先端尖，还能最大限度地减少GA +的伤害，在此过程中的APT尖。伴随地的低千伏铣削的，可视化的形状，在SEM中的APT前端控制的物质的量应被删除从尖端的顶点（ 图2g）。 </li><li>再次转入试样的TEM检查GB尖的顶点的位置。使试样的概览图像（ 图2h），能够获得精确的了解GB位置时，试样直径的演变和半柄角。这是必要的，以便获得最佳的APT数据重建。此外，使用低倍率和减少曝光时间，以减少电子束引起的损害和C的污染，这可能会导致在APT测量较高的故障率。 </li></ol> 3。一个的CAMECA LEAP 3000X HR系统APT分析<ol><li>在亚太保持装入标本呃。然后，装入标本冰球的四个转盘之一。 </li><li>插入传送带含有试样的冰球负载锁内部和开始抽装载锁定。当负载锁内的真空度〜10 -7乇时，插入圆盘传送带内的缓冲室。 </li><li>在等待CA。 1小时来恢复缓冲室中的真空度（约7×10 -9乇），将试样从缓冲室主要分析室。这是与水平转移的棒，其中的手动操作装置。 </li><li>内的APT，凉爽下降到60 K的温度在开始测量之前，这样低的温度将在分析过程中，避免在试样表面的原子的扩散。这里我们注意到，60 K是设定温度，而不是真正的上APT尖测量，这应该是较高的，由于激光热处理试样的温度。凯洛格等人所提出的27日 ，温TURE可以估算考虑到相对充电状态比。不幸的是，在这项工作中的真实温度的提示无法计算主要是未知的，因为这一领域的CIGS材料蒸发。 </li><li> APT实验进行了使用绿色激光，其波长约532 nm和12皮秒的脉冲长度的激光模式。 </li></ol> 4。 APT数据重建<ol><li>打开RHIT文件（原始数据后直接获得APT测量）与CAMECA的综合可视化和分析软件（IVAS 3.6.2）28一般用来重建三维地图。 </li><li>执行重建三维地图使用以下八个步骤28: <ol><li>第1步-这是一个只读窗格，让所有的性质和内容的详细信息，选定研究的设置 。 </li><li>第2步- 选择离子的序列范围 。本步骤定义离子序列范围相对标本电压被选中的重建数据。 </li><li>第3步- 选择探测器的投资回报率 。此步骤可为机会，以去除离子探测器外的投资回报率（黑色椭圆探测器事件直方图）。 </li><li>步骤4 - TOF改正 。此步骤中计算的电压， - 飞行时间（TOF），分析检测器的平面性（"碗校正"）修正。 </li><li>第5步- 大众校准 。在质谱分析测得的峰值位置进行校准与已知的同位素/充电状态。 </li><li>第6步- 远程离子分配 。在此步骤中的质谱峰在指定元素同位素的范围。 </li><li>步骤7 - 重建 。此步骤适用于三种重建方法，对采集的数据之一:电压法，柄角法或尖剖面法。最后一个是在目前的研究中，重建我们的三维地图。此方法需要一个扫描电镜（SEM）或透射电子显微镜图像的钛p等示于图2g和图2小时 。在任何点的重建尖端的曲率半径被定义了一系列的SEM图像中定义的点之间的线性内插。 </li><li>第8步- 确认 。在此步骤中，将转换为"重建"选项卡中创建预览保存的分析。 </li></ol></li></ol>

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R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+post-ionization+of+field+evaporated+ions:+A+theoretical+explanation+of+multiple+charge+states.">The post-ionization of field evaporated ions: A theoretical explanation of multiple charge states.</a> Surf. Sci. 116, 273-301 (1982).</li><li>Letellier, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Etude des joints de grains et interphases dans les superalliages Astroloy par microscopie electronique et tomographie atomique [dissertation]. , (1994).</li><li>Hoummada, I., Mangelinck, K., Chow, D., Lee, J., Bernardini, <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Original+methods+for+diffusion+measurements+in+polycrystalline+thin-films.">Original methods for diffusion measurements in polycrystalline thin-films.</a> Defect and Diffusion Forum. 322, 129-150 (2012).</li></ol>

<p class="jove_content"&gt;什么都没有透露。</p&gt;

在当前的工作中，我们提出了铜铟镓硒的随机HAGB中，化合物半导体材料，用于光伏应用APT结果。此外，我们还表明，APT结合互补的技术，如EBSD和TEM是一个功能强大的工具来阐明的CIGS太阳能电池的结构组成性能关系。不幸的是，APT和EDX / EELS在TEM之间的相关性是不可能的，因为首先，EDX / EELS有没有足够的分辨率来检测低Na和O浓度晶界其次，EDX / EELS是不敏感的所有元素，尤其是娜和O <p class="jove_c...

<html>超过二十年的，因为他们的效率高，抗辐射，长期稳定，一直在开发基于铜矿结构的化合物半导体沉积Cu（In，Ga）的硒（CIGS）作为吸收材料的薄膜太阳能电池性能和低的生产成本1-3。可以制造这些太阳能电池中，只有很少的材料消耗，由于CIGS吸收层的良好的光学性能，即，直接带隙和高吸收系数1,2。足以产生高的光吸收体膜的厚度只有几微米。由于电极的光生电荷载流子的扩散路径比较短，CIGS吸收体，可以以多晶形式。铜的最大效率（铟，镓）硒（CIGS）太阳能电池迄今取得的20.4％，这是所有薄膜太阳能电池中的最高值。 ove_content"&gt;为进一步建立的CIGS薄膜光伏技术，既降低生产成本和提高太阳能电池的效率是必不可少的，后者是强烈地依赖于CIGS吸收层的微观结构和化学组成的内部接口，在吸收塔内的特定的晶界（GBS），发挥了举足轻重的作用，因为它们可能影响运输的光生载流子。 CIGS太阳能电池方面尚未解决的主要问题之一是的良性性质CIGS GBS， 即多晶的CIGS吸收薄膜产量优秀的电池效率，尽管高密度的晶界和晶格缺陷。 几位作者研究金紫荆星章CIGS薄膜太阳能级就其电学性能5,6，性格和取向差7-9以及杂质分离10-13。但是，没有明确的联系这些properti之间ES可以成立至今。特别是，有相当大的缺乏有关本地的化学组成和晶界的杂质含量。 在过去的二十年中，原子探针断层扫描（APT）已成为一个有前途的纳米分析技术14-17。直到最近，APT的太阳能电池的研究已经在很大程度上限制在样品制备过程中的困难，并使用传统的脉冲电压的原子探针分析半导体材料的能力有限。这些限制已经在很大程度上克服的发展"升出法的基础上，聚焦离子束（FIB）铣18台 ，并引进脉冲激光APT 16。已经发表了多篇论文关于APT表征CIGS太阳能电池19-23，这是大力鼓励作进一步调查。 本文给出了如何学习内部I指引nterfaces在铜铟镓硒薄膜太阳能电池由原子探针层析成像技术。

atom probe tomography studies on the cu(in,ga)se2 grain boundaries

与已有技术相比，原子探针断层扫描是一个独特的技术，能够在纳米级，并在三维空间中的化学特性的内部接口。事实上，APT具有高灵敏度（ppm级）和高空间分辨率（子纳米）。 在这里做了相当大的努力准备包含所需的晶界结构与已知的APT尖。事实上，特定于站点的样品制备使用聚焦离子束，电子背散射衍射和透射电子显微镜相结合，提出了这项工作。这种方法允许选择晶界已知的结构和位置，铜（铟，镓）硒薄膜薄膜加以研究，原子探针断层扫描。 最后，我们讨论了使用原子探针断层扫描技术来研究晶界（铜铟，镓）硒薄膜太阳能电池的优点和缺点。

图3示出的侧视图（XZ片）元素的地图随机高角度GB（HAGB）28.5° - &lt;511&gt;通过位点特异性制备方法在图2中选择的幼崽 。使用APT，共分离的钠，钾，和O在CIGS HAGB的直接映射。最有可能在这些杂质扩散到吸收层的沉积过程中在〜600℃的CIGS层的SLG衬底 图4a示出了铜，地，镓和硒的浓度分布横跨GB 如图3所示。铜，铟，镓，...

Watch this Scientific Journal Video about Atom Probe Tomography Studies on the CuIn,GaSe2 Grain Boundaries at JoVE.com

Atom Probe Tomography Studies on the CuIn,GaSe2 Grain Boundaries

在这项工作中，我们描述了使用的原子探针层析成像技术研究中的CIGS型太阳能电池的吸收层的晶粒边界。这里也提出一种新颖的方法来准备包含所需的晶界结构与已知的原子探针提示。

原子探针层析成像研究在Cu（铟，镓）硒<sub&gt; 2</sub&gt;晶界

Compared with the existent techniques, atom probe tomography is a unique technique able to chemically characterize the internal interfaces at the ...

atom-probe-tomography-studies-on-the-cu-inga-se2-grain-boundaries

Universidad de Cartagena UDEC

Research

JoVE Journal

Engineering

Atom Probe Tomography Studies on the Cu(In,Ga)Se2 Grain Boundaries

12.7K 次观看.  Max-Planck-Institut für Eisenforschung GmbH. 在这项工作中，我们描述了使用的原子探针层析成像技术研究中的CIGS型太阳能电池的吸收层的晶粒边界。这里也提出一种新颖的方法来准备包含所需的晶界结构与已知的原子探针提示。

视频: Atom Probe Tomography Studies on the CuIn,GaSe2 Grain Boundaries

In Situ Time-dependent Dielectric Breakdown in the Transmission Electron Microscope: A Possibility to Understand the Failure Mechanism in Microelectronic Devices

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. The aggressive scaling of feature sizes, both on devices and interconnects, leads to serious challenges to ensure the required product reliability. Standard reliability tests and post-mortem failure analysis provide only limited information about the physics of failure mechanisms and degradation kinetics. Therefore it is necessary to develop new experimental approaches and procedures to study the TDDB failure mechanisms and degradation kinetics in particular. In this paper, an in situ experimental methodology in the transmission electron microscope (TEM) is demonstrated to investigate the TDDB degradation and failure mechanisms in Cu/ULK interconnect stacks. High quality imaging and chemical analysis are used to study the kinetic process. The in situ electrical test is integrated into the TEM to provide an elevated electrical field to the dielectrics. Electron tomography is utilized to characterize the directed Cu diffusion in the insulating dielectrics. This experimental procedure opens a possibility to study the failure mechanism in interconnect stacks of microelectronic products, and it could also be extended to other structures in active devices.

In Situ Time-dependent Dielectric Breakdown in the Transmission Electron Microscope: A Possibility to Understand the Failure Mechanism in Microelectronic Devices

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. This paper demonstrates the procedure of an in situ TDDB experiment in the transmission electron microscope, which opens a possibility to study the failure mechanism in microelectronic products.

在透射电子显微镜原位时间相关的介质击穿:一种可能性，了解微电子器件的失效机理

The time-dependent dielectric breakdown (TDDB) in on-chip interconnect stacks is one of the most critical failure mechanisms for microelectronic devices. ...

科研

工程学

Electron Channeling Contrast Imaging for Rapid III-V Heteroepitaxial Characterization

Misfit dislocations in heteroepitaxial layers of GaP grown on Si(001) substrates are characterized through use of electron channeling contrast imaging (ECCI) in a scanning electron microscope (SEM). ECCI allows for imaging of defects and crystallographic features under specific diffraction conditions, similar to that possible via plan-view transmission electron microscopy (PV-TEM). A particular advantage of the ECCI technique is that it requires little to no sample preparation, and indeed can use large area, as-produced samples, making it a considerably higher throughput characterization method than TEM. Similar to TEM, different diffraction conditions can be obtained with ECCI by tilting and rotating the sample in the SEM. This capability enables the selective imaging of specific defects, such as misfit dislocations at the GaP/Si interface, with high contrast levels, which are determined by the standard invisibility criteria. An example application of this technique is described wherein ECCI imaging is used to determine the critical thickness for dislocation nucleation for GaP-on-Si by imaging a range of samples with various GaP epilayer thicknesses. Examples of ECCI micrographs of additional defect types, including threading dislocations and a stacking fault, are provided as demonstration of its broad, TEM-like applicability. Ultimately, the combination of TEM-like capabilities &#8211; high spatial resolution and richness of microstructural data &#8211; with the convenience and speed of SEM, position ECCI as a powerful tool for the rapid characterization of crystalline materials.

The use of electron channeling contrast imaging in a scanning electron microscope to characterize defects in III-V/Si heteroexpitaxial thin films is described. This method yields similar results to plan-view transmission electron microscopy, but in significantly less time due to lack of required sample preparation.

电子通道造影的快速III-V异质特征

Misfit dislocations in heteroepitaxial layers of GaP grown on Si(001) substrates are characterized through use of electron channeling contrast imaging ...

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

Energy dispersive X-ray spectroscopy within the scanning transmission electron microscope (STEM) provides accurate elemental analysis with high spatial resolution, and is even capable of providing atomically resolved elemental maps. In this technique, a highly focused electron beam is incident upon a thin sample and the energy of emitted X-rays is measured in order to determine the atomic species of material within the beam path. This elementally sensitive spectroscopy technique can be extended to three dimensional tomographic imaging by acquiring multiple spectrum images with the sample tilted along an axis perpendicular to the electron beam direction.
Elemental distributions within single nanoparticles are often important for determining their optical, catalytic and magnetic properties. Techniques such as X-ray tomography and slice and view energy dispersive X-ray mapping in the scanning electron microscope provide elementally sensitive three dimensional imaging but are typically limited to spatial resolutions of &gt; 20 nm. Atom probe tomography provides near atomic resolution but preparing nanoparticle samples for atom probe analysis is often challenging. Thus, elementally sensitive techniques applied within the scanning transmission electron microscope are uniquely placed to study elemental distributions within nanoparticles of dimensions 10-100 nm.
Here, energy dispersive X-ray (EDX) spectroscopy within the STEM is applied to investigate the distribution of elements in single AgAu nanoparticles. The surface segregation of both Ag and Au, at different nanoparticle compositions, has been observed.

The use of energy dispersive X-ray tomography in the scanning transmission electron microscope to characterize elemental distributions within single nanoparticles in three dimensions is described.

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 ...

Epitaxial Growth of Perovskite Strontium Titanate on Germanium via Atomic Layer Deposition

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and conformality by taking advantage of self-limiting reactions between vapor-phase precursors and the growing film. Perovskite oxides present potential for next-generation electronic materials, but to-date have mostly been deposited by physical methods. This work outlines a method for depositing SrTiO3 (STO) on germanium using ALD. Germanium has higher carrier mobilities than silicon and therefore offers an alternative semiconductor material with faster device operation. This method takes advantage of the instability of germanium's native oxide by using thermal deoxidation to clean and reconstruct the Ge (001) surface to the 2&#215;1 structure. 2-nm thick, amorphous STO is then deposited by ALD. The STO film is annealed under ultra-high vacuum and crystallizes on the reconstructed Ge surface. Reflection high-energy electron diffraction (RHEED) is used during this annealing step to monitor the STO crystallization. The thin, crystalline layer of STO acts as a template for subsequent growth of STO that is crystalline as-grown, as confirmed by RHEED. In situ X-ray photoelectron spectroscopy is used to verify film stoichiometry before and after the annealing step, as well as after subsequent STO growth. This procedure provides framework for additional perovskite oxides to be deposited on semiconductors via chemical methods in addition to the integration of more sophisticated heterostructures already achievable by physical methods.

This work details the procedures for the growth and characterization of crystalline SrTiO3 directly on germanium substrates by atomic layer deposition. The procedure illustrates the ability of an all-chemical growth method to integrate oxides monolithically onto semiconductors for metal-oxide semiconductor devices.

锗通过原子层沉积钙钛矿型钛酸锶的外延生长

Atomic layer deposition (ALD) is a commercially utilized deposition method for electronic materials. ALD growth of thin films offers thickness control and ...

化学

Comprehensive Characterization of Extended Defects in Semiconductor Materials by a Scanning Electron Microscope

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications of semiconductor materials. However, it is still under debate how the defect structure determines the band structure, and therefore, the recombination behavior of electron-hole pairs responsible for the optical and electrical properties of the extended defects. The present paper is a survey of procedures for the spatially resolved investigation of structural and of physical properties of extended defects in semiconductor materials with a scanning electron microscope (SEM). Representative examples are given for crystalline silicon. The luminescence behavior of extended defects can be investigated by cathodoluminescence (CL) measurements. They are particularly valuable because spectrally and spatially resolved information can be obtained simultaneously. For silicon, with an indirect electronic band structure, CL measurements should be carried out at low temperatures down to 5 K due to the low fraction of radiative recombination processes in comparison to non-radiative transitions at room temperature. For the study of the electrical properties of extended defects, the electron beam induced current (EBIC) technique can be applied. The EBIC image reflects the local distribution of defects due to the increased charge-carrier recombination in their vicinity. The procedure for EBIC investigations is described for measurements at room temperature and at low temperatures. Internal strain fields arising from extended defects can be determined quantitatively by cross-correlation electron backscatter diffraction (ccEBSD). This method is challenging because of the necessary preparation of the sample surface and because of the quality of the diffraction patterns which are recorded during the mapping of the sample. The spatial resolution of the three experimental techniques is compared.

The optical, electrical, and structural properties of dislocations and of grain boundaries in semiconductor materials can be determined by experiments performed in a scanning electron microscope. Electron microscopy has been used to investigate cathodoluminescence, electron beam induced current, and diffraction of backscattered electrons.

通过扫描电子显微镜在半导体材料的扩展缺陷的全面表征

Extended defects such as dislocations and grain boundaries have a strong influence on the performance of microelectronic devices and on other applications ...

A Novel Method for In Situ Electromechanical Characterization of Nanoscale Specimens

Electrically assisted deformation (EAD) is increasingly being used to improve the formability of metals during processes such as sheet metal rolling and forging. Adoption of this technique is proceeding despite disagreement concerning the underlying mechanism responsible for EAD. The experimental procedure described herein enables a more explicit study compared to previous EAD research by removing thermal effects, which are responsible for disagreement in interpreting previous EAD results. Furthermore, as the procedure described here enables EAD observation in situ and in real time in a transmission electron microscope (TEM), it is superior to existing post-mortem methods that observe EAD effects post-test. Test samples consist of a single crystal copper (SCC) foil having a free-standing tensile test section of nanoscale thickness, fabricated using a combination of laser and ion beam milling. The SCC is mounted to an etched silicon base that provides mechanical support and electrical isolation while serving as a heat sink. Using this geometry, even at high current density (~3,500 A/mm2), the test section experiences a negligible temperature increase (&#60;0.02 &#176;C), thus eliminating Joule heating effects. Monitoring material deformation and identifying the corresponding changes to microstructures, e.g. dislocations, are accomplished by acquiring and analyzing a series of TEM images. Our sample preparation and in situ experiment procedures are robust and versatile as they can be readily utilized to test materials with different microstructures, e.g., single and polycrystalline copper.

A Novel Method for In Situ Electromechanical Characterization of Nanoscale Specimens

Isolating electrical and thermal effects on electrically assisted deformation (EAD) is very difficult using macroscopic samples. Metallic sample micro- and nanostructures together with a custom test procedure have been developed to evaluate the impact of applied current on the formation without joule heating and evolution of dislocations on these samples.

一种新的方法<em&gt;原位</em&gt;纳米级样品的机电表征

Electrically assisted deformation (EAD) is increasingly being used to improve the formability of metals during processes such as sheet metal rolling and ...

Atom Probe Tomography Analysis of Exsolved Mineral Phases

Element diffusion rates and temperature/pressure control a range of fundamental volcanic and metamorphic processes. Such processes are often recorded in lamellae exsolved from host mineral phases. Thus, the analysis of the orientation, size, morphology, composition and spacing of exsolution lamellae is an area of active research in the geosciences. The conventional study of these lamellae has been conducted by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), and more recently with focused ion beam (FIB)-based nanotomography, yet with limited chemical information. Here, we explore the use of atom probe tomography (APT) for the nanoscale analysis of ilmenite exsolution lamellae in igneous titanomagnetite from ash deposits erupted from the active Soufri&#232;re Hills Volcano (Montserrat, British West Indies). APT allows the precise calculation of interlamellar spacings (14&#8211;29 &#177; 2 nm) and reveals smooth diffusion profiles with no sharp phase boundaries during the exchange of Fe and Ti/O between the exsolved lamellae and the host crystal. Our results suggest that this novel approach permits nanoscale measurements of lamellae composition and interlamellar spacing that may provide a means to estimate the lava dome temperatures necessary to model extrusion rates and lava dome failure, both of which play a key role in volcanic hazard mitigation efforts.

Analysis of the morphology, composition, and spacing of exsolution lamellae can provide essential information to understand geological processes related to volcanism and metamorphism. We present a novel application of APT for the characterization of such lamellae and compare this approach to the conventional use of electron microscopy and FIB-based nanotomography.

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 ...

环境科学

Processing of Bulk Nanocrystalline Metals at the US Army Research Laboratory

Given their potential for significant property improvements relative to their large grained counterparts, much work has been devoted to the continued development of nanocrystalline metals. Despite these efforts, the transition of these materials from the lab bench to actual applications has been blocked by the inability to produce large scale parts that retain the desired nanocrystalline microstructures. Following the development of a method proven to stabilize the nanosized grain structure to temperatures approaching that of the melting point for the given metal, the US Army Research Laboratory (ARL) has progressed to the next stage in the development of these materials - namely the production of large scale parts suitable for testing and evaluation in a range of relevant test environments. This report provides a broad overview of the ongoing efforts in the processing, characterization, and consolidation of these materials at ARL. In particular, focus is placed on the methodology used for producing the nanocrystalline metal powders, in both small and large-scale amounts, that are at the center of ongoing research efforts.

This paper provides a brief overview of the ongoing efforts at the Army Research Laboratory on the processing of bulk nanocrystalline metals with an emphasis on the methodologies used for the production of the novel metal powders.

美国陆军研究实验室散装纳米晶金属的加工

Given their potential for significant property improvements relative to their large grained counterparts, much work has been devoted to the continued ...

Theoretical Calculation and Experimental Verification for Dislocation Reduction in Germanium Epitaxial Layers with Semicylindrical Voids on Silicon

Reduction of threading dislocation density (TDD) in epitaxial germanium (Ge) on silicon (Si) has been one of the most important challenges for the realization of monolithically integrated photonics circuits. The present paper describes methods of theoretical calculation and experimental verification of a novel model for the reduction of TDD. The method of theoretical calculation describes the bending of threading dislocations (TDs) based on the interaction of TDs and non-planar growth surfaces of selective epitaxial growth (SEG) in terms of dislocation image force. The calculation reveals that the presence of voids on SiO2 masks help to reduce TDD. Experimental verification is described by germanium (Ge) SEG, using an ultra-high vacuum chemical vapor deposition method and TD observations of the grown Ge via etching and cross-sectional transmission electron microscope (TEM). It is strongly suggested that the TDD reduction would be due to the presence of semicylindrical voids over the SiO2 SEG masks and growth temperature. For experimental verification, epitaxial Ge layers with semicylindrical voids are formed as the result of SEG of Ge layers and their coalescence. The experimentally obtained TDDs reproduce the calculated TDDs based on the theoretical model. Cross-sectional TEM observations reveal that both the termination and generation of TDs occur at semicylindrical voids. Plan-view TEM observations reveal a unique behavior of TDs in Ge with semicylindrical voids (i.e., TDs are bent to be parallel to the SEG masks and the Si substrate).

Theoretical calculation and experimental verification are proposed for a reduction of threading dislocation (TD) density in germanium epitaxial layers with semicylindrical voids on silicon. Calculations based on the interaction of TDs and surface via image force, TD measurements, and transmission electron microscope observations of TDs are presented.

硅上半圆柱空隙锗外延层位错还原的理论计算和实验验证

Reduction of threading dislocation density (TDD) in epitaxial germanium (Ge) on silicon (Si) has been one of the most important challenges for the ...

Sample Preparation and Experimental Design for In Situ Multi-Beam Transmission Electron Microscopy Irradiation Experiments

There is a need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these stressors are combined there may be synergistic effects that enable unique microstructural evolution mechanisms to activate. Understanding of these mechanisms is necessary for the input and refinement of predictive models and critical for engineering of next generation materials. The basic physics and underlying mechanisms require advanced tools to be investigated. The in situ ion irradiation transmission electron microscope (I&#179;TEM) is designed to explore these principles.
To quantitatively probe the complex dynamic interactions in materials, careful preparation of samples and consideration of experimental design is required. Particular handling or preparation of samples can easily introduce damage or features that obfuscate the measurements. There is no one correct way to prepare a sample; however, many mistakes can be made. The most common errors and things to consider are highlighted within. The I&#179;TEM has many adjustable variables and a large potential experimental space, therefore it is best to design experiments with a specific scientific question or questions in mind.
Experiments have been performed on large number of sample geometries, material classes, and with many irradiation conditions. The following are a subset of examples that demonstrate unique in situ capabilities utilizing the I3TEM. Au nanoparticles prepared by drop casting have been used to investigate the effects of single ion strikes. Au thin films have been used in studies on the effects of multibeam irradiation on microstructure evolution. Zr films have been exposed to irradiation and mechanical tension to examine creep. Ag nanopillars were subjected to simultaneous high temperature, mechanical compression, and ion irradiation to study irradiation induced creep as well. These results impact fields including: structural materials, nuclear energy, energy storage, catalysis, and microelectronics in space environments.

Sample preparation techniques are outlined with specific considerations for in situ ion irradiation TEM experiments. Ion species, energy, and fluence are discussed with methods for how to select and compute them. Finally, procedures for conducting an experiment are described and accompanied by the representative results.

There is a need to understand materials exposed to overlapping extreme environments such as high temperature, radiation, or mechanical stress. When these ...

原子探针层析成像研究在Cu（铟，镓）硒

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