The authors would like to thank R&#252;diger Rosenkranz and Sven Niese (Fraunhofer IKTS-MD) for their assistance in sample preparation, and Ude Hangen, Douglas Stauffer, Ryan Major and Oden Warren (Hysitron Inc.) for their technical support on the PI95 TEM holder. The support of the Center for Advancing Electronics Dresden (cfaed) and the Dresden Center for Nanoanalysis (DCN) at Technische Universit&#228;t Dresden is acknowledged as well.

1.准备样品的聚焦离子束（FIB）变薄（图1） <ol><li>切割全晶圆成小片（约10毫米×10mm）的用金刚石划线。 </li><li>纪念"针尖对针尖"结构对芯片的位置。 </li><li>锯切割机芯片2毫米尺寸，以获得60微米的酒吧。酒吧包含了"针尖对针尖"结构的中心。 </li><li>胶水使用强力胶铜半环上的目标吧。下一步，胶水在Cu样品台的酒吧还使用强力胶。然后，用银膏来设置半环和铜样品台之​​间的导通。 注意:当处理样品，确保始终戴上防静电腕带，以防止静电放电，这可能在样品中损坏敏感结构。 </li></ol> 2. FIB减薄在扫描电子显微镜（图2） <ol><li>把一个在步骤1中得到的样品ñSEM样品阶段，小心地将舞台变成了SEM。 </li><li>选择沉积模式，并建立必要的保护铂层的尺寸（面积和厚度）。始终使用30千伏离子束维持最高的精度。调谐电流，以获得满意的效率，依赖于所需的Pt层的尺寸。 <ol><li>沉积的Pt线接触一个衬垫，以在Cu阶段（地电位）。接着，沉积厚的Pt层上的"尖到尖的"结构，这是非常重要的，以尽量减少在FIB减薄工艺的离子损伤和加强薄片层的顶部上。这是在FIB制备中使用的标准程序。 </li><li>采取小心不通过Pt层进行铂沉积时引进的"尖到尖的"结构的顶部的两个焊盘之间的任何导电路径。任何导电通路，将短路电路（ 图2A和B）。 </li></ol></li><li> FIB铣削<ol><li>使用30千伏的电压为10Pa和电流晋级决赛。薄靶棒成H酒吧透射电镜薄片150和180纳米之间的厚度。 </li><li>切一个缺口接近垫（V + PAD），这将通过在TEM的传感器尖端被感动。使用缺口作为标记，以确定在TEM的正确垫。 </li></ol></li></ol>从扫描电镜3.样品传输到TEM的<ol><li>戴上防静电腕带接触样品之前。 </li><li>卸除从SEM阶段的准备H-酒吧样本。从SEM中取出时，请在Cu阶段的样本。 </li><li>修复铜级到TEM持有人。移动TEM支架接近测试结构（几百微米的距离测试结构）的光学显微镜下的传感器尖端。 <ol><li>将TEM座插入TEM谨慎。在TR期间不要使用任何清洁处理（ 如 ，等离子清洗）ansfer过程，否则薄片可能受到影响。 </li></ol></li><li>保留时间为15分钟内或更短的样品传输，以避免过分暴露于环境水分和氧。 </li></ol> 4.建立电气连接（图3） <ol><li> TEM的支架连接到它的控制系统和数字​​源。然后切换控制系统和数字​​源表上。 </li><li>通过调整旋钮上的TEM持有人在做换能器尖端测试结构的粗略方法时，显示屏在TEM传感器尖端。 <ol><li>移动TEM支架靠近V +垫的传感器尖端（≤500纳米）。使换能器尖端相同的水平:作为垫（Z高度）。调的尖端的位置，使前端面对V +垫的中心。 </li></ol></li><li>联系传感器尖到V +垫。设置在顶端一个非常低的电压（0.5 V至约1 V），而接近垫。监视当前simultaneously以确保接触被建立。 </li></ol> 5. 在原位实验TDDB <ol><li>使用200千伏的加速电压以TEM。移动电子束到感兴趣的区域;选择合适的放大倍率和聚焦影像。 </li><li>使用低照度步骤（≤8），以减少对测试结构的光束的损害。使用冷凝器光圈以仅在该H-棒样品的薄的部分定位的照明区域。 </li><li>关于使用数字源，同时记录在原位的TEM图像（2-3帧/秒）的"尖到尖的"结构施加恒定电压（≤40 V）。通过使用自脚本代码， 例如，使用DigitalMicrograph软件自动记录图像。 </li><li>暂停实验看到金属的表观扩散到ULK介质时，做了电子能谱成像（ESI）的化学分析。 <ol><li>将过滤器狭缝孔进入OMEG一个能量过滤器的TEM。 </li><li>调整滤波器淤孔的宽度，以获得在电子能量损失谱（EELS）的适当能量宽度（10-20伏特）。 </li><li>按住Shift键的能量在EELS铜M-边吸收峰。 </li><li>返回到成像模式获得的铜的M-边缘有吸收峰的能量过滤TEM图像。 </li><li>转移能量至铜的M-边缘的前边缘区，并得到另一种能量过滤TEM图像。 </li><li>校正两个图像之间的样品的漂移。 </li><li>由第二个将所述第一图像以获得Cu的跳跃比图像。 </li></ol></li><li>继续TDDB实验:使用数字源的"尖到尖的"结构重新应用恒定电压（≤40 V）和记录的TEM图像。 </li></ol> 6.计算机断层扫描<ol><li>执行时的TDDB​​实验完成的TEM计算机断层扫描，以获取有关二三维分布信息ffused颗粒。 </li><li>倾斜的样品和记录倾斜系列138°的。使用1°倾斜的步骤，并在在明视场（BF）STEM模式的每一步记录图像。 </li><li>重建系列（包括对准的图像，确定倾斜轴，重建的体积和分割，以形成三维断层容积）。 </li></ol>

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</ol>

No competing financial interests.

在TDDB实验成功的前提是良好的样品制备，特别是在SEM FIB研磨过程。首先，一个厚的Pt层上的"尖到尖的"结构的顶部具有待沉积。的厚度和Pt层的尺寸可以通过SEM操作者进行调整，但必须遵循三个原则:（1）厚度和尺寸是足够的，以保护从在整个研磨过程中可能的离子束损坏的目标区域; （2）还有一个比较厚的Pt层（≥400纳米）上的研磨后留下的样品的顶部，它保护从内部和外部的应力的微妙样品并最小化应力与电介质击穿在下一TDDB的贡献实验; （3）的尺寸不应太大，否则的导电路径可能这是用来将电压施加到测试结构的两个焊盘之间形成。此外，关键的一步是何时停止晋级决赛的离子束。离子研磨必须在测试结构消失前立即中断一次一个专门设计的铜"虚拟"的互连结构，因为中央的Cu互连组成的"尖到尖的"结构和之间存在仅〜60纳米空间它们。如果"尖到尖的"结构出现在现场SEM图像将是太迟了。该H-棒的TEM薄片的厚度是有针对性地为约150至180纳米。此厚​​度允许以TEM在200千伏的加速电压的电子透明度和也保持相对厚的电介质在其上封装"尖到尖的"结构的两侧。另一方面，样品厚度为150-180毫微米将ESI化学分析过程中导致显著多个非弹性散射，因此这些效果，需要考虑到结果分析以及。 当处理或转移样品，戴上防静电STRA页。这是非常重要的，因为观察到在我们的实验中几个样本静电放电损坏，如果防静电腕带不易被磨损。最关键的转印步骤是从SEM转移到TEM。的传送时间，必须严格地在15分钟内或更小的限制。在环境空气样品的长时间曝光可能会吸收水分，破坏了"尖到尖的"结构，一个例子示于图4A中 。该样品储存在环境空气两周测试之前。在违反的TaN / Ta阻挡层影响的内在破坏机制和缩短测试结构的寿命。大量的铜扩散，然后启用。 一个关注的TEM 原位 TDDB研究是在ULK介质的束损伤。因此，这是非常重要的，以尽量减少在实验18中的光束的影响。多种策略可以被选择以减少这种影响，但它可以不能完全消除。该选项可以被分为三种方法。一种可能性是使用一个小的冷凝器孔径来减少能量的沉积的H棒型样品18中的总量。另一种选择是经营透射电镜在低电压（≤80千伏）19-21和/或低的电子剂量22-25。预计此选项可直接减少对样品的光束伤害。此外，扫描透射电子显微镜（STEM）的模式可以是低剂量显微技术，以及，如果实验参数正确地选择。因此，如果它是在所用的TEM一个可能的选择的STEM模式应优先。选择低照明亮度和记录有选择的，合理的间隔时间（低剂量）的TEM照片也建议18导致进一步降低束损伤。 除了内在的TDDB​​，TEM的样品制备和TEM观察理论上可以影响最终BReakdown。然而，观察到被认为是对TDDB损坏机制是有效的，因为:（1）用少得多的TEM束照射（低剂量STEM成像，低照度步骤和记录的图像，每隔30分钟/ 1小时），测试样品显示了类似的故障机制，在我们以前的TEM观察（连续记录图像，相对高剂量TEM模式）16-18; （2）中的电场被确认为动力和金属颗粒17（ 图5B和6A）的迁移的通过反转电连接的来源;金属颗粒和电介质击穿（3）迁移均被观察到在特定位置，其中尖到尖的间距比较小和Ta / TaN的阻挡层相对薄，而不是到处透射电镜束的照射区域内; （4）铂沉积的厚层在样品的顶部可防止最距离Ga离子的垂直注入的污染 - 的德圣结构被认为是主要的污染自由即使有污染从镓离子的横向损伤侧壁（约60nm）的表面上的少量。因此，样品制备和TEM观察应不影响本征失效机理的解释，以一个显著量。 对样品制备和实验装置复杂的过程，需要的是可能是主要的缺点。这种方法只适用于在特别设计的测试结构。因此，相对于传统的测试方法的设计和复杂的制造工艺的专用测试结构导致相当多的努力。最后，值得指出的是，样品通过在TEM束照射的修改是不可避免的，如果电子束照射在很长一段时间的微妙样品。不过，我们认为这种方法可以ENA竹叶提取的TDDB​​失效机理及降解动力学研究。 在实验的进一步发展可能能够提供定量数据用于在电介质作为所施加的电压和/或时间的函数的铜迁移和帮助制定铜/ ULK片上互连堆叠的更合适的模型。在我们的研究中，在所述的SiCN层的底部的Cu桥， 如图5C中 ESI信号明确地指出这样的事实，铜沿主电介质/的SiCN界面最有可能扩散。主要电介质的这顶表面被平面化过程的影响，并且预期具有最高量的缺陷/故障，则导致与的SiCN层的相对较弱的接口。扩散过程，使显著铜的运动，应该发生在那里。该电子传导机制，Cu扩散之前，并导致介电损伤，应遵循普尔 - 法兰克行为，theref矿石利于√E模型。从这个模型中的偏差不能推导出与这里提出的实验方法，但由于需要使合理的测试时间的大偏差。应当指出，虽然，降低所施加的电压和产生的电场应该在炼这里描述的实验方法，将来的任务之一。实际芯片的工作偏差是1至3伏。这里施加的电压是相当高的量级，因此其他影响可能在升高的电压发挥更主要作用。为此目的，新的测试结构被设计具有20至50纳米的量级的显著减少间距。然后，较小的电压可以施加和实验数据仍然可以在合理的时间量来获得的。 Cu的运动，在低偏压可能消除由于介电损坏发生的阈值的存在，然后可表征为施加的偏置和时间的函数。这些努力西港岛线l条即将研究的一部分，并能证明或证伪的冲击损伤模型，从物理损坏机理的角度来看，目前最有可能的模型来描述在低偏置10 TDDB效应。 透射X射线显微术（TXM）可以为这个实验被采用，以及如果空间分辨率可以提高到超过10纳米少得多。更重要的是，更好的传输能力，比TEM低剂量的辐射可能增加其对其它有源微电子器件应用。

由于铜互连首次被引入超大规模集成电路（ULSI）技术在1997年1，低k和超低k值（ULK）电介质被采纳到后端-的线（BEOL）片上的互连之间的绝缘材料。新材料， 例如结合，铜以降低电阻和低k / ULK电介质为低电容，克服增加的阻容（RC）的影响引起的延迟由互连尺寸收缩2,3，但是，这样做的好处是侵占通过微电子器件近年来持续侵略性缩放。使用低k / ULK材料导致在制造过程中和产品的可靠性的各种挑战，尤其是当在互连间距达到约100纳米或更小4-6。 TDDB是指一种介电材料的物理失效机制作为时间的函数下的电场。的TDDB​​可靠性试验通常进行加速条件（高架电场和/或升高的温度）下。 的TDDB​​在片上互连堆叠是用于微电子装置，它已经提出在可靠性社区强烈的关注的最关键的失效机制之一。它将继续在可靠性工程师，因为ULK电介质的聚光灯更弱的电气性能和机械性能被集成到先进技术节点的设备与。 专用实验已经进行调查TDDB失效机理7-9，和一个显著量的努力已投入到开发其描述电场的装置10-13和寿命之间的关系的模型。现有的研究有利于可靠性工程师微电子的社区;然而，许多查林GES依然存在，许多问题仍需要进行详细的解答。例如，成熟的模型来描述物理破坏机理及降解动力学的TDDB​​过程和各实验验证仍然缺乏。作为一个特殊的需要，更合适的模型，需要替代的保守√E模型14。 由于TDDB调查中非常重要的组成部分，典型故障分析正面临着前所未有的挑战， 即提供全面和确凿的证据来解释失败的机制和降解动力学物理。显然，检查数以百万计的通孔和纳米级铜线路平方米的一招一式易地成像故障部位是不是合适的选择障碍这一挑战，因为它是非常耗时，而且对破坏机理的动力学信息有限可以提供。因此，一项紧迫的任务已经出现开发第二，优化实验，以获得更好的方法来研究TDDB失效机理和降解动力学。 在本文中，我们将展示原位实验方法来研究铜/ ULK互连堆叠的TDDB失效机理。以高品质成像和化学分析能力的TEM被用于研究的专门测试结构的动力学过程。 原位电试验被整合到TEM实验以提供升高的电场到电介质。定制的"尖到尖的"结构，包括完全封装铜互连和绝缘用ULK材料，被设计在32纳米CMOS技术节点。此处所述的实验过程也可扩展到在有源器件的其它结构。

<table><tbody><tr><td>Automatic Dicing Saw</td><td>DISCO Kiru-Kezuru-Migaku Technologies</td><td></td><td></td></tr><tr><td>Scanning Electron Microscope</td><td>Zeiss</td><td>Zeiss Nvision 40</td><td></td></tr><tr><td>Picoindentor</td><td>Hysitron</td><td>Hysitron Pi95</td><td></td></tr><tr><td>Keithley SourceMeter</td><td>Keithley</td><td>Keithley 2602/237</td><td></td></tr><tr><td>Transmission Electron Microscope</td><td>FEI</td><td>FEI Tecnai F20</td><td></td></tr><tr><td>Transmission Electron Microscope</td><td>Zeiss</td><td>Zeiss Libra 200</td><td></td></tr></tbody></table>

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.

图4显示了明视场（BF）TEM从原位测试图像。有被部分破坏的TaN /钽障碍和预先存在的铜原子在ULK电介质的电试验（ 图4A）之前由于环境延长储存。只有376秒，40 V后，介电击穿开始，并伴随着与铜的距离M1金属两大迁移通路，具有正电位参考接地侧15-16。扩散的Cu粒子在ULK电介质的最终击穿（ 图4B）之后显示在高炉TEM图像。 在一个完美的样本， 即 FIB准备和TEM成像（ 图5A）之间的快速传输，在"针尖对针尖"结构是完整无氮化钽/ Ta阻挡层的损坏。相同的电压（40伏特）施加到该样品。 50余分钟，直到该样本存活故障发生原因的完整的钽/ Ta阻挡层。细分后的TEM图像示于图5B。显然，金属原子迁移到在SiO 2与M 1金属的底角，具有由红色箭头17表示的正电位。与ESI化学分析（ 图5C）证明有铜在的SiCN层和ULK电介质，它不能从图5B中的BF TEM图像的对比度检测之间的断裂界面的迁移路径。与ESI化学分析和原位 TDDB实验在TEM的结合，使TDDB失效机理和降解动力学15-16中以更直接和全面的方式进行调查。 体层摄影术是一种选择，以铜颗粒从"针尖对针尖"结构的积极的一面扩散出来的3D分布特征。 图图6B描绘的3D渲染以TEM获得由计算机断层扫描样本的切片。将黄色粒子表示在SiO 2中的迁移Cu粒子。 <img alt="图1" src="/files/ftp_upload/52447/52447fig1.jpg" /> 图中的样品实验前的1。原理的图像被置于扫描电子显微镜（SEM）。（A）的一个完整的晶片。 （ 二）从全晶圆的芯片。 （ 三）与被粘在样品阶段铜半环的"针尖对针尖"结构的目标吧。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/52447/52447fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图2" src="/files/ftp_upload/52447/52447fig2.jpg" /> 图2。 </stroNG&gt; 的H酒吧样本的聚焦离子束（FIB）技术，在扫描电镜和"针尖对针尖"结构的示意图像制造。（A）和（B）在SEM。 （C）是"针尖对针尖"结构的示意图。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/52447/52447fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图3" src="/files/ftp_upload/52447/52447fig3.jpg" /> 图3.实验装置在透射型电子显微镜（TEM）。接触接近过程（A） 的示意图像。前（B）干安装的图像在原地 TDDB实验。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/52447/52447fig3large.jpg" target="_blank">请点击此处查看次的放大版本。</a>是图。 <img alt="图4" src="/files/ftp_upload/52447/52447fig4.jpg" /> 之前的现场试验图4。代表TEM照片的"针尖对针尖"结构扩散到铜的ULK介质。（A）电气测试。 （ 二）电气测试后， <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/52447/52447fig4large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图5" src="/files/ftp_upload/52447/52447fig5.jpg" /> 图5.代表TEM图像一个完美的"针尖对针尖"的结构。电气试验前（A）明场（BF）TEM图像。 （B）中的电试验后的BF TEM图像。 （C）萨尔瓦多ectron铜分布的光谱图像。 <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/52447/52447fig6large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图6" src="/files/ftp_upload/52447/52447fig6.jpg" /> 图6. STEM图像和3D渲染的电气测试后，"针尖对针尖"结构。（A）STEM图像。 （B）中的3D渲染以TEM获得由计算机断层扫描样品（蓝色:"提示到尖"的结构，黄色:Cu粒子，绿色:晶体管结构的下方）。

Watch this Scientific Journal Video about In Situ Time-dependent Dielectric Breakdown in the Transmission Electron Microscope: A Possibility to Understand the Failure Mechanism in Microelectronic Devi

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. ...

in-situ-time-dependent-dielectric-breakdown-transmission-electron

Nanyang Technological University

Research

JoVE Journal

Engineering

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

8.7K 次观看.  Fraunhofer Institute for Ceramic Technologies and Systems. 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. 

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

Revealing Dynamic Processes of Materials in Liquids Using Liquid Cell Transmission Electron Microscopy

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted significant interests across the research fields of materials science, physics, chemistry and biology. The key enabling technology is a liquid cell. We fabricate liquid cells with thin viewing windows through a sequential microfabrication process, including silicon nitride membrane deposition, photolithographic patterning, wafer etching, cell bonding, etc. A liquid cell with the dimensions of a regular TEM grid can fit in any standard TEM sample holder. About 100 nanoliters reaction solution is loaded into the reservoirs and about 30 picoliters liquid is drawn into the viewing windows by capillary force. Subsequently, the cell is sealed and loaded into a microscope for in situ imaging. Inside the TEM, the electron beam goes through the thin liquid layer sandwiched between two silicon nitride membranes. Dynamic processes of nanoparticles in liquids, such as nucleation and growth of nanocrystals, diffusion and assembly of nanoparticles, etc., have been imaged in real time with sub-nanometer resolution. We have also applied this method to other research areas, e.g., imaging proteins in water. Liquid cell TEM is poised to play a major role in revealing dynamic processes of materials in their working environments. It may also bring high impact in the study of biological processes in their native environment.

We have developed a self-contained liquid cell, which allows imaging through liquids using a transmission electron microscope. Dynamic processes of nanoparticles in liquids can be revealed in real time with sub-nanometer resolution.

在液体中使用液体池透射电子显微镜揭示材料的动态过程

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted ...

科研

工程学

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

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

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 ...

Using Synchrotron Radiation Microtomography to Investigate Multi-scale Three-dimensional Microelectronic Packages

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data acquisition times with high spatial resolution. In the electronics industry there is serious interest in performing failure analysis on 3D microelectronic packages, many which contain multiple levels of high-density interconnections. Often in tomography there is a trade-off between image resolution and the volume of a sample that can be imaged. This inverse relationship limits the usefulness of conventional computed tomography (CT) systems since a microelectronic package is often large in cross sectional area 100-3,600 mm2, but has important features on the micron scale. The micro-tomography beamline at the Advanced Light Source (ALS), in Berkeley, CA USA, has a setup which is adaptable and can be tailored to a sample&#39;s properties, i.e., density, thickness, etc., with a maximum allowable cross-section of 36 x 36 mm. This setup also has the option of being either monochromatic in the energy range ~7-43 keV or operating with maximum flux in white light mode using a polychromatic beam. Presented here are details of the experimental steps taken to image an entire 16 x 16 mm system within a package, in order to obtain 3D images of the system with a spatial resolution of 8.7 &#181;m all within a scan time of less than 3 min. Also shown are results from packages scanned in different orientations and a sectioned package for higher resolution imaging. In contrast a conventional CT system would take hours to record data with potentially poorer resolution. Indeed, the ratio of field-of-view to throughput time is much higher when using the synchrotron radiation tomography setup. The description below of the experimental setup can be implemented and adapted for use with many other multi-materials.

For this study synchrotron radiation micro-tomography, a non-destructive three-dimensional imaging technique, is employed to investigate an entire microelectronic package with a cross-sectional area of 16 x 16 mm. Due to the synchrotron&#39;s high flux and brightness the sample was imaged in just 3 min&#160;with an 8.7 &#181;m spatial resolution.

利用同步辐射微断层调查的多尺度三维微电子封装

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data ...

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 ...

All-electronic Nanosecond-resolved Scanning Tunneling Microscopy: Facilitating the Investigation of Single Dopant Charge Dynamics

The miniaturization of semiconductor devices to scales where small numbers of dopants can control device properties requires the development of new techniques capable of characterizing their dynamics. Investigating single dopants requires sub-nanometer spatial resolution, which motivates the use of scanning tunneling microscopy (STM). However, conventional STM is limited to millisecond temporal resolution. Several methods have been developed to overcome this shortcoming, including all-electronic time-resolved STM, which is used in this study to examine dopant dynamics in silicon with nanosecond resolution. The methods presented here are widely accessible and allow for local measurement of a wide variety of dynamics at the atomic scale. A novel time-resolved scanning tunneling spectroscopy technique is presented and used to efficiently search for dynamics.

We demonstrate an all-electronic method to observe nanosecond-resolved charge dynamics of dopant atoms in silicon with a scanning tunneling microscope.

全电子纳秒分辨扫描隧道显微镜: 促进单一掺杂剂电荷动力学的研究

The miniaturization of semiconductor devices to scales where small numbers of dopants can control device properties requires the development of new ...

In Situ Transmission Electron Microscopy with Biasing and Fabrication of Asymmetric Crossbars Based on Mixed-Phased a-VOx

Resistive switching crossbar architecture is highly desired in the field of digital memories due to low cost and high-density benefits. Different materials show variability in resistive switching properties due to the intrinsic nature of the material used, leading to discrepancies in the field because of underlying operation mechanisms. This highlights a need for a reliable technique to understand mechanisms using nanostructural observations. This protocol explains a detailed process and methodology of in&#160;situ nanostructural analysis as a result of electrical biasing using transmission electron microscopy (TEM). It provides visual and reliable evidence of underlying nanostructural changes in real time memory operations. Also included is the methodology of fabrication and electrical characterizations for asymmetric crossbar structures incorporating amorphous vanadium oxide. The protocol explained here for vanadium oxide films can be easily extended to any other materials in a metal-dielectric-metal sandwiched structure. Resistive switching crossbars are predicted to serve the programmable logic and neuromorphic circuits for next-generation memory devices, given the understanding of the operation mechanisms. This protocol reveals the switching mechanism in a reliable, timely, and cost-effective way in any type of resistive switching materials, and thereby predicts the device&#39;s applicability.

In Situ Transmission Electron Microscopy with Biasing and Fabrication of Asymmetric Crossbars Based on Mixed-Phased a-VOx

Presented here is a protocol for analyzing nanostructural changes during in&#160;situ biasing with transmission electron microscopy (TEM) for a stacked metal-insulator-metal structure. It has significant applications in resistive switching crossbars for the next generation of programmable logic circuits and neuromimicking hardware, to reveal their underlying operation mechanisms and practical applicability.

基于混合相位a-VOx的不对称横杆的偏置和制造现场传输电子显微镜

Resistive switching crossbar architecture is highly desired in the field of digital memories due to low cost and high-density benefits. Different ...

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.

<meta charset="utf8"></head><body>原位多光束透射电子显微镜辐照实验的样品制备和实验设计

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.

原位多光束透射电子显微镜辐照实验的样品制备和实验设计

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

Light-Induced In Situ Transmission Electron Microscopy for Observation of the Liquid-Soft Matter Interaction

The current protocol describes the modifications of the transmission electron microscope (TEM) setup for in situ light-induced observations. A glass optical fiber inserted into the electron column above the objective lens polepiece, and a laser, an adjustable light source, was used to fabricate the device. After the illuminator has been calibrated using an external measuring system, it allows one to adjust the intensity of the lighting to the needs of the observed process. This lighting system was utilized to image antimicrobial photodynamic therapy phenomena, which are currently the subject of intense research. The sample was prepared by spotting a suspension of bacteria on a carbon, graphene, or silicon nitride substrate, blotting the excess solution, spotting the photosensitizer solution, blotting the excess liquid again, and then assembling the liquid cell with a second substrate or graphene film. The process of the imaging experiment itself includes choosing the right place for observation with the use of low magnification and a minimum dose of electrons, and then cyclical activation of the light source to capture subsequent images at specified intervals with the minimum amount of electrons necessary. The electron dose of each exposure and the time and intensity of lighting used need to be carefully recorded due to the complexity of the observed phenomena as, at the same time, the process is both light- and electron-driven. After the actual experiment is performed, additional control observations must be made, in which the same doses of electrons are used but without additional light influence and smaller doses of electrons are used for higher doses of light. This makes it possible to distinguish light-induced microstructural effects from those caused by electrons in both the fields of life and materials science.

Light-Induced In Situ Transmission Electron Microscopy for Observation of the Liquid-Soft Matter Interaction

The present protocol describes transmission electron microscope (TEM) modifications with a light illumination system, the fabrication of liquid cells, and in situ TEM observations of light-induced interactions between bacterial cells and a photosensitizer. The sample preparation methods, electron beam damage, and imaging are also discussed.

光诱导 原 位透射电子显微镜观察液-软物质相互作用

The current protocol describes the modifications of the transmission electron microscope (TEM) setup for in situ light-induced observations. A glass ...

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

摘要

探索更多视频

在液体中使用液体池透射电子显微镜揭示材料的动态过程

电池的使用同步为基础的硬X射线微断层故障分析

利用同步辐射微断层调查的多尺度三维微电子封装

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

一种新的方法

全电子纳秒分辨扫描隧道显微镜: 促进单一掺杂剂电荷动力学的研究

基于混合相位a-VO_x的不对称横杆的偏置和制造现场传输电子显微镜

原位多光束透射电子显微镜辐照实验的样品制备和实验设计

原位多光束透射电子显微镜辐照实验的样品制备和实验设计

光诱导原位透射电子显微镜观察液-软物质相互作用

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

摘要

探索更多视频

在液体中使用液体池透射电子显微镜揭示材料的动态过程

电池的使用同步为基础的硬X射线微断层故障分析

利用同步辐射微断层调查的多尺度三维微电子封装

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

一种新的方法

全电子纳秒分辨扫描隧道显微镜: 促进单一掺杂剂电荷动力学的研究

基于混合相位a-VOx的不对称横杆的偏置和制造现场传输电子显微镜

原位多光束透射电子显微镜辐照实验的样品制备和实验设计

原位多光束透射电子显微镜辐照实验的样品制备和实验设计

光诱导 原 位透射电子显微镜观察液-软物质相互作用

基于混合相位a-VO_x的不对称横杆的偏置和制造现场传输电子显微镜

光诱导原位透射电子显微镜观察液-软物质相互作用