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>

<ol>
	<li>Edelstein, 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=Full+Copper+Wiring+in+a+Sub-0.25+&#181;m+CMOS+ULSI+Technology.">Full Copper Wiring in a Sub-0.25 &#181;m CMOS ULSI Technology.</a> IEDM Tech. Dig. , 773-776 (1997).</li><li>List, S., Bamal, M., Stucchi, M., Maex, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+global+view+of+interconnects.">A global view of interconnects.</a> Microelectron. Eng. 83 (11/12), 2200-2207 (2006).</li><li>Meindl, J. D., Davis, J. A., Zarkesh-Ha, P., Patel, C. S., Martin, K. P., Kohl, P. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Interconnect+opportunities+for+gigascale+integration.">Interconnect opportunities for gigascale integration.</a> IBM J. Res. Develop. 46 (2/3), 245-263 (2002).</li><li>Zhang, X. F., Wang, Y. W., Im, J. H., Ho, P. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chip-Package+Interaction+and+Reliability+Improvement+by+Structure+Optimization+for+Ultralow-k+Interconnects+in+Flip-Chip+Packages.">Chip-Package Interaction and Reliability Improvement by Structure Optimization for Ultralow-k Interconnects in Flip-Chip Packages.</a> IEEE Trans. Device Mater. Reliab. 12 (2), 462-469 (2012).</li><li>Lee, K. D., Ogawa, E. T., Yoon, S., Lu, X., Ho, P. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electromigration+reliability+of+dual-damascene+Cu/porous+methylsilsesquioxane+low+k+interconnects.">Electromigration reliability of dual-damascene Cu/porous methylsilsesquioxane low k interconnects.</a> Appl. Phys. Lett. 82 (13), 2032 (2003).</li><li>Zschech, E., 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=Stress-induced+phenomena+in+nanosized+copper+interconnect+structures+studied+by+x-ray+and+electron+microscopy.">Stress-induced phenomena in nanosized copper interconnect structures studied by x-ray and electron microscopy.</a> J. Appl. Phys. 106 (9), 093711 (2009).</li><li>Tan, T. L., Hwang, N., Gan, C. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dielectric+Breakdown+Failure+Mechanisms+in+Cu-SiOC+low-k+interconnect+system.">Dielectric Breakdown Failure Mechanisms in Cu-SiOC low-k interconnect system.</a> IEEE Trans. Bimodal. 7 (2), 373-378 (2007).</li><li>Zhao, 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=Direct+observation+of+the+1/E+dependence+of+time+dependent+dielectric+breakdown+in+the+presence+of+copper.">Direct observation of the 1/E dependence of time dependent dielectric breakdown in the presence of copper.</a> Appl. Phys. Lett. 98 (3), 032107 (2011).</li><li>Breuer, T., Kerst, U., Boit, C., Langer, E., Ruelke, H., Fissel, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Conduction+and+material+transport+phenomena+of+degradation+in+electrically+stressed+ultra-low-k+dielectric+before+breakdown.">Conduction and material transport phenomena of degradation in electrically stressed ultra-low-k dielectric before breakdown.</a> J. Appl. Phys. 112 (12), 124103 (2012).</li><li>Lloyd, J. R., Liniger, E., Shaw, T. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Simple+model+for+time-dependent+dielectric+breakdown+in+inter-+and+intralevel+low-k+dielectrics.">Simple model for time-dependent dielectric breakdown in inter- and intralevel low-k dielectrics.</a> J. Appl. Phys. 98 (8), 084109 (2005).</li><li>Chen, F., 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+Comprehensive+Study+of+Low-k+SiCOH+TDDB+Phenomena+and+Its+Reliability+Lifetime+Model+Development.">A Comprehensive Study of Low-k SiCOH TDDB Phenomena and Its Reliability Lifetime Model Development.</a> , 46-53 (2006).</li><li>Wu, W., Duan, X., Yuan, J. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modeling+of+Time-Dependent+Dielectric+Breakdown+in+Copper+Metallization).">Modeling of Time-Dependent Dielectric Breakdown in Copper Metallization).</a> IEEE Trans. Device Mater. Reliab. 3 (2), 26-30 (2003).</li><li>Achanta, R. S., Plawsky, J. L., Gill, W. N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+time+dependent+dielectric+breakdown+model+for+field+accelerated+low-k+breakdown+due+to+copper+ions.">A time dependent dielectric breakdown model for field accelerated low-k breakdown due to copper ions.</a> Appl. Phys. Lett. 91 (23), 234106 (2007).</li><li>Chen, F., Shinosky, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Soft+breakdown+characteristics+of+ultralow-k+time-dependent+dielectric+breakdown+for+advanced+complementary+metal-oxide+semiconductor+technologies.">Soft breakdown characteristics of ultralow-k time-dependent dielectric breakdown for advanced complementary metal-oxide semiconductor technologies.</a> J. Appl. Phys. 108 (5), 054107 (2010).</li><li>Yeap, K. B., 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=An+Experimental+Methodology+for+the+In-Situ+Observation+of+the+Time-Dependent+Dielectric+Breakdown+Mechanism+in+Copper/Low-k+On-Chip+Interconnect+Structures.">An Experimental Methodology for the In-Situ Observation of the Time-Dependent Dielectric Breakdown Mechanism in Copper/Low-k On-Chip Interconnect Structures.</a> , (2013).</li><li>Yeap, K. B., 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=In+situ+study+on+low-k+interconnect+time-dependent-dielectric-breakdown+mechanisms).">In situ study on low-k interconnect time-dependent-dielectric-breakdown mechanisms).</a> J. Appl. Phys. 115 (12), 124101 (2014).</li><li>Liao, Z. Q., 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=In-situ+Study+of+the+TDDB-Induced+Damage+Mechanism+in+Cu/Ultra-low-k+Interconnect+Structures.">In-situ Study of the TDDB-Induced Damage Mechanism in Cu/Ultra-low-k Interconnect Structures.</a> Microelectron. Eng. In Press, (2014).</li><li>Liao, Z. Q., 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+New+In+Situ+Microscopy+Approach+to+Study+the+Degradation+and+Failure+Mechanisms+of+Time-Dependent+Dielectric+Breakdown:+Set-Up+and+Opportunities.">A New In Situ Microscopy Approach to Study the Degradation and Failure Mechanisms of Time-Dependent Dielectric Breakdown: Set-Up and Opportunities.</a> Adv. Eng. Mater. 16 (5), 486-493 (2014).</li><li>Lee, Z., Meyer, J. C., Rose, H., Kaiser, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Optimum+HRTEM+image+contrast+at+20+kV+and+80+kV-Exemplified+by+graphene.">Optimum HRTEM image contrast at 20 kV and 80 kV-Exemplified by graphene.</a> Ultramicroscopy. 112 (1), 39-46 (2012).</li><li>Bell, D. C., Russo, C. J., Kolmykov, D. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=40+keV+atomic+resolution+TEM.">40 keV atomic resolution TEM.</a> Ultramicroscopy. 114, 31-37 (2012).</li><li>Kaiser, U., 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=Transmission+electron+microscopy+at+20+kV+for+imaging+and+spectroscopy.">Transmission electron microscopy at 20 kV for imaging and spectroscopy.</a> Ultramicroscopy. 111 (8), 1239-1246 (2011).</li><li>Egerton, R. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Control+of+radiation+damage+in+the+TEM.">Control of radiation damage in the TEM.</a> Ultramicroscopy. 127, 100-108 (2013).</li><li>Jiang, N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Damage+mechanisms+in+electron+microscopy+of+insulating+materials.">Damage mechanisms in electron microscopy of insulating materials.</a> J. Phys. D: Appl. Phys. 46, 305502 (2013).</li><li>Buban, J. P., Ramasse, Q., Gipson, B., Browning, N. D., Stahlberg, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=High-resolution+low-dose+scanning+transmission+electron+microscopy.">High-resolution low-dose scanning transmission electron microscopy.</a> J. Electron Microsc. 59 (2), 103-112 (2010).</li><li>Egerton, R. F., Li, P., Malac, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Radiation+damage+in+the+TEM+and+SEM.">Radiation damage in the TEM and SEM.</a> Micron. 35 (6), 399-409 (2004).</li></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?...

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。 ?...

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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. ...

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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 ...

Studying Dynamic Processes of Nano-sized Objects in Liquid using Scanning Transmission Electron Microscopy

Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a microfluidic chamber assembled in the specimen holder for Transmission Electron Microscopy (TEM) and STEM. The microfluidic system consists of two silicon microchips supporting thin Silicon Nitride (SiN) membrane windows. This article describes the basic steps of sample loading and data acquisition. Most important of all is to ensure that the liquid compartment is correctly assembled, thus providing a thin liquid layer and a vacuum seal. This protocol also includes a number of tests necessary to perform during sample loading in order to ensure correct assembly. Once the sample is loaded in the electron microscope, the liquid thickness needs to be measured. Incorrect assembly may result in a too-thick liquid, while a too-thin liquid may indicate the absence of liquid, such as when a bubble is formed. Finally, the protocol explains how images are taken and how dynamic processes can be studied. A sample containing AuNPs is imaged both in pure water and in saline.

This protocol describes the operation of a liquid flow specimen holder for scanning transmission electron microscopy of AuNPs in water, as used for the observation of nanoscale dynamic processes.

使用扫描透射电子显微镜研究纳米大小的物体的动态过程中的液体

Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a ...

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.

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 ...

Quantitative Atomic-Site Analysis of Functional Dopants/Point Defects in Crystalline Materials by Electron-Channeling-Enhanced Microanalysis

A novel elemental and chemical analysis scheme based on electron-channeling phenomena in crystalline materials is introduced, where the incident high-energy electron beam is rocked with the submicrometric pivot point fixed on a specimen. This method enables us to quantitatively derive the site occupancies and site-dependent chemical information of impurities or intentionally doped functional elements in a specimen, using energy-dispersive X-ray spectroscopy and electron energy-loss spectroscopy attached to a scanning transmission electron microscope, which is of significant interest to current materials science, particularly related to nanotechnologies. This scheme is applicable to any combination of elements even when the conventional Rietveld analysis by X-ray or neutron diffraction occasionally fails to provide the desired results because of limited sample sizes and close scattering factors of neighboring elements in the periodic table. In this methodological article, we demonstrate the basic experimental procedure and analysis method of the present beam-rocking microanalysis.

We provide a general outline of quantitative microanalysis methods for estimating the site occupancies of impurities and their chemical states by taking advantage of electron-channeling phenomena under incident electron beam-rocking conditions, which reliably extract information from minority species, light elements, oxygen vacancies, and other point/line/planar defects.

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

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