A study of the damage on FIB-prepared TEM samples of AlxGa1-xAs

The damage produced by focused ion beam (FIB) milling on a TEM sample of AlGaAs crystals has been studied. The damage observed on the sidewall of an AlGaAs transmission electron microscopy (TEM) sample was an amorphous layer. The thickness of the amorphous layer linearly increased with an increase in FIB accelerating voltage from 5 to 30 kV. The thickness of the amorphous layer of Al(x)Ga(1-x)As was constant at 3 nm and was independent of the Al concentration x when the accelerating voltage was below 5 kV. The thickness of the amorphous layer of Al(x)Ga(1-x)As decreased with an increase in Al concentration x when the accelerating voltage was above 5 kV. FIB milling at 5 kV effectively minimizes the thickness of the amorphous layer and also provides flat sidewalls on multilayer samples of Al(x)Ga(1-x)As that are prepared for TEM and scanning electron microscopy (SEM).     

Specimen preparation for high-resolution transmission electron microscopy using focused ion beam and Ar ion milling

We have developed a focused ion beam (FIB)-Ar ion-milling technique for high-resolution transmission electron microscopy. A micrometresized specimen was mounted on a cross section of metal foil of a few micrometres thick, using FIB microsampling. Following this, a 2 degrees wedgeshaped part was made in the specimen using FIB. Finally, the specimen was milled using an Ar ion beam to remove the FIB-damaged layers. We applied the FIB-Ar ion milling technique to a CeO(2)/Gd(2)Zr(2)O(7) multilayer specimen, resulting in the crystal lattice fringes of both layers being clearly observable in comparison to a specimen finished using a Ga ion beam at an accelerating voltage of 10 kV.     

Improvements in performance of focused ion beam cross-sectioning: aspects of ion-sample interaction

A gallium (Ga) focused ion beam (FIB) has been applied increasingly to 'site-specific' preparation of cross-sectional samples for transmission electron microscopy (TEM), scanning TEM, scanning electron microscopy and scanning ion microscopy. It is absolutely required for FIB cross-sectioning to prepare higher-quality samples in a shorter time without sacrificing the site specificity. The present paper clarifies the parameters that impose limitation on the following performances of the FIB cross-sectioning: milling rate, cross-sectioning at a right angle with respect to the sample surface, curtain structures formed on the cross sections, ion implantation and ion damage. All of these are discussed from the viewpoint of ion-sample interaction. Improvements for these performances achieved by diminishing their limiting origins or by correcting the resultants are described. Especially, the FIB scanning speed is significantly utilizable to improve the milling rate. A microsampling method, which allows the FIB incidence in a sidewards or upwards direction as well as downwards with respect to the microsample surface, is very effective to minimize the curtain structures.     

Reducing focused ion beam damage to transmission electron microscopy samples

One of the most important applications of focused ion beam (FIB) systems is sample preparation for transmission electron microscopy (TEM). However, the use of the FIB inherently involves changing and damaging the sample, and thereby degrades the TEM resolution. This paper addresses the beam-induced damage and artifacts, particularly in applications involving silicon semiconductors. The damage appears in the form of amorphization on the surface of the TEM foil. The characteristics of this amorphous damage were studied by making TEM observations of cross sections of the affected foil. The damage is typically 20 to 30 nm thick for a 30 keV FIB, which is generally overly thick for modern silicon devices with feature sizes less than 250 nm. This paper reviews the reported damage depths of FIB-prepared samples, which are determined by experiments and calculations. Several damage reduction techniques, such as the use of gas-assisted etching, low energy FIB, cleaning the FIBfabricated cross section by wet or dry etching and cleaning by broad ion beam (BIB) milling have also been reviewed, with emphasis on applicability to silicon devices. We conclude that the use of low energy FIB and cleaning by argon BIB are particularly efficient techniques.     

Experimental observation of FIB induced lateral damage on silicon samples

Scanning spreading resistance microscopy (SSRM) and scanning capacitance microscopy (SCM) were used to analyze focused ion beam (FIB) induced lateral damage around milled structures on silicon. For this purpose, circular shaped structures were realized, and the influence of the implanted Ga dose (ranging from 10¹⁵ to 10¹⁷ cm^?2) and of the patterned area dimension (diameters ranging from 1 to 4 μm) on the damage were examined. It is shown that the extension of the lateral damage around FIB milled structures is much larger than the area of the purposely irradiated regions (up to a factor of 5) and increases with both, Ga dose and pattern diameter. Besides, the unique capability of SCM and SSRM techniques for the detection of FIB induced damage is demonstrated. In particular, it is shown that their high sensitivity to low densities of defects allows detecting larger damaged areas compared to Atomic Force Microscopy (AFM) topography maps.     

Ga contamination in silicon by Focused Ion Beam milling: Dynamic model simulation and Atom Probe Tomography experiment

Focused Ion Beam (FIB) milling is a widely used and important technique to prepare Transmission Electron Microscopy (TEM) lamella samples. However, it unavoidably introduces contamination in the samples like implanted ions. While the conventional ion-solid simulation model, Binary Collision Approximation (BCA), is unable to describe the FIB process, a dynamic BCA model is used in this study to predict the level of Ga implantation along the substrate depth. The FIB process involves significant material transport and local composition alteration, which requires a dynamic model for simulation. To validate the dynamic BCA model's application on simulating the FIB process, atomic level composition analysis Atom Probe Tomography (APT) is performed on Ga FIB processed silicon samples. The experimental data confirm that the dynamic BCA model is capable to predict FIB induced Ga ion implantation in silicon samples.     

DB-FIB中由不完全分解的Pt导致样品表面污染的解决方法

双束聚焦离子束（DB-FIB）已经成为半导体工业中,尤其是失效分析（FA）工作中非常重要的工具,被广泛应用于集成电路的缺陷分析和修整、TEM（透射电子显微镜）的薄片试样制备等方面。在制备TEM样品时,为了避免后期切削时Ga离子束对表层的损伤,在Ga离子束切削样品之前往往会在样品需要观测的位置上沉积一层Pt薄膜作保护层。目前,最常用的方法是先用电子束辅助沉积（E-beam assisted deposition）的方法在样品表面镀一层Pt薄膜,然后再在其上用离子束辅助沉积（I-beam assisted deposition）的方法镀一层较厚的Pt保护层。但是最近在TEM样品观测过程中,发现用DB-FIB制备的样品表面会出现球状或岛状的黑色颗粒,这种现象严重影响TEM对样品的分析。经EDX成分分析,该颗粒的主要成分为Pt,C,Ga.。通过设计一系列的实验对黑色颗粒形成原因及解决方法进行了研究。实验结果表明,这些颗粒的出现与I-BeamPt的沉积电流有关,采用48pA的I-Beam电流沉积Pt会避免黑色颗粒的出现,并且对该模型作出了解释。     

Transmission electron microscopy and atom probe specimen preparation from mechanically alloyed powder using the focused ion-beam lift-out technique

The preparation of transmission electron microscopy (TEM) and atom probe-field ion microscopy (AP-FIM) specimens from mechanically alloyed Ti-Cu-Ni-Sn powder has been explored. Applying the focused ion beam (FIB) based in situ lift-out technique, it has been demonstrated that specimen preparation can be carried on single micrometre-sized powder particles without the use of any embedding media. Since the particles did not incorporate any micropores, as revealed by cross-sectioning, the standard procedure known for bulk samples could be simply implemented to the powder material. A sequence of rectangular cuts and annular milling was found to be a highly efficient way of forming a tip-shaped AP-FIM specimen from a square cross-section blank. A Ga level < or =1 at.% was detected if a low beam current of 10 pA was chosen for the final ion-milling stages. Implanted Ga ions were mostly confined to a zone of about 2 nm in thickness and indicated that ion-induced structural transformations were negligible.     

A review of focused ion beam technology and its applications in transmission electron microscopy

The role of focused ion beam (FIB) fabrication in the development of sample preparation techniques for transmission electron microscopy (TEM) has been described in this paper. Since the repeatability of FIB sampling and TEM observations has become important, the microsampling and in situ lift-out methods are currently in wide use. Furthermore, artifacts induced during FIB milling and the consequent difficulties with energy dispersive X-ray spectroscopy are detailed. The remarkably increased capability of scanning ion microscopy and its applications are also discussed.     

FIB参数对低介电常数介质TEM样品制备的影响

研究了使用聚焦离子束(FIB)方法制备低k介质的TEM样品时离子束参数对介质微观形貌的影响,发现低k介质的微观形貌与离子束参数具有较强的相关性。传统大离子束流、高加速电压的FIB参数将导致低k介质多孔性增加、致密度下降;且k值越低,离子束参数影响越大。对于亚65nm工艺中使用的k值为2.7的介质,当离子束流减小到50pA、加速电压降低到5kV时,FIB制样方法对介质致密度的影响基本可忽略,样品微观形貌得到了显著改善;而对于65nm工艺中使用的k值为3.0的介质,其微观形貌受离子束参数的影响则相对较小。     

Advanced FIB sample preparation techniques for high resolution TEM investigations of HEMT structures

In this paper advanced sample preparation techniques based on focused ion beam (FIB) optimized for TEM investigation of high electron mobility transistor (HEMT) structures are presented. It is shown that the usage of an innovative in-situ lift-out method combined with X2 window and backside milling techniques as well as live thickness control and end point detection can significantly improve the quality of electron transparent samples required for high resolution TEM investigations. This advanced preparation flow is evaluated and demonstrated at GaN HEMT structures for atomic resolution TEM investigation.     

Local thickness and composition analysis of TEM lamellae in the FIB

High-resolution TEM image quality is greatly impacted by the thickness of the TEM sample (lamella) and the presence of any surface damage layer created during FIB–SEM sample preparation. Here we present a new technique that enables measurement of the local thickness and composition of TEM lamellae and discuss its application to the failure analysis of semiconductor devices. The local thickness in different device regions is accurately measured based on the X-ray emission excited by the electron beam in the FIB–SEM. Examples using this method to guide FIB–SEM preparation of high quality lamellae and to characterise redeposition are shown for Si and III–V semiconductor devices.     

聚焦离子束制备透射电子显微镜样品的两种厚度判断方法

透射电镜样品的厚度是透射电镜(TEM)表征中一个重要参数,快速准确地判断样品厚度是制备高质量样品的前提.本文通过使用聚焦离子束(FIB)制备了带有厚度梯度的透射电镜样品(Si、SrTiO3和LaAlO3),并提出两种制样过程中快速判断厚度的方法.第一种通过扫描电子显微镜(SEM)的衬度变化经验地判断样品的厚度;第二种是用FIB在样品边缘切一个斜边,通过SEM测量斜边侧面的宽度用几何方法推断样品的厚度.这两种方法都通过会聚束电子衍射(CBED)和电子能量损失谱(EELS)测量的厚度作为检验标准.对比认为,样品较薄时用SEM衬度测厚比较合适;样品比较厚时用几何方法测量比较直接.     

Cu/Ta/SiO2/Si薄膜在纳米压痕下的分层现象研究

采用磁控溅射技术在热氧化单晶硅衬底上先后淀积了厚度分别为50nm的Ta膜和400 nm的Cu膜.使用纳米压入仪在样品表面进行压入测试,在薄膜表面制造出残留压痕.使用扫描电镜(SEM)、聚焦离子束(FIB)、透射电镜(TEM)和X射线能谱仪(EDX)对残留压痕形貌、剖面上的分层现象进行观察,确定分层所在的位置.发现在69 mN的最大载荷作用后,在TA/SiO2界面处发生分层.分层的原因主要归结为在应力作用下,多层膜中各种材料的应变、弹性恢复能力不同.     

2D-mapping of dopant distribution in deep sub micron CMOS devices by electron holography using adapted FIB-preparation

Transmission electron microscopy (TEM) is a widely used tool for analysis of very large scale integrated (VLSI) semiconductor devices. As a special TEM-feature, off-axis electron holography obtains information about the electrical characteristics of a specimen, which are connected to the dopant concentration in the bulk material. Compared with conventional TEM, application of electron holography for dopant profiling demands a higher quality of specimen preparation, e.g. in terms of thickness homogeneity. Since preparation by means of focused ion beam (FIB) has become an industrial standard for TEM-investigations, its facilities are investigated for meeting the high holographic demands. It turned out that, besides many advantages like precision and speed, the use of FIB for preparation introduces new specific problems, e.g. it is hardly possible to visualize doped areas of semiconductors on a classical, thin FIB specimen. Additionally, some artifacts of FIB-preparation have no great importance for normal TEM analysis, but do significantly influence the results of holographic analysis. In order to satisfy the higher demands of preparation for holography, a special procedure for FIB-preparation has been newly developed.     

Physical failure analysis in semiconductor industry—challenges of the copper interconnect process

Since the copper interconnect dimensions shrunk continuously, physical failure analysis becomes increasingly important for process optimization. Failure localization and defect analysis in interconnect structures as well as analysis of barrier/seed step coverage are challenges of the copper inlaid technology. Failure localization in via chain test structures using voltage contrast analysis with SEM/FIB tools and OBIRCH and subsequent destructive failure analysis using FIB/SEM and TEM are described. The inspections of voids in copper interconnects and of buried residuals in vias are typical tasks for process monitoring, which make the application of leading-edge analytical techniques necessary. Barrier/seed step coverage analysis at via chains challenges both TEM sample preparation and analysis. 3D object reconstruction by electron tomography is a promising future method for this task.     

FIB and TEM observations of defects in hot-dip zinc coatings

The characteristic ability of FIB (focused ion beam) fabrication to remove materials from a very small and/or precisely located slab using an accelerated Ga ion beam were employed to prepare cross-sectional thin films of zinc-coated steel sheets composed of Fe-Zn intermetallic compounds. A few defects observed frequently on the galvannealed (GA) coating surface were analyzed. Streaky marks indicated the rich concentration of oxides at the interface between the galvannealed coating and the steel substrate. The annealing experiment indicated the existence of Mn and Si oxides on the steel substrate. The grain size of ferrite in the extreme surface of the substrate was smaller as compared with conventional IF (Interstitial Free) steels. Furthermore, some superlattice spots were observed at the fine ferrite grain. Defects that are termed 'wavy pattern' and 'dross' were also analyzed by the combination of the FIB and TEM (Transmission Electron Microscope) techniques.     

Electron beam induced carbon deposition using hydrocarbon contamination for XTEM analysis

The optimal parameters of electron beam induced carbon deposition (EBICD) using hydrocarbon contamination were studied as a function of electron beam energy and scanning time to avoid the mixing or damage layer formation at the interface of the electron beam assisted Pt protection layer and the sample surface by dual beam focused ion beam (DB FIB) for cross sectional transmission electron microscopy (XTEM) analysis. The optimal condition of EBICD was determined. The thickness of EBICD layer increases with electron beam scanning time and amount of hydrocarbon contamination on the sample surface. EBICD using hydrocarbon contamination successfully provides a carbon protection layer for XTEM analysis.     

电子束致沉积手控生长碳纳米线

用电子束致沉积(EBID)来制备各种纳米尺寸的结构在纳米材料的制备和器件构建方面有着良好的应用前景。相对于聚焦离子束(FIB),它具有对样品损伤小和所得结构尺寸更小等优点。此前,电子束致沉积的工作大多数在扫描电镜中完成,而在透射电镜中沉积直到近两年才发展起来。本文尝试在普通热发射透射电镜中,手动控制生长碳纳米线、点等结构。对碳纳米线的生长过程进行了原位观测,并对电子束斑的大小、形状和辐照时间对沉积物形状的影响作了初步的研究。最后对电子束致沉积可控生长无定型碳纳米线可能的应用作了一些探索。     

A method for multidirectional TEM observation of a specific site at atomic resolution

A new technique has been developed for the three-dimensional structure characterisation of a specific site at atomic resolution. In this technique, a focused ion beam (FIB) system is used to extract a specimen from a desired site as well as to fabricate the electron transparent specimen. A specimen holder with a specimen stage rotation mechanism has also been developed for use with both an FIB system and a high-resolution transmission electron microscope (TEM). The specimen holder allows both the FIB milling of a specimen and its observation in TEM without remounting the specimen from the specimen holder. A specimen for the three-dimensional TEM observation is extracted using the FIB micro-sampling technique and shaped into a pillar to mount on a tip of a needle stub enabling a multidirectional observation. The technique was applied to the multidirectional observation of the crystal structure of an Si single crystal at atomic resolution. The crystal lattice fringes of the two Si(111) planes with distances of 0.31 nm as well as the lattice fringes of the Si(200) with distances of 0.19 nm were clearly observed.