Focused Ion Beam Study of Ni5Al Single Splat Microstructure

2006 ◽  
Vol 983 ◽  
Author(s):  
Yuhong Wu ◽  
Meng Qu ◽  
Lucille A Giannuzzi ◽  
Sanjay Sampath ◽  
Andrew Gouldstone

AbstractThermally sprayed (TS) coatings are widely used for surface engineering across a range of industries, including aerospace, infrastructure and biomedical. TS materials are formed via the successive impingement, rapid quenching and build-up of molten powder particles on a substrate. The impacted ‘splats’ are thus the fundamental microstructural constituents of the coatings, and their intrinsic properties, as well as intersplat bonding and morphology, dictate coating behavior. Beyond the obvious practical considerations, from a scientific standpoint, splats represent a fascinating template for study, due to the highly non-equilibrium processing conditions (rapid deceleration from sub-sonic velocities, million-degree/sec cooling rates). In the literature, many studies of isolated splats on substrates have been carried out, but these have focused on overall morphology (disc-shape vs fragmented). Direct observations of microstructure, in particular cross-section, are limited in the specimen preparation stage due to splat size (tens of microns in diameter, 1-2 microns in thickness). However, Focused Ion Beam (FIB) techniques have allowed this problem to be addressed in a robust manner; in this paper we will discuss such approaches to observe Ni5Al splats on stainless steel substrates. Cross-sections through the splat and the substrate were created by recourse to ion milling and the ion beam itself provided good channeling contrast for grain imaging. The typical splat microstructure with sub-micron Ni(Al) columnar grains, a chill zone at the bottom and a lift off area is observed in high detail. In addition, an amorphous aluminum oxide top layer of 100-200 nm is partially present on top of the Ni(Al) columnar grains. At the splat/substrate interface, defects such as micro- and nano-scale pores were characterized for the first time and will be discussed. These observations provide insights into splat and interface formation during the deposition process and may drastically improve our current understanding of Ni5Al splat properties.

1997 ◽  
Vol 480 ◽  
Author(s):  
M. W. Phaneuf ◽  
N. Rowlands ◽  
G. J. C. Carpenter ◽  
G. Sundaram

AbstractFocused Ion Beam (FIB) systems have been steadily gaining acceptance as specimen preparation tools in the semiconductor industry. This is largely due to the fact that such instruments are relatively commonplace as failure analysis tools in semiconductor houses, and are commonly used in the preparation of cross-sections for imaging under the ion beam or using an electron beam in an SEM. Additionally, the ease with which cross-sectional TEM specimens of semiconductor devices can be prepared using FIB systems has been well demonstrated. However, this technology is largely unknown outside the semiconductor industry. Relatively few references exist in the literature on the preparation of cross-sectional TEM specimens of non-semiconductor materials by FIB. This paper discusses a specific use of FIB technology in the preparation of cross-sectional TEM specimens of non-semiconductor samples that are difficult to prepare by conventional means. One example of such materials is commercial galvannealed steel sheet that is used to form corrosion resistant auto-bodies for the automobile industry. Cross-sectional TEM specimens of this material have proved difficult and time-intensive to prepare by standard polishing and ion milling techniques due to galvanneal's inherent flaking and powdering difficulties, as well as the different sputtering rates of the various Fe-Zn intermetallic phases present in the galvannealed coatings. TEM results from cross-sectional samples of commercial galvannealed steel coatings prepared by conventional ion milling and FIB techniques are compared to assess image quality, the size of the electron-transparent thin regions that can be readily prepared and the quality of samples produced by both techniques. Specimen preparation times for both techniques are reported.


2018 ◽  
Author(s):  
C.S. Bonifacio ◽  
P. Nowakowski ◽  
M.J. Campin ◽  
M.L. Ray ◽  
P.E. Fischione

Abstract Transmission electron microscopy (TEM) specimens are typically prepared using the focused ion beam (FIB) due to its site specificity, and fast and accurate thinning capabilities. However, TEM and high-resolution TEM (HRTEM) analysis may be limited due to the resulting FIB-induced artifacts. This work identifies FIB artifacts and presents the use of argon ion milling for the removal of FIB-induced damage for reproducible TEM specimen preparation of current and future fin field effect transistor (FinFET) technologies. Subsequently, high-quality and electron-transparent TEM specimens of less than 20 nm are obtained.


1997 ◽  
Vol 3 (S2) ◽  
pp. 357-358
Author(s):  
C. Amy Hunt

The demand for TEM analysis in semiconductor failure analysis is rising sharply due to the shrinking size of devices. A well-prepared sample is a necessity for getting meaningful results. In the past decades, a significant amount of effort has been invested in improving sample preparation techniques for TEM specimens, especially precision cross-sectioning techniques. The most common methods of preparation are mechanical dimpling & ion milling, focused ion beam milling (FIBXTEM), and wedge mechanical polishing. Each precision XTEM technique has important advantages and limitations that must be considered for each sample.The concept for both dimpling & ion milling and wedge specimen preparation techniques is similar. Both techniques utilize mechanical polishing to remove the majority of the unwanted material, followed by ion milling to assist in final polishing or cleaning. Dimpling & ion milling produces the highest quality samples and is a relatively easy technique to master.


2021 ◽  
Author(s):  
C.S. Bonifacio ◽  
P. Nowakowski ◽  
R. Li ◽  
M.L. Ray ◽  
P.E. Fischione

Abstract With the introduction of new materials, new device structures, and shrinking device dimensions, failure mechanisms evolve, which can make identifying defects challenging. Therefore, an accurate and controllable delayering process to target defects is desirable. We present a workflow comprised of bulk device delayering by broad Ar ion beam milling, plan view specimen preparation by focused ion beam tool, followed by site-specific delayering by concentrated Ar ion beam milling. The result is an accurately delayered device, without sample preparation-induced artifacts, that is suitable for uncovering defects during physical failure analysis.


1999 ◽  
Vol 5 (S2) ◽  
pp. 908-909
Author(s):  
J.L. Drown-MacDonald ◽  
B.I. Prenitzer ◽  
T.L. Shofner ◽  
L.A. Giannuzzi

Focused Ion Beam (FIB) specimen preparation for both scanning and transmission electron microscopy (SEM and TEM respectively) has seen an increase in usage over the past few years. The advantage to the FIB is that site specific cross sections (or plan view sections) may be fabricated quickly and reproducibly from numerous types of materials using a finely focused beam of Ga+ ions [1,2]. It was demonstrated by Prenitzer et al. that TEM specimens may be acquired from individual Zn powder particles by employing the FIB LO specimen preparation technique [3]. In this paper, we use the FIB LO technique to prepare TEM specimens from Mount Saint Helens volcanic ash.Volcanic ash from Mount Saint Helens was obtained at the Microscopy and Microanalysis 1998 meeting in Atlanta. TEM analysis of the ash was performed using the FIB lift out technique [1]. Ash powders were dusted onto an SEM sample stud that had been coated with silver paint.


1991 ◽  
Vol 254 ◽  
Author(s):  
Reza Alani ◽  
Joseph S. Jones ◽  
Peter R. Swann

AbstractThe construction and performance of an updated gas source precision ion milling system are described. The system is based on an existing focused ion beam machine which is able to image and mill selected areas of specimens that are too thick for TEM studies. The specimen image is formed using either secondary electrons or secondary ions, captured by a dual detector. The work chamber consists of three major components: the ion gun, the ion column and the specimen chamber. The ion gun is an electron impact ionization type with an optimized source size and allows the use of variety of gases. The updated system employs an objective lens with shorter focal length to enhance the resolution. The specimen chamber with an improved specimen eucentric stage, accepts side entry TEM specimen holders. This enables the specimen to move between the TEM and the instrument for further precision thinning as required without removal of the specimen from the holder and consequent risk of damage. The upgraded system resolves features <1μm in thickness. Its point milling rate for Ni is 1.4μm/min. The ability of the instrument for imaging and localized milling is demonstrated by a number of TEM images of semiconductors, metals, ceramics and composites.


2007 ◽  
Vol 15 (1) ◽  
pp. 18-19
Author(s):  
A. Thesen ◽  
H. Hoffmeister ◽  
M. Schumann ◽  
P. Gnauck

Recent developments in nano- and semiconductor technology have substantially increased the demand for accurate and efficient site specific cross-sectioning of specimens and preparation of TEM samples. Moreover, nano-research is facing new challenges for manipulation, observation, and modification of devices on a submicron scale. At the same time in materials science a new focus on analytical nanoscale investigations—not only of specimen surfaces and cross sections—but on sample volumes is emerging.These demanding requirements can be met if a focused ion beam (FIB) column for nanoscale structuring is combined with a high resolution SEM that is used to monitor the FIB milling and deposition process on a nanometer scale. Such an integrated Cross-Beam® system enables the high resolution observation and direct control of the FIB milling process in real time. Using this concept it is possible to prepare site specific TEM samples and cross sections with nano-scale accuracy. Such a system can be complemented with a gas injection system (GIS), for deposition and enhanced etching of specific materials, as well as, in-situ micro manipulation systems, and analytical detectors such as EDX and EBSP systems.


Author(s):  
C.S. Bonifacio ◽  
P. Nowakowski ◽  
M.J. Campin ◽  
J.T. Harbaugh ◽  
M. Boccabella ◽  
...  

Abstract The sub-nanometer resolution that transmission electron microscopy (TEM) provides is critical to the development and fabrication of advanced integrated circuits. TEM specimens are usually prepared using the focused ion beam, which can cause gallium-induced artifacts and amorphization. This work presents the use of a concentrated argon ion beam for reproducible TEM specimen preparation using automatic milling termination and targeted ion milling of device features; the result is high-quality and electron-transparent specimens of less than 30 nm. Such work is relevant for semiconductor product development and failure analysis.


2000 ◽  
Vol 647 ◽  
Author(s):  
H. D. Wanzenboeck ◽  
H. Langfischer ◽  
A. Lugstein ◽  
E. Bertagnolli ◽  
U. Grabner ◽  
...  

AbstractFocused Ion Beam (FIB) technology allows to process various materials within a lateral range below 100 nm. The feasibility to mechanically sputter as well as to direct-write nanostructures and the fact that Ga-ions are utilized is unique for this method. The focused Ga-ions are used to locally induce a chemical vapor deposition of volatile precursor molecules adsorbed on a surface. Local deposition of metals and dielectrics has been achieved on a sub-µm scale utilizing a focused ion beam. This method is highly suitable for advanced microelectronic semiconductor fabrication. However, material specifications are narrow for these tailor-made applications. The effect of the Ga-ions implanted into the material both during sputtering and deposition has been realized as a key parameter for the function of FIB processed microelectronic devices. For Si-based semiconductors Ga can be used as dopant intentionally implanted into a Si substrate to locally modify the conductivity of Si. The results of locally confined ion irradiation on the surface roughness of a Si surface have been exploited by atomic force microscopy (AFM). Both local sputter depletion of the sample surface as well as sub-µm deposition of selected metals or dielectrics by ion-induced chemical vapor deposition (CVD) has been examined. The penetration depth and the distribution of Ga ions during the deposition process have been studied by simulation and experimentally by profiling with secondary ion mass spectroscopy (SIMS). Transmission Electron Microscopy (TEM) of cross-sections of the ion processed materials has revealed amorphisation of the crystalline substrate. For focused ion beam assisted deposition the effects of ion irradiation on the interface to the substrate and the local efficiency of the deposition are illustrated and discussed. The prospects of focused ion beam processing for modification of microelectronic devices in the sub-µm range and the limitations are demonstrated by the examples shown.


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