Microstructural Observation of Focused Ion Beam Modification of Ni Silicide/Si Thin Films

1996 ◽  
Vol 439 ◽  
Author(s):  
Miyoko Tanaka ◽  
Kazuo Furuya ◽  
Tetsuya Saito

AbstractFocused ion beam (FIB) irradiation of a thin Ni2Si layer deposited on a Si substrate was carried out and studied using an in-situ transmission electron microscope (in-situ TEM). Square areas on sides of 4 by 4 and 9 by 9 μm were patterned at room temperature with a 25keV Ga+-FIB attached to the TEM. The structural changes of the films indicate a uniform milling; sputtering of the Ni2Si layer and the damage introducing to the Si substrate. Annealing at 673 K results in the change of the Ni2Si layer into an epitaxial NiSi2 layer outside the FIB irradiated area, but several precipitates appear around the treated area. Precipitates was analyzed by energy dispersive X-ray spectroscopy (EDS). Larger amount of Ni than the surrounding matrix was found in precipitates. Selected area diffraction (SAD) patterns of the precipitates and the corresponding dark field images imply the formation of a Ni rich silicide. The relation between the FIB tail and the precipitation is indicated.

1996 ◽  
Vol 438 ◽  
Author(s):  
Miyoko Tanaka ◽  
Kazuo Furuya ◽  
Tetsuya Saito

AbstractFocused ion beam (FIB) irradiation of a thin Ni2Si layer deposited on a Si substrate was carried out and studied using an in-situ transmission electron microscope (in-situ TEM). Square areas on sides of 4 by 4 and 9 by 9 μm were patterned at room temperature with a 25keV Ga+-FIB attached to the TEM. The structural changes of the films indicate a uniform milling; sputtering of the Ni2Si layer and the damage introducing to the Si substrate. Annealing at 673 K results in the change of the Ni2Si layer into an epitaxial NiSi2 layer outside the FIB irradiated area, but several precipitates appear around the treated area. Precipitates was analyzed by energy dispersive X-ray spectroscopy (EDS). Larger amount of Ni than the surrounding matrix was found in precipitates. Selected area diffraction (SAD) patterns of the precipitates and the corresponding dark field images imply the formation of a Ni rich silicide. The relation between the FIB tail and the precipitation is indicated.


1996 ◽  
Vol 441 ◽  
Author(s):  
K. Tsujimoto ◽  
S. Tsuji ◽  
H. Saka ◽  
K. Kuroda ◽  
H. Takatsuji ◽  
...  

AbstractThe recent attention paid to stress migration of aluminum (Al) electrodes in thin-film transistor liquid crystal display (TFT-LCD) applications indicates that wiring materials with low electrical resistivities are of considerable interest for their potential use in higher-resolution displays. In this paper, we firstly describe how as-grown Al whiskers on Al electrodes fabricated on a LCD-grade glass substrate can be characterized by means of a high-voltage transmission electron microscope (HV-TEM) operated at 1 MV. The whiskers ranging from 300 to 400 nm in diameter are sufficient to be transparent to high-voltage electrons. This allows detailed observation of whisker characteristics such as its morphology and crystallography. In most cases, the as-grown Al whiskers in our study had straight rod shapes, and could be regarded as single crystals. Secondly, we report on the in-situ fabrication and observation of Al whiskers at elevated temperature with the HV-TEM. Since relatively thick TEM samples (up to about 1 mm) can be set on a sample holder in the HV-TEM, various growth stages of Al whiskers can be investigated under various heating conditions. Finally, we demonstrate a TEM sample preparation method for the cross-section of an individual Al whisker, using focused ion beam (FIB) etching. This technique makes it possible to reduce the thickness of an Al whisker close to the root. Both bright- and dark-field TEM images provide nanostructural information on the whisker/Al thin-film interface.


1997 ◽  
Vol 480 ◽  
Author(s):  
M. A. Wall ◽  
T. W. Barbee

AbstractThe success of in-situ transmission electron microscopy experimentation is often dictated by proper specimen preparation. We report here a novel technique permitting the production of crosssectioned tensile specimens of multilayered films for in-situ deformation studies. Of primary importance in the development of this technique is the production of an electron transparent microgauge section using focused ion beam technology. This micro-gauge section predetermines the position at which plastic deformation is initiated; crack nucleation, growth and failure are then subsequently observed.


Author(s):  
Valery Ray

Abstract Gas Assisted Etching (GAE) is the enabling technology for High Aspect Ratio (HAR) circuit access via milling in Focused Ion Beam (FIB) circuit modification. Metal interconnect layers of microelectronic Integrated Circuits (ICs) are separated by Inter-Layer Dielectric (ILD) materials, therefore HAR vias are typically milled in dielectrics. Most of the etching precursor gases presently available for GAE of dielectrics on commercial FIB systems, such as XeF2, Cl2, etc., are also effective etch enhancers for either Si, or/and some of the metals used in ICs. Therefore use of these precursors for via milling in dielectrics may lead to unwanted side effects, especially in a backside circuit edit approach. Making contacts to the polysilicon lines with traditional GAE precursors could also be difficult, if not impossible. Some of these precursors have a tendency to produce isotropic vias, especially in Si. It has been proposed in the past to use fluorocarbon gases as precursors for the FIB milling of dielectrics. Preliminary experimental evaluation of Trifluoroacetic (Perfluoroacetic) Acid (TFA, CF3COOH) as a possible etching precursor for the HAR via milling in the application to FIB modification of ICs demonstrated that highly enhanced anisotropic milling of SiO2 in HAR vias is possible. A via with 9:1 aspect ratio was milled with accurate endpoint on Si and without apparent damage to the underlying Si substrate.


Author(s):  
Jian-Shing Luo ◽  
Hsiu Ting Lee

Abstract Several methods are used to invert samples 180 deg in a dual beam focused ion beam (FIB) system for backside milling by a specific in-situ lift out system or stages. However, most of those methods occupied too much time on FIB systems or requires a specific in-situ lift out system. This paper provides a novel transmission electron microscopy (TEM) sample preparation method to eliminate the curtain effect completely by a combination of backside milling and sample dicing with low cost and less FIB time. The procedures of the TEM pre-thinned sample preparation method using a combination of sample dicing and backside milling are described step by step. From the analysis results, the method has applied successfully to eliminate the curtain effect of dual beam FIB TEM samples for both random and site specific addresses.


2019 ◽  
Author(s):  
Genevieve Buckley ◽  
Gediminas Gervinskas ◽  
Cyntia Taveneau ◽  
Hari Venugopal ◽  
James C. Whisstock ◽  
...  

AbstractCryo-transmission electron tomography (cryo-ET) in association with cryo-focused ion beam (cryo-FIB) milling enables structural biology studies to be performed directly within the cellular environment. Cryo-preserved cells are milled and a lamella with a thickness of 200-300 nm provides an electron transparent window suitable for cryo-ET imaging. Cryo-FIB milling is an effective method, but it is a tedious and time-consuming process, which typically results in ~10 lamellae per day. Here, we introduce an automated method to reproducibly prepare cryo-lamellae on a grid and reduce the amount of human supervision. We tested the routine on cryo-preserved Saccharomyces cerevisiae and demonstrate that this method allows an increased throughput, achieving a rate of 5 lamellae/hour without the need to supervise the FIB milling. We demonstrate that the quality of the lamellae is consistent throughout the preparation and their compatibility with cryo-ET analyses.


1995 ◽  
Vol 380 ◽  
Author(s):  
C. Deng ◽  
J. C. Wu ◽  
C. J. Barbero ◽  
T. W. Sigmon ◽  
M. N. Wybourne

ABSTRACTA fabrication process for sub-100 nm Ge wires on Si substrates is reported for the first time. Wires with a cross section of 6 × 57 nm2 are demonstrated. The wire structures are analyzed by atomic force (AFM), scanning electron (SEM), and transmission electron microscopy (TEM). Sample preparation for TEM is performed using a novel technique using both pre and in situ deposition of multiple protection layers using a Focused Ion Beam (FIB) micromachining system.


2016 ◽  
Vol 22 (6) ◽  
pp. 1350-1359 ◽  
Author(s):  
Xiang Li Zhong ◽  
Sibylle Schilling ◽  
Nestor J. Zaluzec ◽  
M. Grace Burke

AbstractIn recent years, an increasing number of studies utilizing in situ liquid and/or gaseous cell scanning/transmission electron microscopy (S/TEM) have been reported. Because of the difficulty in the preparation of suitable specimens, these environmental S/TEM studies have been generally limited to studies of nanoscale structured materials such as nanoparticles, nanowires, or sputtered thin films. In this paper, we present two methodologies which have been developed to facilitate the preparation of electron-transparent samples from conventional bulk metals and alloys for in situ liquid/gaseous cell S/TEM experiments. These methods take advantage of combining sequential electrochemical jet polishing followed by focused ion beam extraction techniques to create large electron-transparent areas for site-specific observation. As an example, we illustrate the application of this methodology for the preparation of in situ specimens from a cold-rolled Type 304 austenitic stainless steel sample, which was subsequently examined in both 1 atm of air as well as fully immersed in a H2O environment in the S/TEM followed by hyperspectral imaging. These preparation techniques can be successfully applied as a general procedure for a wide range of metals and alloys, and are suitable for a variety of in situ analytical S/TEM studies in both aqueous and gaseous environments.


2007 ◽  
Vol 15 (6) ◽  
pp. 38-39
Author(s):  
D. J. MacMahon ◽  
E. Raz-Moyal

Semiconductor manufacturers are increasingly turning to Transmission Electron Microscopes (TEMs) to monitor product yield and process control, analyze defects, and investigate interface layer morphology. To prepare TEM specimens, Focused Ion Beam (FIB) technology is an invaluable tool, yielding a standard milled TEM lamella approximately 15 μm wide, 5 μm deep and ~100 nm thick. Several techniques have been developed to extract these tiny objects from a large wafer and view it in the TEM. These techniques, including ex-situ lift-out, H-bar, and in-situ lift-out, have different advantages and disadvantages, but all require painstaking preparation of one specimen at a time.


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