Failure Analysis of Electronic Material Using Cryogenic FIB-SEM

2012 ◽  
Author(s):  
Nicholas Antoniou ◽  
Adam Graham ◽  
Cheryl Hartfield ◽  
Gonzalo Amador
Keyword(s):  
Integrated Circuits ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Bulk Sample ◽  
Copper Metallization ◽  
Cryogenic Temperatures ◽  
Transmission Electron ◽  
Specific Analysis ◽  
Change Chemical Composition

Abstract Two-beam systems (focused ion beam (FIB) integrated with a scanning electron microscope (SEM)) have enabled site-specific analysis at the nano-scale through in situ “mill and view” capability at high resolution. In addition, a FIB-SEM can be used to cut away a lamella from a bulk sample and thin it for transmission electron microscopy (TEM) imaging. We studied the temperature dependence of FIB milling on compound semiconductors and thin films such as copper that are used in integrated circuits. These materials (GaAs, GaN, InN, etc) react chemically and physically with the gallium in the FIB and change chemical composition and may also change morphology. Copper metallization of IC’s has been difficult to mill without undesirable side effects. FIB milling for analysis of these materials becomes difficult if not impossible. Since temperature can be a big factor in chemical and physical reactions we investigated this and report here the effect of cooling the sample to cryogenic temperatures while milling. In addition, we report on the development of a process to prepare TEM lamellae with FIB entirely in a cryogenic environment.

To Eliminate Curtain Effect of FIB TEM Samples by a Combination of Sample Dicing and Backside Milling

2014 ◽  
Author(s):  
Jian-Shing Luo ◽  
Hsiu Ting Lee
Keyword(s):  
Sample Preparation ◽  
Focused Ion Beam ◽  
Preparation Method ◽  
Low Cost ◽  
Ion Beam ◽  
Sample Preparation Method ◽  
Site Specific ◽  
Dual Beam ◽  
Transmission Electron

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.

scholarly journals Automated cryo-lamella preparation for high-throughput in-situ structural biology

2019 ◽  
Author(s):  
Genevieve Buckley ◽  
Gediminas Gervinskas ◽  
Cyntia Taveneau ◽  
Hari Venugopal ◽  
James C. Whisstock ◽  
...  
Keyword(s):  
Saccharomyces Cerevisiae ◽  
Structural Biology ◽  
Focused Ion Beam ◽  
Electron Tomography ◽  
Ion Beam ◽  
Automated Method ◽  
Cellular Environment ◽  
Transmission Electron

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.

Formation of Sub-100 NM GE Wires on Si by E-Beam Evaporation/Lithography

1995 ◽  
Vol 380 ◽  
Author(s):  
C. Deng ◽  
J. C. Wu ◽  
C. J. Barbero ◽  
T. W. Sigmon ◽  
M. N. Wybourne
Keyword(s):  
Cross Section ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Si Substrates ◽  
Novel Technique ◽  
Atomic Force ◽  
Transmission Electron ◽  
First Time ◽  
Scanning Electron

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.

scholarly journals Sample Preparation Methodologies for In Situ Liquid and Gaseous Cell Analytical Transmission Electron Microscopy of Electropolished Specimens

2016 ◽  
Vol 22 (6) ◽  
pp. 1350-1359 ◽  
Author(s):  
Xiang Li Zhong ◽  
Sibylle Schilling ◽  
Nestor J. Zaluzec ◽  
M. Grace Burke
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
General Procedure ◽  
Ion Beam ◽  
Metals And Alloys ◽  
Stainless Steel Sample ◽  
Transmission Electron ◽  
Wide Range

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.

scholarly journals Computer-Controlled Polishing System For Preparing Multiple Pre-FIB TEM Specimens

2007 ◽  
Vol 15 (6) ◽  
pp. 38-39
Author(s):  
D. J. MacMahon ◽  
E. Raz-Moyal
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Product Yield ◽  
Interface Layer ◽  
Ex Situ ◽  
Advantages And Disadvantages ◽  
Transmission Electron ◽  
Invaluable Tool ◽  
Electron Microscopes

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.

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

1996 ◽  
Vol 439 ◽  
Author(s):  
Miyoko Tanaka ◽  
Kazuo Furuya ◽  
Tetsuya Saito
Keyword(s):  
Structural Changes ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Dark Field ◽  
In Situ Tem ◽  
Si Substrate ◽  
Ion Beam Modification ◽  
Surrounding Matrix ◽  
Transmission Electron

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.

scholarly journals Mechanical and Compositional Implications of Gallium Ion Milling on Epoxy Resin

Polymers ◽  
2021 ◽  
Vol 13 (16) ◽  
pp. 2640
Author(s):  
Raz Samira ◽  
Atzmon Vakahi ◽  
Rami Eliasy ◽  
Dov Sherman ◽  
Noa Lachman
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Soft Materials ◽  
Morphological Data ◽  
Ion Milling ◽  
Element Analysis ◽  
Transmission Electron ◽  
Direct Measurements ◽  
Quantitative Results

Focused Ion Beam (FIB) is one of the most common methods for nanodevice fabrication. However, its implications on mechanical properties of polymers have only been speculated. In the current study, we demonstrated flexural bending of FIB-milled epoxy nanobeam, examined in situ under a transmission electron microscope (TEM). Controllable displacement was applied, while real-time TEM videos were gathered to produce morphological data. EDS and EELS were used to characterize the compositions of the resultant structure, and a computational model was used, together with the quantitative results of the in situ bending, to mechanically characterize the effect of Ga+ ions irradiation. The damaged layer was measured at 30 nm, with high content of gallium (40%). Examination of the fracture revealed crack propagation within the elastic region and rapid crack growth up to fracture, attesting to enhanced brittleness. Importantly, the nanoscale epoxy exhibited a robust increase in flexural strength, associated with chemical tempering and ion-induced peening effects, stiffening the outer surface. Young’s modulus of the stiffened layer was calculated via the finite element analysis (FEA) simulation, according to the measurement of 30 nm thickness in the STEM and resulted in a modulus range of 30–100 GPa. The current findings, now established in direct measurements, pave the way to improved applications of polymers in nanoscale devices to include soft materials, such as polymer-based composites and biological samples.

TEM Sample Preparation Using A Focused Ion Beam and A Probe Manipulator

1996 ◽  
Author(s):  
L.R. Herlinger ◽  
S. Chevacharoenkul ◽  
D.C. Erwin
Keyword(s):  
Electron Microscope ◽  
Integrated Circuits ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specific Area ◽  
Sem Analysis ◽  
Imaging Analysis ◽  
Mechanical Grinding ◽  
Transmission Electron ◽  
Multiple Samples

Abstract Cross-sectioning is a necessary technique for the failure analysis of integrated circuits. Historically, the majority of samples have been prepared for scanning electron microscope (SEM) analysis. Today's smaller geometry devices, however, increasingly require the improved spatial resolution afforded by the transmission electron microscope (TEM), both in imaging analysis and in elemental analysis. Specific-area cross-section TEM (SAXTEM) analysis allows the failure analyst to identify defects that may go undiscovered in the SEM. A procedure is described for a timely preparation of SAXTEM samples using a focused ion beam (FIB) instrument and a manipulator probe. This procedure extends the state-of-the-art in several key respects: A) no mechanical grinding is necessary, B) samples as large as the FIB chamber can be accommodated, e.g., whole wafers, C) multiple samples can be prepared from one die, D) the procedure is faster and more repeatable than previously reported procedures.

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