scholarly journals A versatile cryo-transfer system, connecting cryogenic focused ion beam sample preparation to atom probe microscopy

PLoS ONE ◽  
2021 ◽  
Vol 16 (1) ◽  
pp. e0245555
Author(s):  
Chandra Macauley ◽  
Martina Heller ◽  
Alexander Rausch ◽  
Frank Kümmel ◽  
Peter Felfer
Keyword(s):  
Sample Preparation ◽  
Focused Ion Beam ◽  
Environmental Control ◽  
Structural Information ◽  
Morphological Changes ◽  
Ion Beam ◽  
Atom Probe ◽  
Al Alloy ◽  
Transfer System ◽  
Ambient Conditions

Atom probe tomography (APT) is a powerful technique to obtain 3D chemical and structural information, however the ‘standard’ atom probe experimental workflow involves transfer of specimens at ambient conditions. The ability to transfer air- or thermally-sensitive samples between instruments while maintaining environmental control is critical to prevent chemical or morphological changes prior to analysis for a variety of interesting sample materials. In this article, we describe a versatile transfer system that enables cryogenic- or room-temperature transfer of specimens in vacuum or atmospheric conditions between sample preparation stations, a focused ion beam system (Zeiss Crossbeam 540) and a widely used commercial atom probe system (CAMECA LEAP 4000X HR). As an example for the use of this transfer system, we present atom probe data of gallium- (Ga)-free grain boundaries in an aluminum (Al) alloy specimen prepared with a Ga-based FIB.

Automated Sample Depth Targeting with Low kV Cleaning by Focused Ion Beam Microscopy for Atom Probe Tomography

2020 ◽  
Author(s):  
Woo Jun Kwon ◽  
Jisu Ryu ◽  
Christopher H. Kang ◽  
Michael B. Schmidt ◽  
Nicholas Croy
Keyword(s):  
Sample Preparation ◽  
Atom Probe Tomography ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Region Of Interest ◽  
Atom Probe ◽  
Sample Volume ◽  
Cleaning Process ◽  
Site Specific ◽  
Sample Depth

Abstract Focused ion beam (FIB) microscopy is an essential technique for the site-specific sample preparation of atom probe tomography (APT). The site specific APT and automated APT sample preparation by FIB have allowed increased APT sample volume. In the workflow of APT sampling, it is very critical to control depth of the sample where exact region of interest (ROI) for accurate APT analysis. Very precise depth control is required at low kV cleaning process in order to remove the damaged layer by previous high kV FIB process steps. We found low kV cleaning process with 5 kV and followed by 2kV beam conditions delivers better control to reached exact ROI on Z direction. This understanding is key to make APT sample with fully automated fashion.

Preparation of 3D Atom Probe Samples of Multilayered Film Structures using a Focused Ion Beam

2000 ◽  
Vol 6 (S2) ◽  
pp. 522-523 ◽  
Author(s):  
R. L. Martens ◽  
D. J. Larson ◽  
T. F. Kelly ◽  
A. Cerezo ◽  
P.’H. Clifton ◽  
...  
Keyword(s):  
Sample Preparation ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Deposition Process ◽  
Atom Probe ◽  
Film Structure ◽  
Preparation Technique ◽  
Preparation Methods ◽  
Recent Developments ◽  
Previous Sample

Focused ion beam (FIB) instruments have become essential for the preparation of atom probe samples from heterogeneous materials. Previous sample preparation methods such as electropolishing are limited in their application due to either geometrical or electrochemical constraints. Recent developments in sample preparation using a FIB have enabled the production of AP samples from various materials and, more importantly, from non-traditional sample geometries that contain multilayered thin film structures (MLF).Most sample preparation using a FIB first involves a sample that has been reduced in size through some manual sample preparation technique like tripod polishing or cutting. Smaller, thinner samples require less milling time in the FIB. A silicon wafer etched with the “Bosch” process was used to produce a surface that contains millions of 20, 16, 12, 8, and 4 μm square by -180 μrn long “posts”, Fig. 1. A multilayer film structure is deposited on the flat surface of the silicon posts in a standard deposition process.

Nanocomposite Polyurethane Foams Via POSS Blends

2002 ◽  
Vol 733 ◽  
Author(s):  
Brock McCabe ◽  
Steven Nutt ◽  
Brent Viers ◽  
Tim Haddad
Keyword(s):  
High Temperature ◽  
Sample Preparation ◽  
Room Temperature ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Polyurethane Foams ◽  
Development Projects ◽  
Polymer Systems ◽  
Polyurethane Resin ◽  
Military Development

AbstractPolyhedral Oligomeric Silsequioxane molecules have been incorporated into a commercial polyurethane formulation to produce nanocomposite polyurethane foam. This tiny POSS silica molecule has been used successfully to enhance the performance of polymer systems using co-polymerization and blend strategies. In our investigation, we chose a high-temperature MDI Polyurethane resin foam currently used in military development projects. For the nanofiller, or “blend”, Cp7T7(OH)3 POSS was chosen. Structural characterization was accomplished by TEM and SEM to determine POSS dispersion and cell morphology, respectively. Thermal behavior was investigated by TGA. Two methods of TEM sample preparation were employed, Focused Ion Beam and Ultramicrotomy (room temperature).

TEM Sample Preparation Tricks for Advanced DRAMs

2015 ◽  
Author(s):  
Ching Shan Sung ◽  
Hsiu Ting Lee ◽  
Jian Shing Luo
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Integrated Circuit ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Tem Analysis ◽  
Cross Sectional ◽  
Transmission Electron ◽  
Characterization Of Materials

Abstract Transmission electron microscopy (TEM) plays an important role in the structural analysis and characterization of materials for process evaluation and failure analysis in the integrated circuit (IC) industry as device shrinkage continues. It is well known that a high quality TEM sample is one of the keys which enables to facilitate successful TEM analysis. This paper demonstrates a few examples to show the tricks on positioning, protection deposition, sample dicing, and focused ion beam milling of the TEM sample preparation for advanced DRAMs. The micro-structures of the devices and samples architectures were observed by using cross sectional transmission electron microscopy, scanning electron microscopy, and optical microscopy. Following these tricks can help readers to prepare TEM samples with higher quality and efficiency.

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.

A Methodology to Reduce Ion Beam Induced Damage in TEM Specimens Prepared by FIB

2002 ◽  
Author(s):  
Chin Kai Liu ◽  
Chi Jen. Chen ◽  
Jeh Yan.Chiou ◽  
David Su
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Sample Preparation ◽  
Integrated Circuit ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Tem Analysis ◽  
Sensitive Issue ◽  
Transmission Electron

Abstract Focused ion beam (FIB) has become a useful tool in the Integrated Circuit (IC) industry, It is playing an important role in Failure Analysis (FA), circuit repair and Transmission Electron Microscopy (TEM) specimen preparation. In particular, preparation of TEM samples using FIB has become popular within the last ten years [1]; the progress in this field is well documented. Given the usefulness of FIB, “Artifact” however is a very sensitive issue in TEM inspections. The ability to identify those artifacts in TEM analysis is an important as to understanding the significance of pictures In this paper, we will describe how to measure the damages introduced by FIB sample preparation and introduce a better way to prevent such kind of artifacts.

Solving the Voltage Contrast on Floating Substrate with Standard FA Toolset

2016 ◽  
Author(s):  
Julien Goxe ◽  
Béatrice Vanhuffel ◽  
Marie Castignolles ◽  
Thomas Zirilli
Keyword(s):  
Electron Microscope ◽  
Scanning Electron Microscope ◽  
Sample Preparation ◽  
Failure Analysis ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Silicon On Insulator ◽  
Mixed Signal ◽  
Voltage Contrast ◽  
Scanning Electron

Abstract Passive Voltage Contrast (PVC) in a Scanning Electron Microscope (SEM) or a Focused Ion Beam (FIB) is a key Failure Analysis (FA) technique to highlight a leaky gate. The introduction of Silicon On Insulator (SOI) substrate in our recent automotive analog mixed-signal technology highlighted a new challenge: the Bottom Oxide (BOX) layer, by isolating the Silicon Active Area from the bulk made PVC technique less effective in finding leaky MOSFET gates. A solution involving sample preparation performed with standard FA toolset is proposed to enhance PVC on SOI substrate.

High-Throughput, Site-Specific Sample Prep of Ultra-Thin TEM Lamella for Process Metrology and Failure Analysis

2012 ◽  
Author(s):  
Roger Alvis ◽  
Jeff Blackwood ◽  
Sang-Hoon Lee ◽  
Matthew Bray
Keyword(s):  
Sample Preparation ◽  
Failure Analysis ◽  
Process Monitoring ◽  
High Throughput ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Memory Devices ◽  
Site Specific ◽  
Critical Dimensions ◽  
Tem Lamella

Abstract Semiconductor devices with critical dimensions less than 20nm are now being manufactured in volume. A challenge facing the failure analysis and process-monitoring community is two-fold. The first challenge of TEM sample prep of such small devices is that the basic need to end-point on a feature-of-interest pushes the imaging limit of the instrument being used to prepare the lamella. The second challenge posed by advanced devices is to prepare an artifact-free lamella from non-planar devices such as finFETs as well as from structures incorporating ‘non-traditional’ materials. These challenges are presently overcome in many advanced logic and memory devices in the focused ion beam-based TEM sample preparation processes by inverting the specimen prior to thinning to electron transparency. This paper reports a highthroughput method for the routine preparation of artifact-free TEM lamella of 20nm thickness, or less.

Metallic Nanoneedles Arrays for TEM Sample Preparation “Lift-Out”

2012 ◽  
Author(s):  
Romaneh Jalilian ◽  
David Mudd ◽  
Neil Torrez ◽  
Jose Rivera ◽  
Mehdi M. Yazdanpanah ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
Electron Microscope ◽  
Sample Preparation ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Beam System ◽  
Transmission Electron ◽  
Nanoneedle Array ◽  
Superior Mechanical Properties ◽  
And Performance

Abstract The sample preparation for transmission electron microscope can be done using a method known as "lift-out". This paper demonstrates a method of using a silver-gallium nanoneedle array for a quicker sharpening process of tungsten probes with better sample viewing, covering the fabrication steps and performance of needle-tipped probes for lift-out process. First, an array of high aspect ratio silver-gallium nanoneedles was fabricated and coated to improve their conductivity and strength. Then, the nanoneedles were welded to a regular tungsten probe in the focused ion beam system at the desired angle, and used as a sharp probe for lift-out. The paper demonstrates the superior mechanical properties of crystalline silver-gallium metallic nanoneedles. Finally, a weldless lift-out process is described whereby a nano-fork gripper was fabricated by attaching two nanoneedles to a tungsten probe.

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