scholarly journals Atom Probe Tomography for Catalysis Applications: A Review

2019 ◽  
Vol 9 (13) ◽  
pp. 2721 ◽  
Author(s):  
Cédric Barroo ◽  
Austin J. Akey ◽  
David C. Bell
Keyword(s):  
Sample Preparation ◽  
Atom Probe Tomography ◽  
Ion Beam ◽  
3D Structure ◽  
Atom Probe ◽  
Atomic Scale ◽  
High Mass ◽  
Preparation Methods ◽  
Catalytic Materials ◽  
Sample Preparation Methods

Atom probe tomography is a well-established analytical instrument for imaging the 3D structure and composition of materials with high mass resolution, sub-nanometer spatial resolution and ppm elemental sensitivity. Thanks to recent hardware developments in Atom Probe Tomography (APT), combined with progress on site-specific focused ion beam (FIB)-based sample preparation methods and improved data treatment software, complex materials can now be routinely investigated. From model samples to complex, usable porous structures, there is currently a growing interest in the analysis of catalytic materials. APT is able to probe the end state of atomic-scale processes, providing information needed to improve the synthesis of catalysts and to unravel structure/composition/reactivity relationships. This review focuses on the study of catalytic materials with increasing complexity (tip-sample, unsupported and supported nanoparticles, powders, self-supported catalysts and zeolites), as well as sample preparation methods developed to obtain suitable specimens for APT experiments.

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.

Optimization of TEM Sample Preparation to Reduce the Overlapping of TEM Images

2014 ◽  
Author(s):  
Shuqing Duan ◽  
Summer Chen ◽  
Paul Yu ◽  
Ming Li ◽  
Mark Zhang ◽  
...  
Keyword(s):  
Sample Preparation ◽  
Cross Section ◽  
Ion Beam ◽  
Top Down ◽  
Preparation Methods ◽  
Plan View ◽  
Transmission Electron ◽  
Focus Ion Beam ◽  
Sample Preparation Methods ◽  
Section Sample

Abstract This paper reports optimized Transmission Electron Microscopy (TEM) sample preparation methods with Focus Ion Beam (FIB), which are used to reduce or avoid the overlapping of TEM images. Several examples of optimized cross-section sample preparation on 38nm and 45nm pitch are provided with general and novel FIB methods. And its application to plan view TEM sample preparation is also shown. The results establish that the proposed method is useful to reduce or remove pattern overlapping effects in dense structures and can produce higher quality TEM images than can be obtained using conventional top-down FIB-based TEM preparation methods.

Interface Segregation and Nitrogen Measurement in Fe–Mn–N Steel by Atom Probe Tomography

2017 ◽  
Vol 23 (2) ◽  
pp. 385-395 ◽  
Author(s):  
Brian Langelier ◽  
Hugo P. Van Landeghem ◽  
Gianluigi A. Botton ◽  
Hatem S. Zurob
Keyword(s):  
Sample Preparation ◽  
Atom Probe Tomography ◽  
Binary Systems ◽  
Ion Beam ◽  
Atom Probe ◽  
Transformation Kinetic ◽  
Ion Milling ◽  
Voltage Versus ◽  
N Concentration ◽  
Interface Segregation

AbstractImproved understanding of the interactions between solutes and the austenite/ferrite interface can benefit modeling of ferrite growth during austenite decomposition, as the transformation kinetic is significantly affected by solutes that influence interface mobility. Solute-interface interactions dominate solute segregation at the interface in binary systems, but in multi-component alloys, solute–solute interactions may also affect segregation. In this study, interface segregation in Fe–Mn–N is examined and compared with Fe–Mn–C, to reveal the extent to which C affects the segregation of Mn. Atom probe tomography (APT) is well-suited to analyze solute concentrations across the interface, as this technique combines high spatial resolution and compositional sensitivity. Measurements of Mn show that segregation is only observed for Fe–Mn–C. This demonstrates that Mn segregation is primarily driven by an affinity for C, which also segregates to the interface. However, the measurement of N in steels by APT may be affected by a variety of experimental factors. Therefore, in verifying the Fe–Mn–N result, systematic examination is conducted on the influence of pulsing method (voltage versus laser), sample preparation (ion milling versus electropolishing), and vacuum storage on the measured N concentration. Both laser pulsing and focused ion beam sample preparation are observed to decrease the apparent N concentration.

Overview: Recent Progress in Three-Dimensional Atom Probe Instruments and Applications

2007 ◽  
Vol 13 (6) ◽  
pp. 408-417 ◽  
Author(s):  
Alfred Cerezo ◽  
Peter H. Clifton ◽  
Sergio Lozano-Perez ◽  
Peter Panayi ◽  
Gang Sha ◽  
...  
Keyword(s):  
Focused Ion Beam ◽  
Materials Science ◽  
Ion Beam ◽  
Three Dimensional ◽  
Atom Probe ◽  
High Mass ◽  
Large Field ◽  
Specimen Preparation ◽  
Preparation Methods ◽  
Energy Compensation

Over the last few years there have been significant developments in the field of three-dimensional atom probe (3DAP) analysis. This article reviews some of the technical compromises that have led to different instrument designs and the recent improvements in performance. An instrument has now been developed, based around a novel reflectron configuration combining both energy compensation and focusing elements, that yields a large field of view and very high mass resolution. The use of laser pulsing in the 3DAP, together with developments in specimen preparation methods using a focused ion-beam instrument, have led to a significant widening in the range of materials science problems that can be addressed with the 3DAP. Recent studies of semiconductor materials and devices are described.

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.

Improving Sample Preparation Methods For Cannabis-Infused Edible And Topical Products

Planta Medica ◽  
2016 ◽  
Vol 82 (05) ◽  
Author(s):  
M Wilcox ◽  
M Jacyno ◽  
J Marcu ◽  
J Neal-Kababick
Keyword(s):  
Sample Preparation ◽  
Preparation Methods ◽  
Sample Preparation Methods

Thin-Die Flip Chip Physical-FA Process Flow

2002 ◽  
Author(s):  
Andrew J. Komrowski ◽  
N. S. Somcio ◽  
Daniel J. D. Sullivan ◽  
Charles R. Silvis ◽  
Luis Curiel ◽  
...  
Keyword(s):  
Sample Preparation ◽  
Failure Analysis ◽  
Flip Chip ◽  
Semiconductor Industry ◽  
Organic Substrate ◽  
Fault Isolation ◽  
Preparation Methods ◽  
Chip Technology ◽  
Isolation Test ◽  
Sample Preparation Methods

Abstract The use of flip chip technology inside component packaging, so called flip chip in package (FCIP), is an increasingly common package type in the semiconductor industry because of high pin-counts, performance and reliability. Sample preparation methods and flows which enable physical failure analysis (PFA) of FCIP are thus in demand to characterize defects in die with these package types. As interconnect metallization schemes become more dense and complex, access to the backside silicon of a functional device also becomes important for fault isolation test purposes. To address these requirements, a detailed PFA flow is described which chronicles the sample preparation methods necessary to isolate a physical defect in the die of an organic-substrate FCIP.

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