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 ◽  
...  

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.

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

Abstract Fast and accurate examination from the bulk to the specific area of the defect in advanced semiconductor devices is critical in failure analysis. This work presents the use of Ar ion milling methods in combination with Ga focused ion beam (FIB) milling as a cutting-edge sample preparation technique from the bulk to specific areas by FIB lift-out without sample-preparation-induced artifacts. The result is an accurately delayered sample from which electron-transparent TEM specimens of less than 15 nm are obtained.


Author(s):  
Woo Jun Kwon ◽  
Jisu Ryu ◽  
Christopher H. Kang ◽  
Michael B. Schmidt ◽  
Nicholas Croy

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.


2019 ◽  
Vol 9 (13) ◽  
pp. 2721 ◽  
Author(s):  
Cédric Barroo ◽  
Austin J. Akey ◽  
David C. Bell

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.


Author(s):  
L. A. Giannuzzi ◽  
P. R. Howell ◽  
H. W. Pickering ◽  
W. R. Bitler

A primary concern involving transmission electron microscopy (TEM) analysis is whether the electron transparent region under investigation is representative of the bulk material. TEM is frequently employed to examine the microstructure of electrodeposited materials due to their small grain size and high dislocation density. Previous work in this laboratory on palladium electrodeposits has shown that deformation twins and diffusion induced recrystallization may be induced during preparation of thin foils using both twin jet electropolishing and ion beam thinning. Recent developments in TEM sample preparation in the physical sciences include a procedure for the cross-section of heterogeneous layered materials which reduces or eliminates the need for ion milling. In this sample preparation technique, a tripod polisher device is used to mechanically polish the specimen to electron transparency. The purpose of this paper is to report on the influence of the tripod polisher sample preparation technique, on the microstructure of zinc electrodeposits.


1998 ◽  
Vol 4 (S2) ◽  
pp. 656-657 ◽  
Author(s):  
David W. Susnitzky ◽  
Kevin D. Johnson

The ongoing reduction of scale of semiconductor device structures places increasing demands on the sample preparation methods used for transmission electron microscopy (TEM). Much of the semiconductor industry's failure analysis and new process development effort requires specific transistor, metal or dielectric structures to be analyzed using TEM techniques. Focused ion beam (FIB) milling has emerged as a valuable technique for site-specific TEM sample preparation. FIB milling, typically with 25-50kV Ga+ ions, enables thin TEM samples to be prepared with submicron precision. However, Ga+ ion milling significantly modifies the surfaces of TEM samples by implantation and amorphization. Previous work using 90° milling angles has shown that Ga+ ion milling of Si produces a surface damage layer that is 280Å thick. This damage is problematical since the current generation of semiconductor devices requires TEM samples in the 500-1000Å thickness range.


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.


2001 ◽  
Vol 7 (1) ◽  
pp. 24-31 ◽  
Author(s):  
D.J. Larson ◽  
B.D. Wissman ◽  
R.L. Martens ◽  
R.J. Viellieux ◽  
T.F. Kelly ◽  
...  

AbstractA sample preparation method has been developed whereby sharp needle-shaped specimens for atom probe analysis are fabricated from multilayer thin films deposited onto silicon substrates. The specimens are fabricated in an orientation such that atom probe composition profiles across the layer interfaces can be determined with atomic-layer spatial resolution, i.e., the layer normals are parallel to the needle axis. The method uses standard silicon etching techniques and focused ion-beam milling. The feasibility and utility of this technique are shown through its application to a NiFe/CoFe/Cu/CoFe-based thin film structure.


2009 ◽  
Vol 633-634 ◽  
pp. 73-84
Author(s):  
Deng Pan ◽  
S. Kuwano ◽  
T. Fujita ◽  
M. W. Chen

Ultra-large compressive plasticity at room temperature has recently been observed in electrodeposited nanocrystalline nickel (nc-Ni) under micro-scale compression (Pan, Kuwano, Fujita and Chen: Nano Lett. Vol. 7 (2007), p. 2108). With aid of a TEM sample preparation technique employing focused ion beam (FIB), TEM observations on deformed nc-Ni evidenced deformation-induced microstructural evolution of nc-Ni at a variety of strain levels: Whilst the deformation increases, substantial grain growth is uncovered in the nc-Ni. No apparent ex situ evidence of intragranular dislocation activities is found in the deformed sample. As thermal diffusion plays an insignificant role in the deformation in nc-Ni at room temperature (~0.17Tm), this premium plasticity is achieved in accommodation with the grain-boundary-mediated deformation, with assistance of extensive grain growth that is mainly driven by high stresses at steady plastic flow.


2021 ◽  
Author(s):  
Tony Colpaert ◽  
Stefaan Verleye

Abstract This paper describes a fast and effective sample preparation method to allow backside fault localization on GaN package devices. Backside analysis by Photon Emission Microscopy (PEM) is becoming preferable to frontside analysis when the die is covered by metal layers. This paper describes an optimized method for backside sample preparation on GaN package devices having a thick heavily doped p-type silicon substrate. The method combines mechanical and chemical deprocessing steps, resulting in a fast and effective sample preparation technique for PEM analysis. Additionally, the laser marking process parameters to facilitate orientation during the final physical failure analysis by Focused Ion Beam (FIB) are also shared.


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