Optimization Based Geometric Modeling of Nano/Micro Scale Ion Milling of Organic Materials for Multidimensional Bioimaging

Author(s):  
Jing Fu ◽  
Sanjay Joshi

Focused ion beam (FIB) instruments have recently started to be seen in applications to organic materials such as polymers and biological samples. FIB provides a novel tool for sectioning biological samples for electron microscope based imaging or microfabrication with environment friendly materials. The modeling of nano/micro scale geometry accurately sculptured by FIB milling is crucial for generating the milling plan and process control, and for computer simulation based prediction and visualization of the milled geometry. However, modeling of the milled geometry on compound materials, especially for high aspect ratio feature, is still difficult due to the complexity of target material, as well as multiple physical and chemical interactions involved. In this study, a comprehensive model of ion milling with organic targets is presented to address the challenges in using a simulation based approach. At each discrete point of the milled front, the depth is the dynamic result of aggregate interactions from neighboring areas, including physical sputtering and chemical reactions. Instead of determining the exact interactions, the parameters of the proposed model are estimated by studying a number of preliminary milling results followed by a nonlinear optimization model. This platform has been validated by milling different features on water ice in a cryogenic environment, and the simulation and experiment results show great consistency. With the proliferation of nanotechnology in biomedical and biomaterial domains, the proposed approach is expected to be a flexible tool for various applications involving novel and heterogeneous biological targets.

Author(s):  
Jing Fu ◽  
Sanjay B. Joshi

Recently, Focused Ion Beam (FIB) instruments have begun be applied to organic materials such as polymers and biological systems. This provides a novel tool for sectioning biological samples for analysis, or microfabrication with environment friendly materials. The modeling of nano/micro scale geometry accurately sculptured by FIB milling is crucial for generating the milling plan and process control, and for computer simulation for prediction and visualization of the milled geometry. However, modeling of the ion milling process on compound materials, especially for high aspect ratio feature, is still difficult due to the complexity of target material, as well as multiple physical and chemical interactions involved. In this study, a comprehensive model of ion milling with organic targets is presented to address the challenges using a simulation based approach. This platform has also been validated by milling different features on water ice in a cryogenic environment, and the simulation and experiment results show great consistency. With the proliferation of nanotechnology to biomedical and biomaterial domains, the proposed approach is expected to be a flexible tool for various applications involving novel and heterogeneous milling targets.


2018 ◽  
Author(s):  
C.S. Bonifacio ◽  
P. Nowakowski ◽  
M.J. Campin ◽  
M.L. Ray ◽  
P.E. Fischione

Abstract Transmission electron microscopy (TEM) specimens are typically prepared using the focused ion beam (FIB) due to its site specificity, and fast and accurate thinning capabilities. However, TEM and high-resolution TEM (HRTEM) analysis may be limited due to the resulting FIB-induced artifacts. This work identifies FIB artifacts and presents the use of argon ion milling for the removal of FIB-induced damage for reproducible TEM specimen preparation of current and future fin field effect transistor (FinFET) technologies. Subsequently, high-quality and electron-transparent TEM specimens of less than 20 nm are obtained.


Author(s):  
Thomas M. Moore

Abstract The availability of the focused ion beam (FIB) microscope with its excellent imaging resolution, depth of focus and ion milling capability has made it an appealing platform for materials characterization at the sub-micron, or "nano" level. This article focuses on nanomechanical characterization in the FIB, which is an extension of the FIB capabilities into the realm of nano-technology. It presents examples that demonstrate the power and flexibility of nanomechanical testing in the FIB or scanning electron microscope with a probe shaft that includes a built-in strain gauge. Loads that range from grams to micrograms are achievable. Calibration is limited only by the availability of calibrated load cells in the smallest load ranges. Deflections in the range of a few nanometers range can be accurately applied. Simultaneous electrical, mechanical, and visual data can be combined to provide a revealing study of physical behavior of complex and dynamic nanostructures.


2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Alexey A. Polilov ◽  
Anastasia A. Makarova ◽  
Song Pang ◽  
C. Shan Xu ◽  
Harald Hess

AbstractModern morphological and structural studies are coming to a new level by incorporating the latest methods of three-dimensional electron microscopy (3D-EM). One of the key problems for the wide usage of these methods is posed by difficulties with sample preparation, since the methods work poorly with heterogeneous (consisting of tissues different in structure and in chemical composition) samples and require expensive equipment and usually much time. We have developed a simple protocol allows preparing heterogeneous biological samples suitable for 3D-EM in a laboratory that has a standard supply of equipment and reagents for electron microscopy. This protocol, combined with focused ion-beam scanning electron microscopy, makes it possible to study 3D ultrastructure of complex biological samples, e.g., whole insect heads, over their entire volume at the cellular and subcellular levels. The protocol provides new opportunities for many areas of study, including connectomics.


2015 ◽  
Vol 665 ◽  
pp. 169-172
Author(s):  
Yoshimasa Takahashi ◽  
Hikaru Kondo ◽  
Kazuya Aihara ◽  
Masanori Takuma ◽  
Kenichi Saitoh ◽  
...  

The strength against interfacial fracture initiation from a free-edge of Si/Cu micro-components was evaluated. The micro-scale cantilever specimens containing dissimilar interfaces were fabricated with a focused-ion-beam (FIB) technique, and they were loaded with a quantitative nanoindenter holder operated in a transmission electron microscope (TEM). The specimens were successfully fractured along the Si/Cu interface, and the critical loads at fracture were measured. The critical stress distribution near the free-edge was evaluated with the finite element method (FEM). The near-edge stress distributions of 90°/90°-shaped specimens were scattered while those of 135°/135°-shaped specimens were in good agreement despite the difference in specimen dimensions. Such a difference was discussed in terms of the relation between the magnitude of stress singularity and the microstructures of material.


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.


1999 ◽  
Vol 5 (S2) ◽  
pp. 740-741 ◽  
Author(s):  
C.A. Urbanik ◽  
B.I. Prenitzer ◽  
L.A. Gianhuzzi ◽  
S.R. Brown ◽  
T.L. Shofner ◽  
...  

Focused ion beam (FIB) instruments are useful for high spatial resolution milling, deposition, and imaging capabilities. As a result, FIB specimen preparation techniques have been widely accepted within the semiconductor community as a means to rapidly prepare high quality, site-specific specimens for transmission electron microscopy (TEM) [1]. In spite of the excellent results that have been observed for both high resolution (HREM) and standard TEM specimen preparation applications, a degree of structural modification is inherent to FIB milled surfaces [2,3]. The magnitude of the damage region that results from Ga+ ion bombardment is dependent on the operating parameters of the FIB (e.g., beam current, beam voltage, milling time, and the use of reactive gas assisted etching).Lattice defects occur as a consequence of FIB milling because the incident ions transfer energy to the atoms of the target material. Momentum transferred from the incident ions to the target atoms can result in the creation of point defects (e.g., vacancies, self interstitials, and interstitial and substitutional ion implantation), the generation of phonons, and plasmon excitation in the case of metal targets.


2006 ◽  
Vol 983 ◽  
Author(s):  
Yuhong Wu ◽  
Meng Qu ◽  
Lucille A Giannuzzi ◽  
Sanjay Sampath ◽  
Andrew Gouldstone

AbstractThermally sprayed (TS) coatings are widely used for surface engineering across a range of industries, including aerospace, infrastructure and biomedical. TS materials are formed via the successive impingement, rapid quenching and build-up of molten powder particles on a substrate. The impacted ‘splats’ are thus the fundamental microstructural constituents of the coatings, and their intrinsic properties, as well as intersplat bonding and morphology, dictate coating behavior. Beyond the obvious practical considerations, from a scientific standpoint, splats represent a fascinating template for study, due to the highly non-equilibrium processing conditions (rapid deceleration from sub-sonic velocities, million-degree/sec cooling rates). In the literature, many studies of isolated splats on substrates have been carried out, but these have focused on overall morphology (disc-shape vs fragmented). Direct observations of microstructure, in particular cross-section, are limited in the specimen preparation stage due to splat size (tens of microns in diameter, 1-2 microns in thickness). However, Focused Ion Beam (FIB) techniques have allowed this problem to be addressed in a robust manner; in this paper we will discuss such approaches to observe Ni5Al splats on stainless steel substrates. Cross-sections through the splat and the substrate were created by recourse to ion milling and the ion beam itself provided good channeling contrast for grain imaging. The typical splat microstructure with sub-micron Ni(Al) columnar grains, a chill zone at the bottom and a lift off area is observed in high detail. In addition, an amorphous aluminum oxide top layer of 100-200 nm is partially present on top of the Ni(Al) columnar grains. At the splat/substrate interface, defects such as micro- and nano-scale pores were characterized for the first time and will be discussed. These observations provide insights into splat and interface formation during the deposition process and may drastically improve our current understanding of Ni5Al splat properties.


1997 ◽  
Vol 3 (S2) ◽  
pp. 357-358
Author(s):  
C. Amy Hunt

The demand for TEM analysis in semiconductor failure analysis is rising sharply due to the shrinking size of devices. A well-prepared sample is a necessity for getting meaningful results. In the past decades, a significant amount of effort has been invested in improving sample preparation techniques for TEM specimens, especially precision cross-sectioning techniques. The most common methods of preparation are mechanical dimpling & ion milling, focused ion beam milling (FIBXTEM), and wedge mechanical polishing. Each precision XTEM technique has important advantages and limitations that must be considered for each sample.The concept for both dimpling & ion milling and wedge specimen preparation techniques is similar. Both techniques utilize mechanical polishing to remove the majority of the unwanted material, followed by ion milling to assist in final polishing or cleaning. Dimpling & ion milling produces the highest quality samples and is a relatively easy technique to master.


1999 ◽  
Vol 5 (S2) ◽  
pp. 898-899
Author(s):  
D. Delille ◽  
R. Pantel ◽  
G. Auvert ◽  
E. Van Cappellen

1. IntroductionThe FIB (focused ion beam) is now widely accepted as the most site-specific TEM preparation tool and as such proves to be highly valuable when analysing ULSI devices. However, using high-energy Gallium ions for milling induces amorphization of the crystal surfaces. A method able to quantify this surface alteration on silicon using a combination of CBED (convergent beam electron diffraction) and EELS (electron energy loss spectroscopy) is presented. CBED is a powerful tool that also can generate an accurate measure of crystal thickness. EELS can yield the total sample thickness, so from the difference the combined amorphous layers can be assessed. Two sets of application results are presented: the first one is obtained on a FIB thinned sample using an ion energy of 50 keV and the second set of results confirms the validity of the proposed method on a mechanically polished specimen with no subsequent ion milling.


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