Preparation of TEM samples by focused ion beam (FIB) techniques: applications to the study of clays and phyllosilicates in meteorites

2003 ◽  
Vol 67 (3) ◽  
pp. 581-592 ◽  
Author(s):  
M. R. Lee ◽  
P. A. Bland ◽  
G. Graham
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Mixed Valence ◽  
Planetary Science ◽  
Basal Spacing ◽  
Ion Milling ◽  
Cut Edge ◽  
Transmission Electron ◽  
Study Results ◽  
Argon Ion

AbstractTransmission electron microscope samples were prepared of ALH 78045 and ALH 88045, two clay-and phyllosilicate-bearing Antarctic meteorites, using argon ion milling and focused ion beam (FIB) techniques. ALH 78045 contains clay- and phyllosilicate-filled veins that have formed by terrestrial weathering of olivine, orthopyroxene and metal. Very narrow (∼10 nm) intragranular clay-filled veins could be observed in the TEM samples prepared by argon ion milling, whereas differential thinning and lack of precision in the location of the electron-transparent areas hindered the study of wider (5 — 15 μm) phyllosilicate-filled intergranular veins. Using the FIB instrument, electron-transparent slices were cut from specific parts of the wider veins and lifted out for TEM study. Results show that these veins are occluded by cronstedtite, a mixed-valence Fe-rich phyllosilicate. This discovery shows that silicates can be both dissolved and precipitated during terrestrial weathering within the Antarctic ice. ALH 88045 is one of a small number of known CM1 carbonaceous chondrites. This meteorite is largely composed of flattened ellipsoidal aggregates of serpentine-group phyllosilicates. To determine the mineralogy and texture of phyllosilicates within specific aggregates, TEM samples were prepared by trenching into the cut edge of a sample using the FIB instrument. Results show that Mg-rich aggregates are composed of lath-shaped serpentine crystals with a ∼0.73 nm basal spacing, which is typical of the products of low temperature aqueous alteration within asteroidal parent bodies. Results of this work demonstrate that the FIB has enormous potential in a number of areas of Earth and planetary science.

Low Energy Ar Ion Milling of FIB TEM Specimens from 14 nm and Future FinFET Technologies

2018 ◽  
Author(s):  
C.S. Bonifacio ◽  
P. Nowakowski ◽  
M.J. Campin ◽  
M.L. Ray ◽  
P.E. Fischione
Keyword(s):  
Field Effect Transistor ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Transmission Electron ◽  
High Resolution Tem ◽  
Effect Transistor ◽  
20 Nm ◽  
Argon Ion

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.

Automated End-Point Detection and Targeted Ar+ Milling of Advanced Integrated Circuit FIB TEM Specimens

2017 ◽  
Author(s):  
C.S. Bonifacio ◽  
P. Nowakowski ◽  
M.J. Campin ◽  
J.T. Harbaugh ◽  
M. Boccabella ◽  
...  
Keyword(s):  
Integrated Circuits ◽  
Integrated Circuit ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Specimen Preparation ◽  
Ion Milling ◽  
Transmission Electron ◽  
End Point Detection ◽  
Point Detection ◽  
Argon Ion

Abstract The sub-nanometer resolution that transmission electron microscopy (TEM) provides is critical to the development and fabrication of advanced integrated circuits. TEM specimens are usually prepared using the focused ion beam, which can cause gallium-induced artifacts and amorphization. This work presents the use of a concentrated argon ion beam for reproducible TEM specimen preparation using automatic milling termination and targeted ion milling of device features; the result is high-quality and electron-transparent specimens of less than 30 nm. Such work is relevant for semiconductor product development and failure analysis.

Fast Preparation of Ultrathin FIB Lamellas for MEMs-Based In Situ TEM Experiments

2016 ◽  
Vol 850 ◽  
pp. 722-727 ◽  
Author(s):  
Hui Wang ◽  
Shang Gang Xiao ◽  
Qiang Xu ◽  
Tao Zhang ◽  
Henny Zandbergen
Keyword(s):  
Sample Preparation ◽  
Focused Ion Beam ◽  
Preparation Method ◽  
Ion Beam ◽  
Metallic Alloy ◽  
In Situ Tem ◽  
Ion Milling ◽  
Electrochemical Polishing ◽  
Argon Ion

The preparation of thin lamellas by focused ion beam (FIB) for MEMS-based in situ TEM experiments is time consuming. Typically, the lamellas are of ~5μm*10μm and have a thickness less than 100nm. Here we demonstrate a fast lamellas’ preparation method using special fast cutting by FIB of samples prepared by conventional TEM sample preparation by argon ion milling or electrochemical polishing methods. This method has been applied successfully on various materials, such as ductile metallic alloy Ti68Ta27Al5, brittle ceramics K0.5Na0.5NbO3-6%LiNbO3 and semiconductor Si. The thickness of the lamellas depends on the original TEM sample.

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.

In-Situ Transformation of a Zinc Tem Lift-Out Specimen

1999 ◽  
Vol 5 (S2) ◽  
pp. 928-929
Author(s):  
B.I. Prenitzer ◽  
S. Collins ◽  
L. A. Giannuzzi
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Ion Milling ◽  
Cleaning Operation ◽  
Microstructural Damage ◽  
Transmission Electron ◽  
Metallographic Preparation ◽  
Powder Particles ◽  
Preparation Techniques

The focused ion beam (FIB) lift out (LO) technique has been used to prepare transmission electron microscopy (TEM) specimens from individual Zn powder particles [1]. The Zn microstructure observed by TEM was compared to the Zn microstructure analyzed by traditional metallographic preparation techniques. It was concluded that the Ga focused ion milling produced no apparent microstructural damage to the Zn [1]. A low magnification TEM image of the FIB prepared Zn specimen obtained from a Philips EM430 operating at 300 KeV is shown in figure la.The Zn FIB LO specimen was then processed in a plasma cleaner. After subjecting the Zn specimen to the plasma cleaning operation, the specimen was observed in a Philips EM400 operating at 120 KeV. The Zn specimen completely transformed during in situTEM observation at 120 KeV. The specimen was then subsequently observed in an EM430 to analyze the transformed Zn at 300 KeV.

scholarly journals Having Your Cake and Eating It Too: A Procedure for Obtaining Plan View and Cross Section TEM Images from the Same Site

2005 ◽  
Vol 13 (1) ◽  
pp. 26-29 ◽  
Author(s):  
R.B. Irwin ◽  
A. Anciso ◽  
P.J. Jones ◽  
C. Patton
Keyword(s):  
Sample Preparation ◽  
Cross Section ◽  
Focused Ion Beam ◽  
Bulk Material ◽  
Ion Beam ◽  
Preparation Technique ◽  
Ion Milling ◽  
Plan View ◽  
Transmission Electron ◽  
Final Sample

Sample preparation for Transmission Electron Microscopy (TEM) is usually performed such that the final sample orientation is either a cross section or a plan view of the bulk material, as shown schematically in Figure 1. The object of any sample preparation technique, for either of these two orientations, is to thin a selected volume of the sample from its initial bulk state to electron transparency, ~ 100nm thick. In doing so, the final sample must be mechanically stable, vacuum compatible, and, most of all, unchanged from the initial bulk material. Many techniques have been used to achieve this goal: cleaving, sawing, mechanical polishing, chemical etching, ion milling, focused ion beam (FIB) milling, and many others.

High-Quality Sample Preparation by Low kV FIB Thinning for Analytical TEM Measurements

2007 ◽  
Vol 13 (2) ◽  
pp. 80-86 ◽  
Author(s):  
Sara Bals ◽  
Wim Tirry ◽  
Remco Geurts ◽  
Zhiqing Yang ◽  
Dominique Schryvers
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Beam Specimen ◽  
Specimen Preparation ◽  
Ion Milling ◽  
High Quality ◽  
Transmission Electron ◽  
Quantitative Manner

Focused ion beam specimen preparation has been used for NiTi samples and SrTiO3/SrRuO3 multilayers with prevention of surface amorphization and Ga implantation by a 2-kV cleaning procedure. Transmission electron microscopy techniques show that the samples are of high quality with a controlled thickness over large scales. Furthermore, preferential thinning effects in multicompounds are avoided, which is important when analytical transmission electron microscopy measurements need to be interpreted in a quantitative manner. The results are compared to similar measurements acquired for samples obtained using conventional preparation techniques such as electropolishing for alloys and ion milling for oxides.

Narrow-Beam Argon Ion Milling of Ex Situ Lift-Out FIB Specimens Mounted on Various Carbon-Supported Grids

2018 ◽  
Author(s):  
M. J. Campin ◽  
C. S. Bonifacio ◽  
P. Nowakowski ◽  
P. E. Fischione ◽  
L. A. Giannuzzi
Keyword(s):  
Focused Ion Beam ◽  
Ion Beam ◽  
Semiconductor Industry ◽  
Carbon Support ◽  
Ex Situ ◽  
Specimen Preparation ◽  
Narrow Beam ◽  
Ion Milling ◽  
Preparation Methods ◽  
Argon Ion

Abstract The semiconductor industry recently has been investigating new specimen preparation methods that can improve throughput while maintaining quality. The result has been a combination of focused ion beam (FIB) preparation and ex situ lift-out (EXLO) techniques. Unfortunately, the carbon support on the EXLO grid presents problems if the lamella needs to be thinned once it is on the grid. In this paper, we show how low-energy (< 1 keV), narrow-beam (< 1 μm diameter) Ar ion milling can be used to thin specimens and remove gallium from EXLO FIB specimens mounted on various support grids.

Focused Ion Beam Sectioning and Lift-out Method for Copper and Resist Vias in Organic Low-k Dielectrics

2002 ◽  
Vol 8 (6) ◽  
pp. 502-508 ◽  
Author(s):  
E.J. Crawford ◽  
L. Gignac ◽  
K. Barth ◽  
J. Petrus ◽  
E. Levine
Keyword(s):  
Electron Microscope ◽  
Transmission Electron Microscope ◽  
Focused Ion Beam ◽  
Ion Beam ◽  
Scanning Transmission Electron Microscope ◽  
Sem Analysis ◽  
Ex Situ ◽  
Ion Milling ◽  
Transmission Electron ◽  
Low K

The focused ion beam lift-out technique for scanning electron microscope (SEM) and transmission electron microscope (TEM) sample preparation was shown to be applicable to copper/low-k dielectric semiconductor technology. High resolution SEM, TEM, and scanning transmission electron microscope analyses were performed on metal contacts and resist vias with no evidence of the interface damage or metal smearing commonly observed with mechanical polishing. Ion milling of the sample ex situ to the substrate provided decoration and adjustment of the exposed plane of the section when necessary for SEM analysis.

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