Imaging Thin Films of Nanoporous Low-k Dielectrics: Comparison between Ultramicrotomy and Focused Ion Beam Preparations for Transmission Electron Microscopy

2005 ◽  
Vol 12 (2) ◽  
pp. 156-159 ◽  
Author(s):  
Leslie E. Thompson ◽  
Philip M. Rice ◽  
Eugene Delenia ◽  
Victor Y. Lee ◽  
Phillip J. Brock ◽  
...  

Ultramicrotomy, the technique of cutting nanometers-thin slices of material using a diamond knife, was applied to prepare transmission electron microscope (TEM) specimens of nanoporous poly(methylsilsesquioxane) (PMSSQ) thin films. This technique was compared to focused ion beam (FIB) cross-section preparation to address possible artifacts resulting from deformation of nanoporous microstructure during the sample preparation. It was found that ultramicrotomy is a successful TEM specimen preparation method for nanoporous PMSSQ thin films when combined with low-energy ion milling as a final step. A thick, sacrificial carbon coating was identified as a method of reducing defects from the FIB process which included film shrinkage and pore deformation.

Author(s):  
H. J. Bender ◽  
R. A. Donaton

Abstract The characteristics of an organic low-k dielectric during investigation by focused ion beam (FIB) are discussed for the different FIB application modes: cross-section imaging, specimen preparation for transmission electron microscopy, and via milling for device modification. It is shown that the material is more stable under the ion beam than under the electron beam in the scanning electron microscope (SEM) or in the transmission electron microscope (TEM). The milling of the material by H2O vapor assistance is strongly enhanced. Also by applying XeF2 etching an enhanced milling rate can be obtained so that both the polymer layer and the intermediate oxides can be etched in a single step.


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.


2019 ◽  
Vol 26 (1) ◽  
pp. 120-125 ◽  
Author(s):  
Kenta K. Ohtaki ◽  
Hope A. Ishii ◽  
John P. Bradley

AbstractA new transmission electron microscopy (TEM) specimen preparation method that utilizes a combination of focused ion beam (FIB) methods and ultramicrotomy is demonstrated. This combined method retains the benefit of site-specific sampling by FIB but eliminates ion beam-induced damage except at specimen edges and allows recovery of many consecutive sections. It is best applied to porous and/or fine-grained materials that are amenable to ultramicrotomy but are located in bulk samples that are not. The method is ideal for unique samples from which every specimen is precious, and we demonstrate its utility on fine-grained material from the one-of-a-kind Paris meteorite. Compared with a specimen prepared by conventional FIB methods, the final sections are uniformly thin and free from re-deposition and curtaining artifacts common in FIB specimens prepared from porous, heterogeneous samples.


1999 ◽  
Vol 7 (2) ◽  
pp. 12-15 ◽  
Author(s):  
Lucille A. Giannuzzi ◽  
Richard Young ◽  
Pete Carleson

AbstractDriven by the analytical needs of microelectronics, magnetic media and micro-fabrication industries, focused ion beam (FIB) systems are now capable of milling and manipulating samples for the analysis of microstructure features having dimensions of 180 nm or less, A technique for locating and extracting site specific specimens for examination by transmission electron microscopy (TEM) has been developed. An identified feature can be located and precisely milled with an FIB system from two sides to prepare an ultrathin sample, and then extracted from the region with a glass rod micromanipulator onto a grid for TEM analysis. This specimen preparation method has been applied to semiconductor failure analysis and to the study of metallic and ceramic microsiructures with irregular topographies and complex mufti-layered components.


2000 ◽  
Vol 6 (S2) ◽  
pp. 528-529
Author(s):  
C. Urbanik Shannon ◽  
L. A. Giannuzzi ◽  
E. M. Raz

Automated specimen preparation for transmission electron microscopy has the obvious advantage of saving personnel time. While some people may perform labor intensive specimen preparation techniques quickly, automated specimen preparation performed in a timely and reproducible fashion can significantly improve the throughput of specimens in an industrial laboratory. The advent of focused ion beam workstations for the preparation of electron transparent membranes has revolutionized TEM specimen preparation. The FIB lift-out technique is a powerful specimen preparation method. However, there are instances where the “traditional” FIB method of specimen preparation may be more suitable. The traditional FIB method requires that specimens must be prepared so that the area of interest is as thin as possible (preferably less than 50 μm) prior to FIB milling. Automating the initial specimen preparation for brittle materials (e.g., Si wafers) may be performed using the combination of cleaving and sawing techniques as described below.


Author(s):  
C.S. Bonifacio ◽  
P. Nowakowski ◽  
M.J. Campin ◽  
J.T. Harbaugh ◽  
M. Boccabella ◽  
...  

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.


2005 ◽  
Vol 13 (1) ◽  
pp. 26-29 ◽  
Author(s):  
R.B. Irwin ◽  
A. Anciso ◽  
P.J. Jones ◽  
C. Patton

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.


1999 ◽  
Vol 5 (S2) ◽  
pp. 902-903
Author(s):  
F. Shaapur ◽  
D. Brazeau ◽  
B. Foran

Focused ion beam (FIB) thinning of materials to electron transparency is now a routine procedure for preparation of specimens for transmission electron microscopy (TEM) of microelectronic materials and devices. The nano-scale structural damage, including implantation and amorphization due to this ion milling process has been well investigated and documented. In this paper, we discuss the micro-scale structural damage observed in copper/low-k materials and our efforts to minimize the extent of the damage without compromising the overall specimen preparation time.Figure 1 shows an area-specific cross-sectional specimen prepared from a copper/low-k via-chain test structure using the FIB-milling technique. The procedure involved mechanical thinning of a transverse wafer sliver followed by FIB-milling the area of interest to electron transparency according to conventional steps and conditions' using a liquid Ga+ ion source FIB system. The evidence of structural damage in terms of melting and/or sputtering of the metallization is visible at different areas.


2006 ◽  
Vol 14 (6) ◽  
pp. 58-59
Author(s):  
Ron Anderson

Arecent discussion on the Microscopy Listserver on the subject of microtoming Si reminded many of us of this decades-old issue. Silicon is one of the easiest materials to prepare for TEM analysis with dozens of protocols available including chemical etching, electropolishing, mechanical polishing with and without ion milling, microcleaving, and the use of a focused ion beam instrument. The time involved in Si preparation can range from minutes to a few hours. Things become more complex if it is desired to prepare a Si semiconductor device with high specimen preparation spatial resolution i.e. prepping a prespecified, very small, structure.Now and then a technologist, often times in the biological sciences, is asked to prepare a Si TEM specimen and wonders if Si can be microtomed. The results are almost always a pile of Si dust and frequently a damaged diamond knife.


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