Optimization of FIB-Milling Technique for Preparation of TEM Specimens from Copper/Low-K Materials

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.

1997 ◽  
Vol 480 ◽  
Author(s):  
M. W. Phaneuf ◽  
N. Rowlands ◽  
G. J. C. Carpenter ◽  
G. Sundaram

AbstractFocused Ion Beam (FIB) systems have been steadily gaining acceptance as specimen preparation tools in the semiconductor industry. This is largely due to the fact that such instruments are relatively commonplace as failure analysis tools in semiconductor houses, and are commonly used in the preparation of cross-sections for imaging under the ion beam or using an electron beam in an SEM. Additionally, the ease with which cross-sectional TEM specimens of semiconductor devices can be prepared using FIB systems has been well demonstrated. However, this technology is largely unknown outside the semiconductor industry. Relatively few references exist in the literature on the preparation of cross-sectional TEM specimens of non-semiconductor materials by FIB. This paper discusses a specific use of FIB technology in the preparation of cross-sectional TEM specimens of non-semiconductor samples that are difficult to prepare by conventional means. One example of such materials is commercial galvannealed steel sheet that is used to form corrosion resistant auto-bodies for the automobile industry. Cross-sectional TEM specimens of this material have proved difficult and time-intensive to prepare by standard polishing and ion milling techniques due to galvanneal's inherent flaking and powdering difficulties, as well as the different sputtering rates of the various Fe-Zn intermetallic phases present in the galvannealed coatings. TEM results from cross-sectional samples of commercial galvannealed steel coatings prepared by conventional ion milling and FIB techniques are compared to assess image quality, the size of the electron-transparent thin regions that can be readily prepared and the quality of samples produced by both techniques. Specimen preparation times for both techniques are reported.


2001 ◽  
Vol 7 (S2) ◽  
pp. 956-957
Author(s):  
S. Rubanov ◽  
P.R. Munroe

The technique for the preparation of specimens for transmission electron microscopy (TEM) using the focused ion beam (FIB) miller typically consists of a series of milling steps performed over both sides of an area of interest until an electron transparent membrane is achieved [1]. This process is often accompanied by the formation of damage layers on the surfaces of the specimen. The origins of any damage layer are still not clear. On one hand the process of amorphisation of the target material by the highly energetic ion beam is well known. Alternatively, other workers have reported that this damage layer can be connected with redeposition of milled material. [2,3]. in this paper we have studied redeposition effects during FIB milling of silicon TEM specimens.A FEI xP200 FIB system with a Ga+ ion source operating at 30 kV was used in this work. to study redeposition effects a row of trenches on a silicon specimen was milled under different beam currents ranging from 1000 to 6600 pA. The size of such trenches was 15x10 μm wide and 1 μm deep. The specimen was then removed from the FIB and sputter coated with a ∼50-100 nm thick Au film to preserve the trench surfaces from further damage during subsequent milling. The specimen was then placed back in the FIB system and a second set of trenches 5×8 μm wide and 0.6 μm deep was milled on the bottom of first set of trenches (Fig. 1a). The specimens were sputter coated with Au again and were placed back in the FIB system and the trenches were then covered with 1 μ thick Pt strips using the metal deposition facility of the FIB. The presence of these protection layers (Au and Pt) ensures that the final TEM specimen have unmodified original damage layers resulting from the initial milling steps. Cross-sectional TEM specimens of the trench walls were then prepared using normal FIB procedures (Fig. 1b) [2].


Author(s):  
T. Ohnishi ◽  
H. Koike ◽  
T. Ishitani ◽  
S. Tomimatsu ◽  
K. Umemura ◽  
...  

Abstract A new focused-ion-beam (FIB) micro(μ)-sampling technique has recently been developed to facilitate transmission electron microscope (TEM) specimen preparation, while allowing chips or wafer samples to remain intact. A deep trench is FIB-milled to dig out a small, wedge-shaped portion of the sample (or a microwedge) from the samples area of interest, leaving a small, brige-shaped portion (or a microbridge) to support the microwedge. A metal needle is then manipulated into position for lifting the microwedge, i.e., the μ-sample. FIB-assisted deposition (AD) is used to bond the needle to the μ-sample. FIB-milling of the microbridge then separates the μ-sample from the chip or wafer. The separated μ-sample is mounted onto a TEM grid and secured using FIB-AD. The μ-sample is then FIB-thinned further, to a strip of about 0.1 μm thick. All of the above steps are accomplished under vacuum in the FIB system. This design permits a reliable and user-friendly environment for TEM specimen preparation, while keeping chips or wafer samples intact. It also permits operators to repeat TEM inspection and FIB-milling so that precise areas of interest may be made available for TEM inspection. Both cross-sectional and plan view TEM μ-sampling are feasible.


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.


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):  
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.


Author(s):  
Valery Ray ◽  
Josef V. Oboňa ◽  
Sharang Sharang ◽  
Lolita Rotkina ◽  
Eddie Chang ◽  
...  

Abstract Despite commercial availability of a number of gas-enhanced chemical etches for faster removal of the material, there is still lack of understanding about how to take into account ion implantation and the structural damage by the primary ion beam during focused ion beam gas-assisted etching (FIB GAE). This paper describes the attempt to apply simplified beam reconstruction technique to characterize FIB GAE within single beam width and to evaluate the parameters critical for editing features with the dimensions close to the effective ion beam diameter. The approach is based on reverse-simulation methodology of ion beam current profile reconstruction. Enhancement of silicon dioxide etching with xenon difluoride precursor in xenon FIB with inductively coupled plasma ion source appears to be high and relatively uniform over the cross-section of the xenon beam, making xenon FIB potentially suitable platform for selective removal of materials in circuit edit application.


1998 ◽  
Vol 4 (S2) ◽  
pp. 860-861 ◽  
Author(s):  
A. Ramirez de Arellano López ◽  
W.-A. Chiou ◽  
K. T. Faber

The results of TEM analyses of materials are critically dependent on the quality of the sample prepared. Although numerous techniques have been developed in the last two decades, differential thinning of inhomogeneous materials remains a serious problem. Recently, focused ion beam (FIB) technique has been introduced for cross-sectional sample preparation for TEM and SEM.A novel system for depositing a fine-grain (∼ 200 nm) ceramic coating on a metal surface via a patent pending Small-Particle Plasma Spray (SPPS) technique has been developed at the Basic Industry Research Laboratory of Northwestern University. To understand the properties of the coated surface, the ceramic/metal interface and the microstructure of the ceramic coating must be investigated. This paper presents a comparison of the microstructure of an A12O3 coating on a mild steel substrate prepared using conventional and FEB techniques.


2001 ◽  
Vol 7 (3) ◽  
pp. 287-291
Author(s):  
Toshie Yaguchi ◽  
Hiroaki Matsumoto ◽  
Takeo Kamino ◽  
Tohru Ishitani ◽  
Ryoichi Urao

AbstractIn this study, we discuss a method for cross-sectional thin specimen preparation from a specific site using a combination of a focused ion beam (FIB) system and an intermediate voltage transmission electron microscope (TEM). A FIB-TEM compatible specimen holder was newly developed for the method. The thinning of the specimen using the FIB system and the observation of inside structure of the ion milled area in a TEM to localize a specific site were alternately carried out. The TEM fitted with both scanning transmitted electron detector and secondary electron detector enabled us to localize the specific site in a halfway milled specimen with the positional accuracy of better than 0.1 µm. The method was applied to the characterization of a precipitate in a steel. A submicron large precipitate was thinned exactly at its center for the characterization by a high-resolution electron microscopy and an elemental mapping.


1998 ◽  
Vol 4 (S2) ◽  
pp. 492-493 ◽  
Author(s):  
M.W. Phaneuf ◽  
J. Li ◽  
T. Malis

Focused Ion Beam or FIB systems have been used in integrated circuit production for some time. The ability to combine rapid, precision focused ion beam sputtering or gas-assisted ion etching with focused ion beam deposition allows for rapid-prototyping of circuit modifications and failure analysis of defects even if they are buried deep within the chip's architecture. Inevitably, creative TEM researchers reasoned that a FIB could be used to produce site specific parallel-sided, electron transparent regions, thus bringing about the rather unique situation wherein the specimen preparation device often was worth as much as the TEM itself.More recently, FIB manufacturers have concentrated on improving the resolution and imaging characteristics of these instruments, resulting in a more general-purpose characterization tool. The Micrion 2500 FIB system used in this study is capable of 4 nm imaging resolution using either secondary electron or secondary ions, both generated by a 50 kV liquid metal gallium ion source.


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