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A.
Mndez-Vilas and J. Daz (Eds.)
______________________________________________
Princeton University, Princeton Institute for the Science and Technology of Materials, 70 Prospect Avenue, Princeton, NJ
08544
2
Present address: School of Engineering and Applied, Harvard University, 29 Oxford Street, Cambridge, MA 02138
Milling makes it possible to locally modify the material surface, prepare cross-sections, and shape sample materials.
Generally, the sputtering rate is proportional to the primary beam current. For milling, a higher beam current should be
used initially, followed by a lower current to create a fine polish. However, a low-current beam must be used for
imaging, or else the sample will be excessively eroded.
The sputtering process can also be made material-selective through a process known as gas assisted etching (GAE).
In this technique, one of several halogen gases is introduced in the immediate vicinity of the milling site. The materialspecific absorbency rates enhance the formation of volatile reaction products under ion bombardment. Typical milling
resolution of around 0.1 m is achieved with GAE, and holes and cuts can be placed within 20 nm [5]. Milling
efficiency of this technique is typically a few m3/nC. GAE is much more efficient than standalone FIB for removing
large volumes of material, and it does not cause unwanted redeposition of already-etched materials. However, GAE can
only be used with certain substrates, as it requires a precursor gas that specifically forms volatile products with the
substrate while avoiding spontaneous reaction. Furthermore, GAE sacrifices some of the precision of unassisted ion
milling for higher speed. The smallest feature sizes it has achieved have been between 200 and 300 nm. Thus, a twostage process of initial GAE followed by ion milling is frequently used when an operation requires bulk volumes of
material removal as well as high precision.
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Fig. 3 Schematic of the SEM and FIB machines, shown in a two-beam configuration [53].
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first be milled using the ion beam and then filled using electron beam deposition to make the final diameter as small as
4 nm [23].
) (A
pattern
1.602 10-15
(1)
Rectangles with depths of about 4 nm and dimensions of 4 x 1 m were milled and investigated, along with grids
consisting of lines 5 m by 20 nm. Atomic force microscopy
was used to characterize the topography of the altered
surface. It was found that results differed for varying doses
of ions. In almost all cases, edge protrusions were noted,
ranging from 0 nm (1013 ions cm-2) to a maximum height of
approximately 1 nm when below a dosage of 1017 ions cm-2.
Edge effects were mainly blamed on Ga+ implantation from
stray ions and redeposition of secondary and backscattered
material [24].
2.1.1 Integrated circuit analysis and modification
The FIB system has found widespread use in the
semiconductor industry for applications in defect analysis
and modification of prototype integrated circuits. The ion
Fig. 4 Combination SEM and FIB passive voltage contrast
beam is capable of precisely milling a cut to disconnect a
images. The FIB portion (right) shows an area of memory
wire while depositing conducting material in another area to
cells after exposing the wings of the floating gates. One
connect two pieces of wire, like a micro-soldering iron, and
floating gate appears bright, indicating that it is grounded and
this is all done with minimal damage to the wafer itself.
therefore the tunnel or gate oxide has failed [25].
When investigating integrated circuits, the lack of visible
evidence on the material surface often makes it difficult to find the defect location; the failure cannot be repaired if it
cannot be found. This problem has been analyzed at FEI Europe, Ltd., and a technique utilizing only the FIB machine
has been developed to effectively locate the area of concern. FEI examined a transistor containing a certain gate
(approximately 1 m2) under which a thin gate oxide layer had broken down due to excessive voltage application
(Figure 4). The source and drain lay on opposite ends of the gate, which sat atop the gate oxide layer, all of which
resided on a silicon substrate. TEM samples of the failure site (<100 nm in diameter) were desired to investigate the
mechanics behind the problem, but first the area of failure had to be located. To do so, an outline of trenches was first
milled around the suspected region using high beam currents. Removal of thin slices along with fast and minimally
destructive imaging was then performed until the structure became apparent. Finally, low beam currents were used to
uncover the region (focusing and stigmation adjustment were performed away from the region to avoid unnecessary
damage). It was found that these basic steps succeeded in efficiently locating a defective area [25]. After locating the
defect, the FIB can be used again for repairing it.
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In other experiments, ion bombardment on hydrogenated silicon-carbon alloy films (a-SiC:H) has been shown to
induce different opacities in crystal layers, depending on whether or not they have been bombarded (Figure 6). This is
of great interest because large optical contrast in a-SiC:H enables a new material for opto-electronic devices and for
severe environmental conditions. A recent study
compared the effects of Ga+ and Sn+ bombardment with
previous experiments that studied As+. Films were
prepared by two different methods: a glow discharge
technique (GD), and reactive magnetron sputtering (SP).
The samples were bombarded at 50 keV (Ga+) and 60
keV (Sn+), with an ion-beam intensity of 2 A/cm2 and
doses between 1015 and 1017 ions cm-2. Both films
showed massive increases (greater for the GD-prepared
film) in optical absorption coefficients compared to
previous experiments with As+, indicating that the
formation of optical contrast was much more effective.
FIBs material altering capabilities as part of an
integrated two-beam system were vividly demonstrated
by the work of Shinji Matsui at the Himeji Institute of
Technology in Japan. It was shown that using the milling
and deposition techniques, complex 3D structures could
be modeled based on software-defined inputs, such as
Fig. 6 Optical contrast pattern written into a GD a-Si0.85C0.15:H
bitmap files, using a digital patterning generator. CAD
film deposited on Corning 7059 glass substrate. The
files were used in conjunction with ion beam deposition
transparent and opaque regions represent un-implanted and
to create spring and bellow shaped 3-D helical structures
implanted parts of the film, respectively. The patterning has
with part dimensions as small as 80 nm (Figure 7) [32].
been performed with the help of a program-controlled Ga+focused ion beam. The minimum feature size is 2.5 m. [31]
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Fig. 8 Abalone shell two-beam cross-section images showing the presence and propagation of screw dislocations
through multiple layers of nacre. A screw dislocation core platelet (a) was selected for analysis, after which trenches
were precisely milled through it by FIB and observed via SEM. The resulting side views (b-d) display the complex
morphology of the biomaterial and reveal features that were previously impossible to view [55].
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Fig. 9 Left: SEM image of sample immediately before lift out (courtesy of FEI Company). Right: image of warping effect. FIB cuts
will be made near both endpoints to relieve residual stresses and decrease warping.
A structural problem that can occur during thinning with the lift-out technique is warping in the sample. As the
material is thinned to less than 200 nm, stresses in the sample cause strain and bending. These bulk stresses can be due
to poor mounting or are sometimes naturally present in the internal structure of the material. In either case, a study by
FEI Europe Ltd. found that cutting one or both of the edges (depending on the degree of the warping) of the almost fully
thinned sample would alleviate the stress by creating space for relaxation. This technique has been shown to solve
almost all warping problems [41, 42].
The FIB systems direct writing capabilities in TEM sample preparation have been exploited not only for materials
science, but also for environmental science applications. For example, copper run-off from the roofs of buildings has
become a serious environmental concern. One proposed solution has been to install filter systems in major runoff areas.
In a study of this concept by the Swiss Federal Institute for Environmental Study and Technology, iron hydroxide was
found to be the most effective Cu filter. The research looked at Cu adsorption on suspended specimens in the water and
in the iron hydroxide. TEM analysis of iron hydroxide samples prepared by the FIB lift out technique showed that the
iron hydroxide was effectively decreasing the copper runoff [43].
2.3 Sample Imaging Defining the Third Dimension
As previously discussed, FIB systems can image as well as modify sample surfaces. As a result, the FIB machine is
uniquely capable of three-dimensional sample imaging. Three-dimensional images can be constructed from a series of
two-dimensional images, which are obtained by milling off layers of a sample using the ion beam and imaging with the
SEM. Interpolation of the two-dimensional images yields a three-dimensional representation, as well as data about the
grain structure and other features. The FIBs singular ability to reveal the internal structure of a material through milling
or gas assisted etching (GAE) is valuable to many researchers because it provides important information on the material
properties and behaviour. For example, the grain structure and grain boundaries yield extensive insight into a materials
mechanical and electrical properties. Internal elemental distribution can also be obtained using SIMS [18, 46]. Dunn
and
Hull
recently
Pt protective strap
demonstrated this ability of the
FIB
to
create
threeStaircase cuts shape
cut
dimensional
volume
reconstructions. Their method
Cross sections
used FIB serial sectioning and
face
linear interpolation to produce
Second
well-defined images of the
milled
samples 3-D structure (Figure
10) [47].
2 m
1 m
a.
5 m
b.
Fig. 10 (a) Schematic of sequential FIB slicing for 3-D reconstruction and a set of slices
taken through a sample; (b) reconstructed surface of a nano-indented PVAC film [56].
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References
[1] Krohn VE. Liquid ion source for heavy particle propulsion. Progr. Astronautics and Rocketry. New York: A. C. Press;
1961. 73-80.
[2] Krohn VE, Ringo GR. Ion source of high brightness using liquid metal. Appl. Phys. Lett. 1975; 27:479.
[3] Orloff J, Utlaut M, Swanson L. High Resolution Focused Ion Beams: FIB and Its Applications. New York: Kluwer
Academic/Plenum Publishers; 2003.
[4] Jamison R, Ph.D. Thesis: Computational and Experimental Quantification of Focused Ion Beam Damage in Silicon During
TEM Sample Preparation. University of California, Berkeley; 2000.
[5] Phaneuf MW. Applications of focused ion beam microscopy to materials science specimens. Micron. 1999; 30:277.
[6] Van Doorselaer K, Van den Reeck M, Van den Bempt L, Young R, Whitney J. How to Prepare Golden Devices Using
Lesser Materials. Proc. 19th International Symposium for Testing and Failure Analysis. 1993.
[7] Russell PE, Stark TJ, Griffis DP, Gonzales JC. Chemically Assisted Focused Ion Beam Micromachining: Overview,
Recent Developments and Current Needs. Microsc. Microanal. 2001; 7S2:928.
[8] Phaneuf MW, Li L. FIB Techniques for Analysis of Metallurgical Specimens. Microsc. Microanal. 2000; 6S2:524.
[9] Casey JD, Phaneuf M, Chandler C, Megorden M, Noll K, Schuman R, Gannon TJ, Krechmer A, Monforte D, Antoniou N,
Bassom N, Li J, Carleson P, Huynh C. Copper device editing: Strategy for focused ion beam milling of copper. J. Vac. Sci.
Technol. B. 2002, 20:2682.
[10] Taniguchi J, Ohno N, Takeda S, Miyamoto I, Komuro M. Focused-ion-beam-assisted etching of diamond in XeF2. J. Vac.
Sci. Technol. B. 1998; 16:2506.
[11] Stanishevsky A. Patterning of diamond and amorphous carbon films using focused ion beams. Thin Solid Films. 2001; 398399:560.
[12] Adams DP, Vasile MJ, Mayer TM, Hodges VC. Focused ion beam milling of diamond: Effects of H20 on yield, surface
morphology and microstructure. J. Vac. Sci. Technol. B. 2003; 21:2334.
[13] Gerlach R, Utlaut M. Focused ion beam methods of nanofabrication: room at the bottom. Proc. SPIE Int. Soc. Opt. Eng.
2001; 4510:96.
[14] Mitsuishi K, Shimojo M, Han M, Furuya K. Electron-beam-induced deposition using a subnanometer-sized probe of highenergy electrons. Appl. Phys. Lett. 2003; 83:2064.
[15] Khizroev S, Bain JA, Litvinov D. Fabrication of nanomagnetic probes via focused ion beam etching and deposition.
Nanotechnology. 2002; 13:619.
[16] Allameh SM, Yao N, Soboyejo WO. Synthesis of self-assembled nanoscale structures by focused ion-beam induced
deposition. Scripta Mater. 2004; 50:915.
[17] Strobel M, Heinig KH, Mller W. Can core/shell nanocrystals be formed by sequential ion implantation? Predictions from
kinetic lattice Monte Carlo simulations. Nucl. Instr. Meth. B. 1999; 148:104.
[18] Hull R, Dunn D, Kubis A. Nanoscale tomographic imaging using focused ion beam sputtering, secondary electron imaging
and secondary ion mass spectrometry. Microsc. Microanal. 2001; 7S2:34.
[19] Gnauck P, Zeile U, Rau W, Schumann M. Real time SEM imaging of FIB milling processes for extended accuracy in cross
sectioning and TEM preparation. Microsc. Microanal. 2003; 9S3:524.
[20] Zimmermann G, Chapman R. In-situ dual-beam (FIBSEM) techniques for probe pad deposition and dielectric integrity
inspection on 0.2mm technology DRAM single cells. Proc. 25th International Symposium for Testing and Failure Analysis.
1999.
[21] Lipp S, Frey L, Lehrer C, Frank B, Demm E, Pauthner S, Ryssel H. Tetramethoxysilane as a precursor for focused ion
beam and electron beam assisted insulator (SiOx) deposition. J. Vac. Sci. Technol. B. 1996; 14:3920.
[22] Rice L. Semiconductor failure analysis using EBIC and XFIB. Microsc. Microanal. 2001; 7S2:514.
[23] Huey BD, Langford RM. Low-dose focused ion beam nanofabrication and characterization by atomic force microscopy.
Nanotechnology. 2003; 14:409.
[24] Young RJ, Moore MV. Chapter 12: Dual beam (FIB-SEM) systems. Introduction to Focused Ion Beams: Instrumentation,
Theory, Techniques and Practice. Gianuzzi LA, Stevie FA, eds. New York: Springer; 2005.
[25] Haythornthwaite R, Nxumalo J, Phaneuf MW. Use of the focused ion beam to locate failure sites within electrically
erasable read only memory microcircuits. J. Vac. Sci. Technol. A. 2004; 22:902.
[26] Li HW, Kang DJ, Blamire MG, Huck WTS. Focused ion beam fabrication of silicon print masters. Nanotechnology. 2003;
14:220.
[27] Liu Y, Longo DM, Hull R. Ultrarapid nanostructuring of poly(methylmethacrylate) films using Ga+. Appl. Phys. Lett.
2003; 82:346.
[28] Arshak K, Mihov M, Arshak A, McDonagh D, Sutton D. Novel dry-developed focused ion beam lithography scheme for
nanostructure. Microelectron. Eng. 2004; 73-73:144.
[29] Harris G, Zhou P. The growth and characterization processes of gallium nitride (GaN) nanowires. National
Nanofabrication User Network. 2001; 2001:34.
[30] Flierl C, White IH, Kuball M, Heard PJ, Allen GC, Marinelli C, Rorison JM, Penty RV, Chen Y, Wang SY. Focused ion
beam etching of GaN. MRS Internet J. N. S. R. 1999; 4S1, G6:75.
[31] Bischoff L, Teichert J, Kitova S, Tsvetkova T. Optical pattern formation in a-SiC: H films by Ga+ ion implantation.
Vacuum. 2002; 69:73.
[32] Anzalone PA, Mansfield JF, Giannuzzi LA. Dual-beam milling and deposition of complex structures using bitmap files and
digital patterning. Microsc. Microanal. 2004; 10S2:1154.
[33] Kang KJ, Yao N, He MY, Evans AG. A Method for in-situ measurement of the residual stress in thin films by using the
focused ion beam. Thin Solid Films. 2003; 443:71.
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FORMATEX 2010
[34] Yao N, Evans AG, Cooper CV. Wear mechanisms operating in diamond like carbon coatings in contact with machined
steel surfaces. Surface and Coatings Technology. 2004; 179:306.
[35] Chen X, Wang R, Yao N, Evans AG, Hutchinson JW, Bruce RW. Foreign object damage in a thermal barrier system:
mechanisms and simulations. Materials Science and Engineering A. 2003; 352:221.
[36] Giannuzzi LA, Drown JL, Brown SR, Irwin RB, Stevie FA. Focused ion beam milling and micromanipulation lift-out for
site specific cross-section TEM specimen preparation. Mat. Res. Soc. Symp. Proc 1997; 480:19.
[37] Cairney JM, Harris SG, Munroe PR, Doyle ED. Transmission electron microscopy of TiN and TiAlN thin films using
specimens prepared by focused ion beam milling. Surf. Coatings Technol. 2004; 183:239.
[38] Volkert CA, Busch S, Heiland B, Dehm G. Transmission electron microscopy of fluorapatite-gelatine composite particles
prepared using focused ion beam milling. J. Microsc.-Oxford. 2004; 214:208.
[39] Rossie BB, Shofner TL, Brown SR, Anderson SD, Jamison MM, Stevie FA. A method for thinning FIB prepared TEM
specimens after lift-out. Microsc. Microanal. 2001; 7S2:940.
[40] Yaguchi T, Konno M, Kamino T, Hashimoto T, Onishi T, Umemura K. FIB micro-pillar sampling technique for 3-D stem
observation and its application. Microsc. Microanal. 2003; 9S2:118.
[41] Wang ZG, Kato N, Sasaki K, Hirayama T, Saka H. Electron holographic mapping of two-dimensional doping areas in
cross-sectional device specimens prepared by the lift-out technique based on a focused ion beam. J. Electron Microsc.
2004; 53:115.
[42] Walker JF. Preparing TEM sections by FIB: stress relief to straighten warping membranes. Inst. Phys. Conf. Ser. 1997;
157:469.
[43] Mavrocordatos D, Steiner M, Boller M. Analytical electron microscopy and focused ion beam: complementary tool for the
imaging of copper sorption onto iron oxide aggregates. J. Microsc.-Oxford. 2003; 210:45.
[44] Sivel VGM, Van den Brand J, Wang WR, Mohdadi H, Tichelaar FD, Alkemade PFA, Zandbergen HW. Application of the
dual-beam FIB/SEM to metals research. J. Mircrosc.-Oxford. 2004; 214:237.
[45] Lou J, Shrotriya P, Allameh S, Yao N, Buchheit T, Soboyejo WO. Plasticity length scale in LIGA nickel MEMS structure.
Mat. Res. Soc. Symp. Proc. 2002; 687:41.
[46] Inkson BJ, Mbus G. 3D determination of grain shape in FeAl by focused ion beam (FIB) tomography. Microsc.
Microanal. 2001; 7S2:936.
[47] Dunn DN, Hull R. Three-dimensional volume reconstructions using focused ion beam serial sectioning. Microsc. Today.
2004; 12(4):52.
[48] Takanashi K, Shibata K, Sakamoto T, Owari M, Nihei Y. Analysis of non-woven fabric fibre using an ion and electron
multibeam microanalyser. Surf. Interface Anal. 2003; 35:437.
[49] Rubanov S, Munroe PR. FIB-induced damage in silicon. J. Microsc.-Oxford. 2004; 214:213.
[50] Sutton D, Parle SM, Newcomb SB. Focused ion beam damage: its characterization and minimization. Inst. Phys. Conf. Ser.
2001; 168:377.
[51] Russell PE, Stark TJ, Griffis DP, Phillips JR, Jarausch KF. Chemically and geometrically enhanced focused ion beam
micromachining. J. Vac. Sci. Technol. B. 1998; 16:2494.
[52] Utlaut M. Micro-machining and mask repair. Focused Ion Beam System: Basics and Applications. Yao N, ed. Cambridge:
Cambridge University Press; 2007.
[53] Yao N. Introduction. Focused Ion Beam System: Basics and Applications. Yao N, ed. Cambridge: Cambridge University
Press; 2007.
[54] Fujii T. Focused ion beam system as a multifunctional tool for nanotechnology. Focused Ion Beam System: Basics and
Applications. Yao N, ed. Cambridge: Cambridge University Press; 2007.
[55] Yao N, Epstein A, Akey A. Screw Dislocations and Spiral Growth in Abalone Nacre. J. Mat. Res. 2006; 21(8):1939-1946.
[56] Langford RM. Preparation for physico-chemical analysis. Focused Ion Beam System: Basics and Applications. Yao N, ed.
Cambridge: Cambridge University Press; 2007.
[57] Principe EL. Advances in Real-Time SEM Imaging during Focused Ion Beam Milling: From 3D Reconstruction to End
Point Detection. Focused Ion Beam System: Basics and Applications. Yao N, ed. Cambridge: Cambridge University Press;
2007.
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