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Microsystem Technologies 5 (1998) 13—17 ( Springer-Verlag 1998

Mechanical stress measurements using micro-Raman spectroscopy


I. De Wolf, H.E. Maes

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Abstract The application of micro-Raman spectroscopy for focused on the sample through a microscope. If a 100]
measurements of mechanical stress in silicon microelectronics objective is used, a probing spot with a diameter of \1 lm can
devices is discussed. The advantages and disadvantages of the be obtained, depending on the optical system and on the
technique are shown through different examples such as Si N wavelength of light.
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and metal lines, isolation structures and solder bumps. Raman scattering arises from an inelastic interaction
between photons (light of the incident laser) and phonons
1 (vibrations of the crystal lattice). The frequency of the Raman
Introduction signal, u, is related to the frequency of the lattice vibrations of
It is well known that during and after processing of semicon- the probed material. Figure 2 shows the Raman spectrum of
ductor devices, mechanical stresses develop in the different crystalline silicon. For this material, the Raman peak is located
films and in the substrate. Various kinds of problems are at u\521 R cm~1. The additional peaks which are visible in
associated with these stresses. Stresses may directly trigger the spectrum are Rayleigh scattered plasma modes from the
nucleation and propagation of dislocations and the formation argon laser. Because strain changes the frequency of the lattice
of voids and cracks. They may influence dopant diffusion, vibrations, it will also shift the Raman frequency. By mapping
affect hot carrier degradation and jeopardize the oxide the frequency shift, u, of the Raman peak at different positions
reliability. Many of these problems will become more acute on the sample, information on the local stress can be obtained.
with the increasing complexity and miniaturisation of the The effects of strain and stress on the Raman frequency of
devices. For this reason, a profound study of this stress is very the optical phonons of most semiconductors used in micro-
important. The number of techniques that can be used for electronics are well known and extensively documented
stress measurements is large. However, none of them is [Anastassakis (1980)]. However, it often remains a difficult
without shortcomings when applied to materials encountered task to use this theory for practical applications encountered in
in microelectronics. Either the resolution is too small, or they microelectronics systems. In the case of uniaxial or biaxial
are destructive, or they have to go hand in hand with complex stress in the studied sample, *u is linearly related to this stress
modelling. A technique which has proved to be very interesting and the Raman data directly provide quantitative information.
for the determination of local stress is micro-Raman spectro- If more complex stress pictures are expected, such as for
scopy [De Wolf (1996a)]. In this paper the application of example at the edge of a film, or near a trench or LOCOS
micro-Raman spectroscopy for the study of local stress in (LOCal Oxidation of Silicon) structure, the relation between
silicon semiconductor devices is discussed. *u and the stress tensor components is more complicated. All
non-zero strain tensor components influence the position of
the Raman peak. In order to obtain quantitative information
2 on the stress in this complex case, some prior knowledge of the
Micro-Raman spectroscopy stress distribution in the sample is required. In other words,
Figure 1 shows the experimental set-up of a typical Raman one has to preassume a stress model. From this model, the
instrument. Light from a laser is focused on the sample and the expected Raman shift can be calculated and compared with the
scattered light is collected and directed into a premono- Raman data, and feed-back can be given to the model. Of
chromator and a spectrometer, to be detected by a CCD course, some experimental parameters, such as the penetration
detector. In micro-Raman spectroscopy (lRS), the light is depth of the laser light in the sample and the diameter of the
focused laser beam on the sample have to be taken into account
[De Wolf (1996b)].
I. De Wolf, H.E. Maes
IMEC, Kapeldreef 75, B-3001 Leuven, Belgium
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Correspondence to: I. De Wolf Examples
Part of this work was funded by the EC project ’Nostradamus’ 3.1
(SMT4-CT95-2024 DG12-RSMT).
The authors thank Rita Rooyackers, Dave Howard and Gonzal Si3N4 lines
Badenes (IMEC), and Michel Ignat (INPG Grenoble) who provided The first semiconductor structures in which the local stress was
many samples. investigated using lRS were LOCOS isolation structures
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Fig. 1. Experimental set-up of a typical


micro-Raman spectrometer

Fig. 2. Raman spectrum of crystalline Si. The other peaks are plasma
lines of the laser
Fig. 3. *u as function of position on 9.4 lm wide, 240 nm/50 nm
Si N /poly-Si line on 10 nm pad oxide on Si
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[Kobayashi et al (1990)]. The isolation of active areas in silicon
by oxidation of the surrounding field indeed introduces large
local stresses in the silicon substrate. Already after the first step the centre. How can this be related to mechanical stress? In
of the LOCOS process, i.e. the deposition and patterning of order to obtain an idea about the sign and the magnitude of the
a nitride mask, stress is introduced in the Si substrate. An stress which corresponds to *u, one can assume uniaxial
example of a lRS experiment on such a structure is shown in stress, r, along the width of the line. This assumption is not too
Fig. 3. This figure shows a map of the shift of the frequency of bad near the center of the line, but it does not hold at the edges.
the Si Raman peak when scanning across a Si N /poly- However, with this assumption, the relation between *u and
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amorphous Si line. A scheme of the sample is shown at the top r becomes simply linear [Anastassakis (1980), De Wolf
of the figure. The laser is first focused far from the line (1996a)]:
(position 0 lm), where the stress can be assumed to be zero.
Next the sample is moved, using an XY-stage, in steps of *u (cm~1)\[2]10~9 r (Pa) (1)
0.1 lm and at each position a Si-Raman spectrum, as the one
shown in Fig. 2, is recorded. A Lorentzian function is fitted to This shows that a positive value of *u indicates compressive
each of these Raman peaks in order to determine the peak stress, and a negative value of *u indicates tensile stress.
frequency. The shift of this frequency from the stress-free A shift of *u \ 0.2 cm~1, as measured in the silicon under the
value, *u, is plotted as a function of the position on the sample centre of the nitride line, would then correspond to a compres-
where the corresponding spectrum was measured. This results sive stress of [100 MPa. Using this approximation of uniaxial
in a plot as shown in Fig. 3. stress, one directly learns that the nitride line imposes
Figure 3 shows that *u becomes negative when approaching compressive stress in the Si under the line and tensile stress
the lines, with maximal negative value just outside the line. near the line’s edge. As mentioned in Chap. 2, it is possible to
When crossing the border, *u changes sign very fast to reach obtain more detailed information on the different stress
a maximum positive value under the line, near the edge. *u components by fitting a stress model to the Raman data [De
remains positive under the line, with some relaxation towards Wolf et al (1996b)]. This was done for these nitride lines using
the so called ‘‘edge force model’’, where it is assumed that the the edges of the nitride mask are lifted. This gives rise to
stress imposed by the line in the silicon can be described by a typical feature in the FO, called the bird’s beak (BB). The
edge forces. A fit of this model to lRS data (open symbols) thickness (d) and length (L) of this BB are indicated in the
from nitride lines with different widths, taking into account figure. This BB formation introduces large local stresses in the
experimental parameters such as probing spot diameter and silicon. The tensile stress peaks, observed in the PBLOCOS
penetration depth, is shown in Fig. 4 (full lines). This structure of Fig. 5a (*u\0), are related to the lifting of the
procedure of fitting theoretical stress models to Raman data nitride edges. For PELOX, these tensile stress peaks are not
can be used for any model describing a device where Raman observed because the BB is very thin (small d). On the other
data can be measured. This way, lRS can be used to hand, the field oxide generates compressive stress in the Si
experimentally verify stress models [De Wolf et al (1996c)]. region under the Si N (active region) due to volume
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expansion. This effect is described by the forces ‘g’ in Fig. 5c. It
can indeed be observed in Fig. 5a and b that the stress under 15
3.2
Isolation structures the nitride lines is compressive (*u[0). This compressive
lRS is very useful to study the influence of changes in the stress is larger in the PELOX structure ([490 MPa) than in the
processing steps of devices on the generated stress. In Fig. 5, PBLOCOS ([200 MPa) because the interface between FO and
the stress in the silicon substrate resulting from two alternative Si is steeper in PELOX, such that the forces ‘g’ are larger.
ways of local isolation [Badenes et al (1997)], PBLOCOS (a)
and PELOX (b), is compared. At the top of the figure, typical 3.3
SEM pictures of the corresponding structures are shown. For Corner effects
clarification, Fig. 5c depicts a conventional LOCOS structure, Figure 6 compares results from a lRS scan across the side and
with field oxide (FO), Si N and Si. During growth of the FO, across the edge of the 5 lm wide active area of a PBLOCOS
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Fig. 4. *u (open symbols) measured on nitride lines (see Fig. 3) with array of lines with width\spacing. The rectangles at the top indicate
different widths. The 9.4 lm line is isolated, the others are part of an the position of the lines

Fig. 5a-c. *u measured on three lines of an array of 3 lm wide of the corresponding structure is shown at the top. c Schematic picture
PBLOCOS a and PELOX b isolation structures. A typical SEM picture of a LOCOS structure
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Fig. 6. a Schematic picture of the edge and side scan across the active (dotted line) and the forces ‘g ’ exerted by the FO, b *u for a scan
area of a PBLOCOS structure, showing the width of the bird’s beak ‘L’ across the side, c *u for a scan across the edge

structure. The side-scan (Fig. 6b) shows a symmetrical picture


of *u, revealing tensile stress at the BB and compressive stress
under the Si N line. The edge-scan however gives an
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asymmetrical picture: the tensile stress due to the BB at the
outer edge (out) is larger than in Fig. 6b, while at the inner BB
(in), it is smaller. This can be explained by the shape of the BB
at position ‘‘out’’ and ‘‘in’’. Indeed, the FO grows from two
sides (top and left) under the outer edge of the nitride mask.
This results in a thicker BB at ‘‘out’’ and consequently in
a larger lifting of the nitride mask. A larger lifting gives rise to
larger tensile stresses. The opposite picture holds at position
‘‘in’’. The BB of the outer edge is longer and thicker than at the
inner edge. This is shown by the dotted lines in Fig. 6a, which
denote contour lines following the tip of the BB. In addition, Fig. 7. Comparison of *u measured near the edge of silicide lines as
Fig. 6c shows that the compressive stress under the nitride a function of the silicide thickness, for different silicides. CoSi (cap)
2
mask is larger near the outer edge and smaller near the inner means CoSi fabricated with a Ti cap
2
edge. This can be explained by the forces ‘g’ exerted by the FO
on the active area. At the outer edge, these forces act from two
sides (top and left), resulting in a larger compressive stress
under the nitride near that position. At the inner side the 3.5
opposite is true. It can be concluded from these lRS results Solder bumps
that, for this kind of structures, the outer edge of the active area Raman spectroscopy can also be applied to study the
will be more prone to stress induced defect formation than the stresses generated by larger systems than the ones mentioned
inner edge. above. Figure 8 shows, e.g., a comparison of the Raman shift,
i.e. the stress, measured in the silicon substrate near solder
3.4 bumps used for flip-chip interconnection during a scan
Metals/silicides towards the bump [De Wolf et al (1997)]. Raman spectra were
It is in general difficult to obtain a Raman signal from metals. collected during a scan towards the bump (see arrow in Fig. 8).
TiSi , e.g., is Raman active, but the Raman peaks are broad and Position ‘‘0’’ indicates the left edge of the socket. Data are
2
very weak, which makes it difficult to extract information on shown for the case of a bump-free TiNiAu socket, a socket with
stress in this silicide. Tungsten is not Raman active. It is a bump with Pb Sn alloy and a socket with a Pb Sn alloy
40 60 95 05
possible, however, to obtain indirectly information on stress, bump. Upon approaching the socket, *u becomes negative,
by measuring *u in the silicon substrate surrounding the indicating tensile stress in the silicon near the socket edge. This
metal [Howard (1995), De Wolf (1995), Ma (1995)]. It is indeed indicates that there is tensile stress in the bump, and
expected that for higher stresses in the metal, or for thicker compressive stress in the silicon substrate underneath the
metal lines, larger stresses are induced by these lines in the bump. The downshift of *u is more negative for the Pb Sn
95 05
silicon substrate. Figure 7 compares the maximum downshift alloy than for the Pb Sn alloy. These experiments confirm
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of *u measured close to the first edge of an array of 3 lm wide that the tensile stress in the bump is larger for a Pb Sn alloy
95 05
silicide lines (3 lm spacing) (*u ) for different silicides with than for the Pb Sn alloy. In addition, they show that these
E 40 60
various thicknesses. This kind of experiments allows stress bumps do introduce large stress gradients in the silicon
comparison in various silicides. If absolute values of this stress substrate, which may be a possible source for defect formation
are required, modelling is necessary. and cracking.
Fig. 9. Temperature shift (*T) and Raman shift (*u) in Si due to 17
changes in the power of the focused laser beam

Fig. 9, a difference in temperature of 4°C already induces


a Si-Raman peak shift of *u\[0.01 cm~1.

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Fig. 8. a Schematic drawing of a top view of a solder bump. The arrow Conclusions
indicates the line along which lRS experiments were performed, lRS is a very interesting and powerful technique to study the
b Raman shift measured for a bare TiNiAu socket (dashed lines: local mechanical stress in silicon devices. The spatial resolu-
diameter 100 lm), a socket with Pb Sn bump (full lines: diameter tion of lRS is about 1 lm, and the sensitivity for stress is about
40 60
100 lm, thickness 24 lm) and a socket with Pb Sn bump (dotted
lines: diameter 100 lm, thickness 24 lm)
95 05 10 MPa. lRS provides information on stress in a non-
destructive way, with reasonable resolution and without the
need for special sample preparation. RS is not restricted to Si,
4 but can be applied to all materials which show a strong, sharp
Hazardous pitfalls Raman signal, both with small dimensions (lm range) and
In order to perform stress measurements using lRS, an large dimensions (no limit).
instrument with good frequency resolution is required. In
addition, knowledge about factors which can influence the
Raman peak frequency, u, is necessary for correct interpreta- References
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changes of u which are not at all related to local stress in the Badenes G; Rooyackers R; De Wolf I; Deferm L (1997) Jpn J Appl Phys
material under study, but which have the same order of 36(3B), 1325
magnitude. These effects can be controlled by using plasma De Wolf I: (1996a) Micro-Raman spectroscopy to study local
mechanical stress in silicon integrated circuits. Topical Review,
lines of the laser as a reference (see Fig. 2, [De Wolf (1996)]).
Semicond Sci Technol 11, 139—154
Plasma lines are Rayleigh scattered lines and any frequency De Wolf I; Maes HE; Jones SK (1996b) J Appl Phys 79(9), 7148—7156
shift of these lines is related to changes in the laser beam De Wolf I; Maes HE; Moffet J; Ignat M (1995) Mater Res Soc Symp
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(1996c) Microelectron Reliab 36(11/12), 1751—1754
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is not only stress but also temperature sensitive. This fact can Howard DJ; De Wolf I; Bender H; Maex K (1995) Mater Res Soc Symp
be used for local temperature measurements [Ostermeir et al. Proc 402
(1992)]. If the heating of the sample by the focused laser beam Kobayashi K; Inoue Y; Nishimura T; Hirayama M; Akasaka Y; Kato T
(1990) J Electrochem Soc 137, 1987—1989
differs from one position on the sample (e.g., where a thick Ma Q; Chiras S; Clarke DR; Suo ZJ (1995) Appl Phys 78(3), 1614—1622
oxide layer is present) to another (e.g., on bare Si), this will Ostermeir R; Brunner K; Abstreiter G; Weber W (1992) IEEE Electron
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