On the residual stress and fracture strength of crystalline silicon wafers

Chris Yang, Frank Mess, Kevin Skenes, Shreyes Melkote, and Steven Danyluk

Citation: Applied Physics Letters 102, 021909 (2013); doi: 10.1063/1.4776706

View online: http://dx.doi.org/10.1063/1.4776706
View Table of Contents: http://scitation.aip.org/content/aip/journal/apl/102/2?ver=pdfcov
Published by the AIP Publishing

Articles you may be interested in

Effect of oxygen and associated residual stresses on the mechanical properties of high growth rate Czochralski
silicon
J. Appl. Phys. 113, 133502 (2013); 10.1063/1.4798599

Effect of surface morphology on the fracture strength of silicon nanobeams

Appl. Phys. Lett. 89, 091901 (2006); 10.1063/1.2338649

Fracture toughness of low-pressure chemical-vapor-deposited polycrystalline silicon carbide thin films

J. Appl. Phys. 99, 013517 (2006); 10.1063/1.2158135

Cracking of GaN on sapphire from etch-process-induced nonuniformity in residual thermal stress

J. Appl. Phys. 89, 6033 (2001); 10.1063/1.1368394

Elastic moduli, strength, and fracture initiation at sharp notches in etched single crystal silicon microstructures
J. Appl. Phys. 85, 3519 (1999); 10.1063/1.369711

Reuse of AIP Publishing content is subject to the terms at: https://publishing.aip.org/authors/rights-and-permissions. IP: 200.130.19.131 On: Mon, 22 Feb 2016 18:02:05
 APPLIED PHYSICS LETTERS 102, 021909 (2013)

On the residual stress and fracture strength of crystalline silicon wafers

Chris Yang,1 Frank Mess,1 Kevin Skenes,2 Shreyes Melkote,1,2 and Steven Danyluk2
1
Georgia Tech Manufacturing Institute, Georgia Institute of Technology, Atlanta, Georgia 30332, USA
2
George W. Woodruff School of Mechanical Engineering, Georgia Institute of Technology, Atlanta,
Georgia 30332, USA
(Received 28 November 2012; accepted 2 January 2013; published online 16 January 2013)
This letter reports on residual stress measurement in thin crystalline silicon wafers with a full-field
near-infrared polariscope. Residual stress is analyzed in combination with observed surface defects,
and the results are related to measured fracture strength variation in the wafers. Measurements
indicate that there is a sawing process-related residual stress in the as-cut wafers, and that etch-
removal of 5 lm from the wafer surface eliminates a damage layer that can significantly reduce
the residual stress in the wafer, and therefore increases the observed fracture strength. There is a
corresponding 2 to 3 lm reduction in the observed characteristic defect size after etching. Fracture
strength anisotropy observed in the wafers is related to defect orientation (scratching grooves and
microcracks) caused by the sawing process. V C 2013 American Institute of Physics.

[http://dx.doi.org/10.1063/1.4776706]
Residual stress in crystalline silicon is of interest due to its
multiple adverse effects on mechanical, optical, and electrical
properties of semiconductor wafers and devices.1–4 For a thin
silicon wafer, tensile residual stress may cause wafer warpage
or even breakage during processing and handling. It can also
introduce dislocation networks that decrease the minority car-
rier life-time in devices.5 Regions of localized residual stress
are generally produced during the solidification process, or
other thermal processing, where large thermal gradients are
present, but may also come from wafer production processes
(e.g., diamond wire sawing) where ductile-mode deformation
and/or phase transformation occur due to a high local contact
pressure. It is therefore critical to understand the residual stress
distribution and magnitude in each process step to improve the
manufacturing process and resultant products.
Several methods, including hole-drilling,6 micro- and
nano-indentation,7,8 x-ray,9,10 Raman,11 shadow moire,12 and
polariscopy,13–15 can be used to measure residual stresses in a
material. For thin crystalline silicon wafers, however, several
of these are impractical due to the required contact with the
wafer, and some techniques only provide spot measurement.
Polariscopy can overcome some of these limitations and our
work has led to a development of a full-field near infrared
(NIR) polariscope for non-destructive residual stress meas-
urements of silicon wafers of size 156 mm  156 mm or
greater. This paper presents the application of this technique
and experimental results of residual stress measurements for
two types of photovoltaic (PV) silicon wafers: Multicrystal-
line Si (mc-Si) wafers and cast mono-like Si wafers, each cut
using an advanced diamond wire sawing technique. The
measured residual stress distribution and magnitude, together
with other surface defects, are used to explain the fracture
strength variation in the wafers.
The operational principle of the polariscope is based on
stress-induced birefringence. For thin silicon wafers, near
infrared polarized light is used for illumination. Optical ani-
sotropy in a material can cause double refraction of the trans-
mitted light, and this can be related to birefringence when
measured by a polariscope. The magnitude of the stress is
indicated by the isochromatic fringe count, i.e., phase retar-
dation, while the stress orientation is related to isoclinic
fringes. The relationship of birefringence to residual stress is
governed by the stress-optic law15
k
smax ¼ jr1  r2 j ¼ d; (1)
2ptC
where smax is the maximum shear stress, which is related to
the two principal stresses (r1 and r2, for the largest and small-
est stresses, respectively), k is the wavelength of the illuminat-
ing light, d is the phase retardation of the two indexes, t is the
sample thickness, and C is the stress-optic coefficient that can
be determined experimentally for a certain material and crys-
talline orientation. From prior work,15 we use an average
stress-optic coefficient of 1.66  1011 Pa1.
Figure 1 shows a schematic of a full-field NIR polari-
scope that can accommodate 156 mm  156 mm or larger
wafers. A white light point source (tungsten-halogen lamp,
with a 1150 nm filter) is first polarized linearly by an infrared
polarizer and then the polarization state is changed to circu-
lar by a first-order quarter waveplate, followed by collima-
tion by an aspherical lens. A fringe multiplier consisting of
two beam splitters can be placed in the front and back of the
sample to increase the transmitted signal, although the results
in this paper were obtained without using beam splitters. The
light transmitted through the sample then passes through
FIG. 1. A schematic diagram of a full-field NIR polariscope.

0003-6951/2013/102(2)/021909/5/$30.00 102, 021909-1 C 2013 American Institute of Physics

V

Reuse of AIP Publishing content is subject to the terms at: https://publishing.aip.org/authors/rights-and-permissions. IP: 200.130.19.131 On: Mon, 22 Feb 2016 18:02:05
 021909-2 Yang et al.
another aspherical lens and is acted on by a second quarter
waveplate and an analyzer. The transmitted image is collected
by a high sensitivity infrared camera in combination with a
frame grabber. The fast axis of the two quarter waveplates is
independently adjusted using a phase stepping technique. A
six step method was utilized in this work to calculate the
phase retardation and isoclinic angle, although ten-step meth-
ods have also been used. The details of the phase stepping
technique employed can be found in the literature.15
Representative residual stress maps of mc-Si and mono-
like Si wafers in the as-cut condition and after 5 lm etching/
damage layer removal are shown in Figure 2. The images in
Figure 2 are colorized gray-scale data for the wafer with a
pixel size of 64 lm. These data are for wafers cut to a
200 lm nominal thickness using a diamond wire saw. It can
be seen that there is a non-uniform distribution of residual
stress in these wafers. A pattern of narrow strips of alterna-
tive high and low residual stresses oriented in a roughly
upward (vertical) direction is observed in the as-cut mc-Si
wafers (Figure 2(a)). A maximum local residual stress of
37.5 MPa and an average residual stress of 6.69 MPa are
observed in this wafer. Chemical etching in HF/HNO3 solu-
tion was done to remove a 5 lm layer on each side, and the
maximum observed residual stress in the wafers is reduced
to 21.9 MPa, and the average residual stress is reduced to
2.86 MPa (Figure 2(b)). A statistical analysis of the measured
residual stresses (Figure 2(c)) indicates a skewed distribution
with a large residual stress tail for the as-cut wafers, but a
hyperbolic distribution for the post-etch wafers. The residual
stress at peak probability is 6.09 MPa for the as-cut mc-Si
wafers, and close to zero for the post-etch wafers. Note the
non-uniformity of the residual stress distribution across the
FIG. 2. Residual stress maps for (a) as-cut cast mc-Si wafers, (b) post-etch cast mc-Si wafers, (d) as-cut cast monolike Si wafers, and (e) post-etch cast mono-
like Si wafers, and statistical distributions for (c) mc-Si wafers and (f) moonlike Si wafers. Pixel size ¼ 64 lm in the images.
Reuse of AIP Publishing content is subject to the terms at: https://publishing.aip.org/authors/rights-and-permissions. IP: 200.130.19.131 On: Mon, 22 Feb 2016 18:02:05
Appl. Phys. Lett. 102, 021909 (2013)
wafer. Due to the inherent inhomogeneity of residual stress
across the wafer surface, traditional point-measurement tech-
niques previously cited are not sufficient or practical for
evaluation of mc-Si or mono-like PV wafers.
The cast mono-like wafers show similar residual stresses
but with a slightly lower magnitude. As there are only large
grains in the mono-like silicon wafers, the residual stresses
are observed to vary with the grain orientation. High and low
residual stresses vary alternatively in the neighboring grains
(Figure 2(d)). A maximum residual stress of 38.9 MPa and
an average residual stress of 5.61 MPa are observed in the
as-cut mono-like wafers. As with the mc-Si wafers, etching
has a pronounced effect on the reduction of residual stress in
the mono-like Si wafers. The residual stress decreases to
28 MPa for the maximum and 3.25 MPa for the average after
the same 5 lm etching (Figure 2(e)). The residual stress dis-
tribution (Figure 2(f)) indicates that the peak intensity is
located at 5.36 and 1.1 MPa for the as-cut and post-etch
wafers, respectively. The surface characteristic of the resid-
ual stress suggests that stresses are correlated to the diamond
wire sawing process where ductile-mode deformation and
phase transformation may occur.
Wafer surfaces before and after etching were examined
by scanning electon microscopy (SEM), as shown in Figure 3.
There are long parallel grooves, interwoven with random pits,
on the as-cut wafer surface (Figure 3(a)). The long grooves
are evidence of scratching and ductile-mode deformation
during diamond wire sawing. Even in the case of crystalline
silicon, an inherently brittle material, plastic deformation is
possible under a high, local contact pressure. Amorphous sili-
con is often found on the silicon surface after sawing as a
result of pressure-induced phase transformation.16 High
 021909-3 Yang et al.
contact pressure at the diamond grit and wafer interface
causes local deformation in the silicon, similar to a shot peen-
ing process. Unlike shot peening, however, the deformation is
highly directional due to the dragging and scratching process
of the diamond grits across the wafer surface during cutting.
The unidirectional deformation in the sawing process also cre-
ates microcracks along the sawing direction. The slightly
overetched microcracks can be clearly seen in the post-etch
surface where microcracks are widened by chemical etching
(Figure 3(b)). It can be seen that there are many small dimples
and a few elongated holes on the wafer surface after a shallow
(5 lm) etch. The small dimples are a remnant of the original
surface contour due to nonuniform etching, but the elongated
holes are evidence of microcracks that are widened by chemi-
cal etching. These long surface microcracks or holes can have
a significant (adverse) effect on the mechanical, electronic,
and optical properties of silicon wafers.
The fracture strength of the silicon wafers was measured
using the four line bending method. Full-sized wafers of
156 mm  156 mm were cut by dicing into 32 individual rec-
tangular samples of 19.5 mm  29 mm. The details of this
experimental method and a discussion of the inflluence of
the dicing damage on the fracture strength can be found else-
where.17 The fracture strength for each rectangular sample is
determined as
3Fðlo  li Þ
r¼ ; (2)
2bd 2
FIG. 4. Weibull distribution of fracture strength for (a) mc-Si wafers and (b) cast monolike Si wafers, in as-cut and after etching under two orthogonal bending
orientations (parallel, P, and perpendicular, V) relative to saw marks.
Reuse of AIP Publishing content is subject to the terms at: https://publishing.aip.org/authors/rights-and-permissions. IP: 200.130.19.131 On: Mon, 22 Feb 2016 18:02:05
Appl. Phys. Lett. 102, 021909 (2013)
FIG. 3. Representative surface SEM
images of (a) as-cut mono-like wafers
and (b) post-etch wafer.
where F is the applied load (resultant of the normal and tan-
gential forces), b is the sample width, d is the wafer thick-
ness, and lo and li are the distances between the lower
supports and the upper loading beams, respectively.
Figure 4 shows the Weibull plots of the fracture strength
distributions for both multicrystalline and mono-like wafers
in the as-cut and etched states for bending in two orientations
relative to the saw marks. A significant fracture strength dif-
ference is observed between the as-cut and the post-etch
wafers, and between the two orthogonal bending orienta-
tions. A statistically higher fracture strength is obtained on
the post-etch wafers than on the as-cut samples for all
wafers. Fracture strength anisotropy with bending orientation
is also observed. A higher fracture strength is measured
when bent perpendicular to the sawing direction, with a
lower fracture strength in the orthogonal direction. The Wei-
bull distribution is observed to be similar in both multicrys-
talline and mono-like wafers.
The characteristic fracture strength at the 63.2% failure
probability is calculated for each wafer type as shown in
Figure 5. The change in measured fracture strength between
the as-cut and the post-etch wafers can be clearly seen. The
fracture strength of the post-etch wafers is substantially
higher than for the as-cut wafers and there is a fracture
strength difference between the two bending orientations.
The characteristic fracture strength in the perpendicular ori-
entation is almost double that in the parallel direction. When
bent parallel to the saw marks, the characteristic strength for
 021909-4 Yang et al. Appl. Phys. Lett. 102, 021909 (2013)

FIG. 5. Characteristic strength for mc-Si and monolike wafers bent (a) parallel to saw marks and (b) perpendiuclar to saw marks.

the as-cut mc-Si and mono-like wafers is 109 and 121 MPa
for the as-cut wafers, respectively, and 165 and 181 MPa for
the post-etch wafers, respectively. When bent perpendicular
to the saw marks, the characteristic stregnth for mc-Si and
mono-like wafers is 229 and 212 MPa for the as-cut wafers,
respectively, and 292 and 343 MPa for the post-etch wafers,
respectively. The difference in measured fracture strength of
these wafers can be explained by the residual stresses and
the orientation of microcracks in the wafers.
In four-line bending tests, the fracture strength of a sam-
ple will be determined by the largest tensile stress present,
which is usually located along the bottom surface of the sam-
ple due to loading geometry. If there is residual stress present
in the sample, it will contribute additively to the bending
stress applied to the sample. The fracture strengh is then
determined by the resultant stress as follows:
pffiffiffi
KIc ¼ Yðr þ rr Þ c; (3)
where r and rr are the applied stress and residual stress,
respectively, c is the length of defects (cracks), and Y is a
dimensionless parameter that is related to the defect shape
and location, and KIc is the fracture toughness. Equation (3)
suggests that a tensile (negative) residual stress will decrease
the fracture strength. This also explains the low fracture
strength measured in the as-cut wafers.
Equation (3) also indicates that there is a defect size
effect on the fracture strength. The characteristic defect size
on a diamond wire sawn wafer will vary depending on the

FIG. 6. (a) A representative surface topographical map of a diamond wire sawn wafer measured by a 3D laser confocal microscope, and schematics of charac-
teristic defects viewed from two prespectives: (b) perpendicular and (c) parallel directions.

Reuse of AIP Publishing content is subject to the terms at: https://publishing.aip.org/authors/rights-and-permissions. IP: 200.130.19.131 On: Mon, 22 Feb 2016 18:02:05
 021909-5 Yang et al.
FIG. 7. Distributions of the theoretically calculated defect size for (a) post-etch wafers and (b) as-cut wafers.
viewing orientation. It is known that in general the diamond
sawn wafer surface consists of many scratching grooves and
microcracks, as shown in Figure 6. As both the grooves and
microcracks are unidirectional, their effect on the observed
fracture strength will be quite different for different load ori-
entations, as can be explained from the perspective of frac-
ture mechanics. Bending perpendicular to the saw marks, the
scratching grooves can be considered as small round defects
as shown schematically in Figure 6(b). Bending parallel to
the direction of the saw marks, the long scratching lines and
associated subsurface microcracks effectively form a large
sharp defect as shown in Figure 6(c). The two different char-
acteristics of the defect size as a function of the relative ori-
entation of applied load and cutting direction cause the
fracture strength anisotropy observed in the silicon wafers.
The characteristic length of defects in the two bending
orientations is calculated by Eq. (3) with parameters of
Y ¼ 1:12, KIc ¼ 0:95 MPa m1=2 , and a maximum tensile re-
sidual stress of rr ¼ 37:5 MPa. Figure 7 shows the distribu-
tion curves of defects for both the as-cut and the post-etch
wafers. It can be seen that there is a skewed distribution of
defect sizes in the wafers in general. However, the distribu-
tion pattern is quite different for the two bending orienta-
tions. There is a low and narrow defect distribution for the
perpendicular bending orientation, but a high and broad dis-
tribution for the parallel bending. The peak defect sizes are
2 lm and 2.5 lm in the perpendicular bending orientation
and 6.5 lm and 7.5 lm in the parallel bending orientation for
post-etched mono-like and mc-Si wafers, respectively. For
the as-cut wafers, the defect size distribution shifts to higher
values. The peak defect sizes are 4 lm and 3 lm in the per-
pendicular bending orientation, and 9 lm and 10 lm in the
parallel bending orientation for the as-cut mono-like and mc-
Si wafers, respectively. These characteristic defect sizes
match well with the experimental results published in litera-
ture.18,19 The defect distribution indicates that the character-
istic defect size reduces by 2 to 3 lm with etching.
In conclusion, the residual stresses in crystalline silicon
wafers were measured nondestructively by a full field NIR
polariscope. The average residual stresses are 5.61–6.69 MPa,
with an observed local maximum residual stress of 37.5–
38.9 MPa in the as-cut wafers. The residual stresses reduce to
2.86–3.25 MPa for the average and 21.9–30 MPa for the local
Reuse of AIP Publishing content is subject to the terms at: https://publishing.aip.org/authors/rights-and-permissions. IP: 200.130.19.131 On: Mon, 22 Feb 2016 18:02:05
Appl. Phys. Lett. 102, 021909 (2013)
maximum in the post-etch wafers. The high residual stresses,
together with large microcracks, lead to low fracture strength
of the as-cut wafers. The fracture strength increases signifi-
cantly after removing the surface damage layer, which trans-
lates to a 2 to 3 lm defect size reduction for a 5 lm etch. The
fracture strength anisotropy is related to the defects, scratch-
ing grooves, and microcracks on the wafer surface.
The results show a detrimental effect of tensile residual
stresses on the fracture strength of crystalline silicon wafers.
Higher tensile residual stresses will lead to lower fracture
strength. It is therefore critical to measure and quantify the
residual stresses in a wafer. The non-destructive measure-
ment provided by a full field NIR polariscope is expected to
be valuable for both offline and inline wafer inspections in
solar cell manufacturing.
The authors would like to thank the Silicon Solar Con-
sortium (SiSoC) industry members for providing the experi-
mental samples.
1
C. H. Wu and J. C. Lambropoulos, J. Cryst. Growth 155, 38 (1995).
2
J. P. Kalejs, J. Cryst. Growth 230, 10 (2001).
3
S. J. Haake and E. A. Patterson, Exp. Mech. 32, 266 (1992).
4
S. He, S. Danyluk, T. Tarasov, and S. Ostapenko, Appl. Phys. Lett. 89,
111909 (2006).
5
B. Sopori, V. Budhraja, P. Rupnowski, S. Johnston, N. Call, H. Moutinho,
and M. Al-Jassim, in Proceedings of the 34th IEEE PVSC (1969), 2009.
6
R. Ahmed, M. E. Fitzpatrick, and N. H. Faisal, Surf. Coat. Technol. 206,
4180 (2012).
7
R. Suterio, A. Albertazzi, and F. K. Amaral, J. Strain Anal. for Eng.
Design 41, 517 (2006).
8
M. Nishikawa and H. Soyama, Mater. Des. 32, 3240 (2011).
9
P. Doig and P. E. J. Flewitt, NDT Int. 11, 127 (1978).
10
A. S. M. Y. Munsi, A. J. Waddell, and C. A. Walker, Strain 39, 3 (2003).
11
T. Kunz, M. T. Hessmann, B. Meidel, and C. J. Brabec, J. Cryst. Growth
314, 53 (2011).
12
Y. Kwon, S. Danyluk, L. Bucciarelli, and J. P. Kalejs, J. Cryst. Growth 82,
221 (1987).
13
K. Ramesh and D. K. Tamrakar, Opt. Lasers Eng. 33, 387 (2000).
14
E. A. Patterson, Strain 38, 27 (2002).
15
S. He, T. Zheng, and S. Danyluk, J. Appl. Phys. 96, 3103 (2004).
16
H. Wu and S. N. Melkote, Mater. Sci. Eng., A 549, 200 (2012).
17
C. Yang, H. Wu, S. Melkote, and S. Danyluk, “Comparative analysis of frac-
ture strength of slurry and diamond wire sawn multicrystalline silicon solar
wafers,” Adv. Eng. Mater. (in press).
18
H. Wu, S. N. Melkote, and S. Danyluk, Adv. Eng. Mater. 14, 342
(2012).
19
A. Bidiville, K. Wasmer, J. Michler, P. M. Nasch, M. van der Meer, and
C. Ballif, Prog. Photovoltaics 18, 563 (2010).