Difficulties making reliability predictions for Si, GaAs, and InP

Grady S. Whit&' a and Linda M. Braun'

aNational Institute of Standards and Technology, Gaithersburg, MD 20899

bLucent Technologies, Murray Hill, NJ 07974

ABSTRACT

The lifetime prediction model that has been developed for brittle materials implicitly assumes an initial
flaw population from which, under the influence of an applied or residual stress, cracks grow to failure.
The relationship between crack growth rate and stress intensity factor is assumed to be a power law
expression. While the tests used to predict lifetimes, i.e., Weibull distribution, inert strength, and dynamic
fatigue, can all be applied to semiconductors without apparent discrepancies, analysis ofthe crack growth
behavior in Si, GaAs, and lnP shows that assumptions in the lifetime model are violated for these materials.
Consequently, lifetime predictions based upon this model will be wrong.

Keywords: crack growth, failure mechanism, GaAs, InP, lifetime, reliability, semiconductor, Si

1. INTRODUCTION

Techniques to determine reliability in oxide ceramics have been extensively developed over the years,
leading to a lifetime prediction formalism that incorporates estimates for the strength ofthe material, the
flaw distribution in the material, and a model describing crack growth rates in the material as a function of
load (applied or residual). While phenornenological, this reliability model has been useful in predicting
lifetimes in window applications"23 and appears to be generally valid for most oxide materials. However,
attempts to apply the model to non-oxide materials, e.g., semiconductors, have run into serious problems.
These problems seem to arise from assumptions associated with the model's determination of flaw
population as well as the relationship between applied load and crack growth rate. In this manuscript, we
will address these two points as they apply to three semiconductor crystals widely used in the opto-
electronics industry: silicon, GaAs, and InP.

2. MODEL

The lifetime prediction model for oxides (Eq. 1) has been thoroughly described elsewhere3'4. Here, we
intend only to highlight certain features and assumptions" embedded in the formalism for comparison with

'1
Correspondence: Email: giady.white(i)nist.ov: Telephone: 3O 975 5752; Fax: 301 975 5334
'I' Some ofthe assumptions that lead to the simplified form ofEq. 1 are not germane to the focus of this
manuscript, which is the applicability ofcurrent models derived for brittle materials to lifetime prediction
ofsemiconductors. However, for clarity, should the reader compare Eq. 1 with the lifetime expressions in
references 3 or 4, we mention the following points. Eq. 1 assumes a) that the flaws leading to failure are
point flaws with a residual stress field identical to that obtained from an indentation and b) that indented
dynamic fatigue specimens are used to obtain lifetime data. Detailed derivations can be found in the
references. Ifthese assumptions are not met, Eq. becomes more complicated, but the three critical points
made in the manuscript remain unchanged. Specifically, the lifetime model depends upon a known
formalism that describes crack growth, a known initial flaw/strength distribution, and knowledge that the
specimen strength can be determined in the absence ofstable crack growth.
Optical Fiber and Fiber Component Mechanical Reliability and Testing, M. John Matthewson,
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 experimental observations.

1
tf
7
x IS)
N'+1(S)
II \N'—2
-N'

In Eq. 1 , tf S defined as the time to failure, c is the applied (or residual) stress to which the component is
subjected, S is the strength of indented specimens in the absence of environmental effects, and S is the
initial strength ofthe material for a given probability offailure, F. The parameters N' and ? are related to
the susceptibility ofthe material to environmentally enhanced crack growth4. Both ofthese paran-leters
will be discussed below. Equation I is a convolution of expressions describing three physical attributes
that are known to control lifetime in brittle materials: flaw distribution, crack growth rate, and inert
strength. In addition, Eq. 1 assumes that dynamic fatigue measurements will be made on indented
specimens to quantify the crack growth behavior in the material. Each ofthese attributes will be discussed
below.

2.1 Flaw distribution

Although Eq. 1 predicts lifetimes for a brittle material with any initial strength, S, usually S is chosen to be
a value for which a large portion, e.g., 95%, ofthe components are expected to survive. This requires that
the relationship between S and the probability of failure, F, be determined. However, brittle materials fail
from flaws that locally amplify the magnitude ofstresses to which the material is subjected5. In structural
ceramics, these flaws include scratches, pores, pits, inclusions, or cracks, resulting from processing,
handling, and use conditions. Since flaws control (limit) the material strength, characterizing the flaw
distribution is a necessity for assessing component reliability. Because the flaw distribution is difficult to
measure but strength is easily measured, the survival probability is generally formulated in terms of
strength3. Two key assumptions leading to Eq. 1 are that the experiments to determine strength distribution
do not alter the initial flaw population and that the flaw population in the test pieces mimics that in the final
component. Implicit in these assumptions is that the flaws change only through the environmentally
enhanced crack growth processes described in Section 2.2 below*. Ifthese assumptions are valid, the
strength, 5, can be determined, for a given F, from Eq. 2.

r
s=st +(s0+s
t (2)
Lk(m,S) in—_-_J
1—F J

The other parameters in Eq. 2 are k, a scaling factor that corrects for differences in the area sampled by the
test pieces and the area under maximum load in the final component, S, the Weibull shape parameter,
the threshold stress below which no failures occur, and m, the Weibull parameter that describes the width
ofthe strength/flaw distribution. As in decreases, (1-F(S)) becomes less sensitive to S. Weibull tests are
usually conducted at high loading rates and in an inert environment to minimize environmental
contributions to the failure.

*
Throughout this paper, we assume that no flaw generation or crack extension is resulting from specimen
mishandling during the experimental procedure.

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 2.2 Crack growth rate

In Eq. 1, all ofthe subcritical crack growth, i.e., stable growth offlaws, is assumed3'4 to be described by a
power law expression that relates crack growth velocity, V, to the stress intensity factor at the flaw, K1:

V=AK1N (3)
Equation 3 is a phenonienological expression that appears to describe most oxide ceramics reasonably well
over the velocity ranges that can easily be measured in a laboratory setting: 10" rn/s < V < 102rn/s. In
this velocity range, direct observations ofcrack growth can be made. N denotes the stress sensitivity of the
crack velocity; the larger N is, the less effective the environment is at enhancing crack growth. As long as
it is known that the physical processes controlling crack growth can be described by an expression of the
form ofEq. 3, the lifetime prediction model (Eq. 1) remains valid**. However, typically, lifetime
predictions are based on dynamic fatigue measurements4, in which no direct observation ofcrack growth
occurs. Rather, an indentation is placed in the center ofa bend specimen to act as a failure site6 and the
specimen is then broken in either four-point7 or biaxial' bending in an appropriate environment (e.g., liquid
water or water vapor). These bend tests, made as a function of loading rate, give rise to the following
expression:
)dY (4)

by which the logarithm ofthe failure strength ofthe material, log(cf), is related to the logarithm of the
1
stressing rate, log(d&dt) by a slope of and an intercept of log(2) (see Eq. 1).
N'+l
The N' determined from Eq. 4 incorporates the effects ofthe indentation residual stress4 and is related to
N", defined by Eq. 3, by N' = (3N+2)/4. The critical point to bear in mind, however, is that N can be
determined from direct measurements ofcrack growth but N' is determined from dynamic fatigue
measurements. In dynamic fatigue measurements, crack growth is never actually observed as a function of
load and environment.

2.3 Inert strength of indented specimens

Eq. 1 contains the term S, the inert strength ofthe indented specimens, which is intended to provide an
upper liiTlit to the dynamic fatigue strength values. The indented inert strength measurements are made in
the same manner as the dynamic fatigue measurements, described previously, except that efforts are made
to avoid any stable crack growth. Since stable crack growth is caused by environmental interactions in the
oxides, typically these tests are made in an inert environment, e.g., N, or Ar, with a loading rate as fast as
possible. In this manner, environmentally enhanced crack growth is minimized. The critical aspect of
determining S is the same as that in determining the Weibull distribution; strength values must be
obtained without the occurrence of stable crack growth.

These three processes, strength distribution measurements, dynamic fatigue, and inert strength
determination, form the basis for lifetime prediction in brittle materials. Ifany one ofthe three is incorrect,
the predicted lifetime (Eq. 1) will be wrong.

**
In this discussion we are ignoring effects ofextrapolating Eq. 3 beyond the range for which it describes
the data. A discussion ofthis issue can be found in reference 12.

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 3. EXPERIMENTAL PROCEDURE
The specimens used in this work are single crystal Si, GaAs, and InP polished single crystals. The faces of
the specimens are (001) and the cleavage planes used for crack propagation are {11O} for GaAs and InP
and {111} for Si.

P12 P12

a) b)
Figure 1 : a) Schematic of DBC specimen. Crack is generated by a Knoop indentation applied to the end of
the specimen. b) Schematic of specimen under constant moment loading. Dead weight load applied to the
ends ofthe bars attached to the specimen generates a stress intensity factor at the crack tip that is
independent of crack length8.

In addition to the experimental procedures referenced above, the constant moment double-cantilevered-
beam (DCB) technique8 is used to measure crack velocity directly. The advantage ofthe constant moment
DCB technique is that K1 is independent ofcrack length. The DCB9, dynamic fatigue'° and Weibull3
procedures used to investigate Si, InP, and GaAs are thoroughly described elsewhere. However, because
the constant moment DCB test is less common than dynamic fatigue, it is outlined below. In the constant
moment DCB technique, a specimen approximately 12 mm x 75 mm x r mm is produced, either by
cleavage or by use ofa diamond saw. In this work, i is approximately 0.4 mm for the InP and GaAs and
1.0 miT' for the Si. A Knoop-shaped diamond is pressed into the center ofthe 12 mm wide end of the
specimen at about 30% ofthe load required to cleave the specimen; after 20 s —45 s a cleavage crack
appears that runs about 1/3 the length ofthe specimen (Figure Ia). A mechanical test machine operating at
constant displacement, rather than constant load, is used to drive the Knoop indentor. The pre-cracked
specimen is then glued to two stainless steel arms and suspended with the two steel arms supported by
fulcrums. Dead weight loading is applied to the ends ofthe arms to generate loading moments in the
specimen on both sides ofthe crack and the resultant crack growth is monitored with a traveling telescope
(Figure lb). The specimen is enclosed in an environmental chamber in which either liquid or gaseous
environments can be introduced.

Although a number ofenvironments have been used in the investigation ofenvironmentally enhanced
fracture ofGaAs" and Si, for the purposes ofthis paper, only two are discussed: distilled water and water

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 vapor at 50% relative humidity (RH). Experiments in 50% RH are conducted by enclosing the specimen
and load train in plastic and purging the system with Ar or N, gas which is passed through a bubbler
system to achieve 50% RH. The system consists oftwo parallel gas paths, one ofwhich passes through
distilled water in two bubblers at room temperature.

4. SUMMARY OF EXPERIMENTAL OBSERVATIONS

Results ofdynamic fatigue measurements in InP and DCB measurements in both InP and GaAs have been
presented elsewhere10'11'12. Here, we review those results as well as present results ofDCB measurements
of Si with a focus on their implications with regard to lifetime predictions.

4.1 GaAs

-5.5

,. -6.0

-6.5

-7.0
0.3 0.4 0.5

K1(MPa*ml2)

Figure 2: DCB data12 ofGaAs in distilled water: N = 36 +1- 3

Figure 2 plots the crack velocity ofGaAs in liquid water as a function ofstress intensity for DCB
measurements. The curve is well behaved and reproducible both within individual specimens and between
specimens. There is a one-to-one relationship between K1 and log (V); i.e., the data are well described by a
function ofthe form ofEq. 3. In contrast, no crack growth is observed for GaAs in a gaseous environment
ofSO% RH in N,. In the attempt to detect crack growth in water vapor, specimens were held under load
for a length of time such that any crack extension corresponding to a velocity > 1 0b0 rn/s would have been
detected.

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 4.2 InP

Figure 3 is a plot ofdata obtained on the same DCB apparatus for a single InP specimen. The data
presented in Fig. 2 are typical ofthe types ofcrack growth behavior observed in each ofthe five InP
specimens. However, no two specimens generated data sets that overlap. More importantly, the crack
velocity and K1 show no functional dependence in DCB measurements; i.e., there is not a well-defined
value of K1 for any value of log (V). The downward arrows in Fig. 2 indicate that the crack velocity was
decreasing over time at a constant K1. Similarly, the upward arrows represent increasing crack velocity as a
function oftime at constant K1. Data points that are connected by arrows represent measurements for
which a load was applied to the specimen and the connected crack velocities were measured without
removing the load. All other data points represent independent measurements for which the load was

-1

-3

,,-\ -4

-5

-6

.7

-8

-9
(). 2 0.3 ().4

K1(}vfPa In112)

Figure 3: DCB data oflnP in distilled water. Data were taken from one specimen, but are typical ofwhat is observed
in all the InP DCB specimens. Circles represent crack growth. Downward pointing triangles indicate that no crack
growth was observed. The log (V) associated with the triangles is the upper limit that crack velocities could attain
without being observed, for the time the specimen was held at load. The arrows represent changes in crack velocity for
a constant Kj under dead-weight loading conditions.

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 applied and subsequently removed for the single velocity value. The data points at the bottom ofFig. 2
represent the fact that, at those values of K1, no crack growth is observed. In these cases, sometimes, it is
possible to observe crack growth upon reducing K1 to a lower value for which crack growth had previously
been observed. Usually when this is done, however, no further crack growth is observed at the lower K1.
The data points with velocities > O rn/s were measured after the crack tip began moving; for several
1

seconds after application ofthe load, the crack tip appeared to be stationary. In one important respect, all
ofthe InP specimens behave similarly. At lower values ofK1, log (V) often decreases with time, but, near
K1, log (V) increases with time. Figure 4 shows the results ofdynamic fatigue experiments for the InP
specimens.

100

c $
. . t, ,
. ,* $
Cl) • . 4

..E
e ••

30
!!!!• ••! I I
0.001 0.()1 0.1 1 10 100 1000
Loading Rate (MIPaJs)

Figure 4: Dynamic fatigue data of InP. Liquid

water and water vapor are indistinguishable. Line
is least squares fit to the data.

4.3 Si

No crack growth is observed in Si in either liquid water or water vapor. A DCB specimen at K1 > 0.95 K1
has been kept in an aqueous environment for over 30 days without any crack motion being detected. In
this case, the environment included HF to remove any Si02 formed on the crack walls. Within the
sensitivity ofthe experiment, any V > 5 x 1012 rn/s would have been observed.

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 5. DISCUSSION
5.1 Environmentally enhanced fracture

The slow crack growth behavior ofGaAs, InP, and Si was distinctly different with one exception. None of
the materials appears to undergo environmentally enhanced fracture in gas. The behavior ofthe three
materials in water has different implications for each material with respect to the effect of crack growth on
lifetime predictions.

Figure 2 shows a well-behaved GaAs crack growth curve fit to Eq. 3. Because Eq. 3is phenomenological,
it is not necessary that the environmental mechanism that drives cracks in GaAs be the same as the one for
which the lifetime prediction model was developed in oxide glasses. It is only necessary that the functional
form be the same. Since Fig. 2 shows a crack growth curve in water with a well defined N-value of36, it
is reasonable to assume that the brittle material reliability model described by Eq. 1 will provide a realistic
prediction for the lifetime ofGaAs under load in liquid water. However, a problem would arise if
measurements were made at 50% RH and the results assumed to apply to water. Under such conditions,
i.e., essentially no environmentally enhanced crack growth, predicted lifetimes for K1 < K1 would be very
long. This is in obvious contrast to the behavior of GaAs in water. These results underscore the necessity
for conducting the measurements in the identical environment envisioned for the final component***.

In contrast to GaAs, InP provides an example ofwhat can occur ifEq. 3 does not describe the crack growth
behavior ofthe material. As mentioned above, Fig. 4 is the dynamic fatigue curve for the thP specimens.
A linear least squares fit to the dynamic fatigue data gives an N-value > 100, which suggests that InP is
only slightly susceptible to environmentally enhanced fracture in liquid water. Statistical analysis of the
data in Fig. 4 results in a wide range ofpossible values for N, but heavily weighted for N > 100. There is
nothing in the data that suggests that the dynamic fatigue data do not provide valid input into the lifetime
prediction model. However, unlike the situation in GaAs, in which the mechanism has changed but the
data are still described by Eq. 3, direct observation ofcrack propagation clearly demonstrates that a power
law expression does not describe crack growth as a function of K1 in water in InP. Indeed, although it is
quite clear that cracks will grow in water over a range of K1 values, it is not clear how K1 is related to crack
growth in InP and that a lifetime prediction based upon a power law relationship is not valid.

Finally, Si shows no evidence ofcrack growth due to the presence ofwater that can be described by Eq. 3.
Lifetime predictions based upon Eq. 1 would be essentially infinite under these conditions and we would
expect neither direct observation ofcrack growth nor indirect measurements such as dynamic fatigue to
suggest that this prediction is in error.

5.2 Flaw population

However, there remains a serious problem with lifetime predictions in all three ofthese materials. As
discussed above, DCB measurements of Si, GaAs and InP exhibit no environmentally enhanced fracture in
water vapor over any K1 tested. However, all three materials do exhibit delayed fracture in air; that is how
the cracks are generated for the DCB specimens. Therefore, in addition to whatever environmental
mechanisms are active in GaAs (Fig. 1) or may be active in InP (Fig. 2), there is another mechanism that
leads to mechanical failure in all three materials. Because the delayed failure in air occurs under Knoop
indentation in constant displacement conditions, the failure may be related to dislocation generation and
motion in a high stress field. lfthis is the case, there is a plastic deformation and, hence, loading rate
dependent process leading to delayed failure in all three materials. However, Weibull measurements
typically are made at a high loading rate to minimize effects ofenvironmentally enhanced fracture. If there
is a rate dependence on inert fracture strength, then Weibull measurements do not sample the same flaw
distribution as is seen in service. However, even if dislocation generation and motion are not related to the
***
It may be worth noting that the authors are aware ofno oxide glass that undergoes environmentally
enhanced crack growth in liquid water but not in water vapor. The difference in behavior of GaAs
suggests a different environmental attack mechanism is operating in this material.

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 observed crack initiation, there remains an unknown mechanism operating that leads to mechanical failure
in all ofthese materials. Because the mechanism is completely unknown, questions regarding the validity
ofboth Eq. 3 and the relationship ofthe flaw populations in the Weibull specimens to that in the final
components need to be investigated.

CONCLUSIONS

Lifetime prediction in brittle materials is based on a model developed for oxide glasses that depends on
three parameters: initial flaw or strength distribution, inert strength ofan indented specimen, and a power
law relationship linking crack velocity to K1. While this model appears to work well for oxide ceramics, it
does not appear to be valid for semiconductors such as Si, GaAs, or InP. In particular, the power law flaw
growth mechanism and, possibly, the Weibull determination offlaw populations need to be examined more
carefully.

REFERENCES

1. S. W. Freiman, E. R. Fuller, Jr., G. D. Quinn, J. B. Quinn, and W. C. Carter, "Reliability Analysis

for BK-7 Glass Aircraft Windows," Final Report for Itek Optical Systems, Order # 71 15-A-1572,
NIST, April 1993.
2. S. M. Wiederhorn, A. G. Evans, E. R. Fuller, Jr., and H. Johnson, "Application of Fracture
Mechanics to Space-Shuttle Windows," I. Am. Ceram. Soc., Vol. 57, No. [7], 319-323 (1974).
3. E. R. Fuller, Jr., SW. Freiman, J. B. Quinn, G. D. Quinn, and W. C. Carter, "Fracture mechanics
approach to the design ofglass aircraft windows: a case study", SPIE 2286 pp. 419-429, 1994.
4. E. R. Fuller, Jr., B. R. Lawn, and R. F. Cook, "Theory of Fatigue for Brittle Flaws Originating
from Residual Stress Concentrations," I Am. Ceram. Soc., Vol. 66, No. [5],3 14-321 (1983).
5. B. R. Lawn, Fracture ofBrittle Solids, Second Edition, Cambridge University Press, Cambridge,
1993.
6. T.P. Dabbs, BR. Lawn, and P.L. Kelly, "A Dynamic Fatigue Study ofSoda-Lime Silicate and
Borosilicate Glasses Using Small Scale Indentation Flaws," Phys. Chern. Glasses 23 [2] 58-66
(1982).
7. ASTM Standard Cl 161-94, " Standard Test Method for Flexural Strength ofAdvanced Ceramics
at Ambient Temperature" AMERICAN SOCIETY FOR TESTING AND MATERIALS, West
Conshohocken, PA (1996).
8. 5. W. Freiman, DR. Mulville, and P.W. Mast, "Crack Propagation Studies in Brittle Materials," J.
Mater. Sci. 8 1527-33 (1973).
9. G.S. White and L.M. Braun, "Strength vs. Stressing Rate and Indentation Crack Growth Behavior
oflndium (III) Phosphide", J. Am. Ceram. Soc. 80 [10] 2699-701, 1997.
10. G.S. White, SW. Freiman, and AM. Wilson, "Environmentally Enhanced Fracture in GaAs," J.
Am. Ceram. Soc. 74 [2] 419-21 (1991).
11. L.M. Braun and G.S. White, "Double Cantilever Beam Measurements ofCrack Growth in
Indium(III) Pliosphide," J. Am. Cerarn. Soc. 80 [2] 503-505 1997.
12. SM. Wiederhorn, "Dependence ofLifetime Predictions on The Form ofthe Crack Propagation
Equation," Fracture 1977, Volume 3, ICF4, Waterloo, Canada pp. 893-902 (1977).

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